Plasma Sprayed Copper-Nickel-Indium Coatings on Titanium Alloys

Copper-nickel-indium coatings were deposited on the surface of titanium alloy specimens by plasma spraying. The structure and properties of the coatings were studied thoroughly using optical and scanning electron microscopy. The mechanical behavior of the Cu-Ni-In coated titanium substrates was examined. The coating was found to decrease the tensile strength of the titanium alloy substrate. The elastic modulus and the ultimate tensile strength of the coated system were found to decrease with increasing coating thickness. The residual stresses of the coated system were also calculated.     

The effect of electron beam sterilization on the physical properties of the bioresorbable polymer coatings on the titanium 6-aluminum 4-vanadium substrate

The aim of the work is to determine the physical properties of titanium 6-aluminum 4-vanadium alloy with poly (glycolide-ϵ-caprolactone) coating after electron beam sterilization. First, the metal substrate is machined with grade 120 and 320 grinding papers. Some of the samples are subjected to anodic oxidation. Then, the samples are coated with a biodegradable polymer layer of poly (glycolide-ϵ-caprolactone). Samples with polymer coatings are subjected to electron beam sterilization. To evaluate the effect of sterilization on physical properties of modified titanium alloy the scanning electron microscopy and atomic force microscopy, adhesion studies of the polymer coating to the metal substrate and wettability tests are applied. On the basis of the obtained results, an increase of the contact angle value is found both after applying the polymer coating to the surface of the tested titanium 6-aluminium 4-vanadium alloy as well as after electron beam sterilization. In addition, a slight increase of the adhesion in sterilized samples comparted to non-sterilized is observed. In scanning electron microscopic observations, traces of machining on the surface of the metal substrate and the continuity of the polymer coatings before and after sterilization are found. In the atomic force microscopic studies in relation to the initial state, a very good mapping of the surface topography of the samples with a homogeneous coating is found.     

Hydroxyapatite coating by dipping method,and bone bonding strength

Hydroxyapatite (HA) was coated onto titanium rods by a dip coating method using HA sol. The HA sols were prepared by dispersing HA crystals less than 100 nm length in distilled water or physiological salt solution using an ultrasonic homogenizer. The surface of the HA coating was homogeneous as determined by scanning electron microscopy (SEM). After implantation of uncoated and HA dip coated titanium rods in dog femurs, new bone formation was observed only around the coated material. The bone bonding strength to HA coated rods was 1.0, 1.5, 2.0 and 2.5 Mpa after 1,2,3 and 4 weeks implantation, respectively, as determined by pull-out testing. These values were over twice that of the uncoated titanium rods at 1–4 weeks after implantation. The dip coated titanium exhibited superior biocompatibility to the uncoated implant and may be of great value for bone repacement applications.This paper was accepted for publication after the 1995 Conference of the European Society of Biomaterials, Oporto, Portugal, 10–13 September.     

正交试验优化金红石型钛白粉 表面包Al2O3的工艺研究

通过正交试验优化了金红石型钛白粉包Al2O3的工艺条件。采用Zeta电位分析仪、扫描电子显微镜、透射电子显微镜、傅里叶红外光谱仪等对所得样品的结构和性能进行了表征与分析。结果表明:包膜的优化工艺条件是钛白粉的质量分数为10%,包膜剂的添加质量分数为4%,包膜温度为60℃,搅拌速度为290r/min;影响金红石型钛白粉包膜的首要因素是钛白粉的质量分数,且低质量分数下更有利于金红石型钛白粉颗粒的表面成膜;Al2O3以化学键的形式键合在金红石型钛白粉颗粒表面,形成Al-O-Ti键。     

In vitro evaluation of a multispecies oral biofilm over antibacterial coated titanium surfaces

Peri-implantitis is an infectious disease that affects the supporting soft and hard tissues around dental implants and its prevalence is increasing considerably. The development of antibacterial strategies, such as titanium antibacterial-coated surfaces, may be a promising strategy to prevent the onset and progression of peri-implantitis. The aim of this study was to quantify the biofilm adhesion and bacterial cell viability over titanium disc with or without antibacterial surface treatment. Five bacterial strains were used to develop a multispecies oral biofilm. The selected species represent initial (Streptococcus oralis and Actinomyces viscosus), early (Veillonella parvula), secondary (Fusobacterium nucleatum) and late (Porphyromonas gingivalis) colonizers. Bacteria were sequentially inoculated over seven different types of titanium surfaces, combining different roughness level and antibacterial coatings: silver nanoparticles and TESPSA silanization. Biofilm formation, cellular viability and bacterial quantification over each surface were analyzed using scanning electron microscopy, confocal microscopy and real time PCR. Biofilm formation over titanium surfaces with different bacterial morphologies could be observed. TESPSA was able to significantly reduce the cellular viability when compared to all the surfaces (p?<?0.05). Silver deposition on titanium surface did not show improved results in terms of biofilm adhesion and cellular viability when compared to its corresponding non-coated surface. The total amount of bacterial biofilm did not significantly differ between groups (p?>?0.05). TESPSA was able to reduce biofilm adhesion and cellular viability. However, silver deposition on titanium surface seemed not to confer these antibacterial properties.

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Controlled adhesion of human lymphocytes on electrically charged polymer surface having phosphorylcholine moiety

The human lymphocytes were interacted with polymer surfaces whose surface potential was controlled by the formation of a polyion complex (PIC) having a phosphorylcholine moiety. 3-(Methacryloyloxypropyl)-trimethyl ammonium iodide as the cationic unit or potassium 3-methacryloyloxypropyl sulfonate as the anionic unit was copolymerized with 2-methacryloyloxyethylphosphorylcholine (MPC) and _n-butyl methacrylate. PIC was made at the solid-liquid interface, that is, an aqueous solution containing an anionic polymer with different concentrations was contacted with a cationic polymer coated polymer membrane. The formation process of PIC was followed using a quartz crystal microbalance, and the PIC surfaces were analyzed by ζ potential and X-ray photoelectron spectroscopy. The surface potential on the PIC was controllable from +20 to -16 mV, which increased in the amount of adsorbed anionic copolymer as the ζ potential decreased toward the negative charge. The PIC surface in contact with human lymphocyte for 5 h was observed using ascanning electron microscopy and the density of the adherent human lymphocyte was determined by the lactate dehydrogenase method. The lymphocyte adhesion on the surface was gradually reduced with an increase in the negative value of the ζ potential. The morphological change in the adherent lymphocytes was not observed on the polymer surfaces with MPC units.The adherent lymphocytes were not activated on the PIC surface. The lymphocyte adhesion with reduced activation could be controlled by changing the surface potential on the polymer with the MPC unit.     

Surface with antimicrobial activity obtained through silane coating with covalently bound polymyxin B

Surfaces exhibiting antimicrobial activity were prepared for potential medical application. A polycationic lipopeptide polymyxin B was selected as the bioactive agent for covalent immobilization onto the surface. First, by using sol–gel technology the inert glass substrate was functionalized by a silane coating with epoxide rings to which the peptide was coupled by means of a catalyst. Preparation of the coating and presence of the peptide on the surface were followed by FTIR, XPS and AFM analyses. The obtained material showed antimicrobial effect indicating that in spite of immobilization the peptide has retained its bioactivity. The coated surface was able to reduce bacterial cell counts of the Gram-negative bacterium Escherichia coli by more than five orders of magnitude in 24 h of incubation. It can be concluded that bioactive coatings with covalently bound polycationic peptides have potential for application on medical devices where leakage into the surrounding is not allowed in order to prevent bacterial growth and biofilm formation.     

Influence of Egyptian nanoilmenite/amorphous silica composite particles on the electrochemical and mechanical properties of cold galvanizing formulation coatings

In the present work, Egyptian ilmenite nanoparticles (FeTiO₃ NPs) were obtained with the average diameters of 20?nm by a direct solid-phase milling process and synthesized amorphous silica powder grains were processed to prepare a novel fabricated Egyptian nanoilmenite/amorphous silica composite (ENI/AS) particles. Flaky-like nature of ENI/AS and the spherical shape of Zn-dust particles were emphasized by scanning electron microscopic (SEM) micrographs. The nano features of ENI/AS particles were confirmed by transmission electron microscope (TEM) investigation. Various alkyd-based cold galvanizing coating formulations were modified using different uniformly dispersing amounts of the processed ENI/AS particles as a modifier to form some nanocomposite coatings. The electrochemical behavior of nanocomposite modified coated steel films in oil-wells formation water solution have been studied by both potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. The mechanical properties of the coated films were studied through some coating tests as cross-cut adhesion, bend and impact to assert their application efficiency. Scanning electron microscope (SEM) technique was utilized to survey the protective film formed on the carbon steel surface by these modified coatings in formation water solution. The results of this study reinforced remarkable corrosion protection properties of ENI/AS modified cold galvanizing coating.     

Initial salivary pellicle formation on solid substrates studied by AFM

Organic layers of salivary biopolymers adsorbed on soft and hard oral tissues, referred to also as salivary pellicle, play a critical role with respect to all surface phenomena taking place in the oral cavity. The initial stages of pellicle formation are of great interest since they determine the ensuing processes of salivary biopolymer adsorption and subsequent adherence of bacteria. In spite of the important physiological role of the pellicle in protecting the enamel surface against short-term acidic attacks, the composition and ultrastructure of the pellicle layer are not yet understood and resolved in detail. The present study utilized atomic force microscopy (AFM), for the first time, to elucidate the morphogenesis and ultrastructural pattern of initial salivary pellicle formation taking place in situ on solid substrates of mica, silicon wafer and graphite. Using tapping mode AFM, salivary pellicles were found in all intraorally exposed specimens and revealed a globular surface morphology of the adsorbed protein layer. The average diameter and height of the adsorbed salivary proteins were determined to be 15 +/- 3 nm and 2.0 +/- 0.5 nm, respectively. It was also found that the surface energy of the substrates affects the rate of pellicle formation, while the overall size of the adsorbed salivary proteins appears to be identical on all studied substrates.     

Studies of bacterial adhesion on TiN, SiO2-TiO2 and hydroxyapatite thin layers deposited on titanium and Ti6Al4V alloy for medical applications

The Staphylococcus epidermidis biofilm formation on titanium or titanium alloy, coated with TiN, SiO₂-TiO₂ and electrodeposited hydroxyapatite, was tested. Surfaces of titanium, Ti6Al4V alloy or TiN, modified with SiO₂-TiO₂ layer, were found to be highly resistant to bacterial adhesion. Only small amounts of bacterial cells were observed on matrices coated by thin hydroxyapatite films, deposited on both SiO₂-TiO₂ and TiN + SiO₂-TiO₂ interlayers. Biological tests showed that the biofilm formed massively on polished and ground titanium and titanium alloy surfaces, also those covered with TiN, but not on those modified with SiO₂-TiO₂ nanofilm.     

Pulse current co-deposition of Ni-WS2 nano-composite film for solid lubrication

This study was undertaken to observe the effect of nano-composite coating on steel surface for enhancing its tribological properties. In the investigation, EN31 steel surfaces were coated with nano-composite (Ni-WS₂) by pulse current co-deposition process in order to improve the tribological properties of the surface. The coatings were prepared according to different parameter settings. The effect of variations on coating thickness, microstructure, surface morphology, microhardness and tribological properties was observed. The maximum coating thickness of 117?µm with 8% by weight of WS₂ particle concentration could be attained with the following parameter settings: applied voltage: 5?V; pulse frequency: 20?Hz; WS₂ concentration: 20?g/l; duty factor: 0.6 and bath temperature: 50°C. The average friction coefficient of the deposited surface was 0.11, which is significantly less than that of the EN31 steel surface (average coefficient of friction >?0.5).     

Controlled adhesion of human lymphocytes on electrically charged polymer surface having phosphorylcholine moiety

The human lymphocytes were interacted with polymer surfaces whose surface potential was controlled by the formation of a polyion complex (PIC) having a phosphorylcholine moiety. 3-(Methacryloyloxypropyl)-trimethyl ammonium iodide as the cationic unit or potassium 3-methacryloyloxypropyl sulfonate as the anionic unit was copolymerized with 2-methacryloyloxyethyl phosphorylcholine (MPC) and n-butyl methacrylate. PIC was made at the solid–liquid interface, that is, an aqueous solution containing an anionic polymer with different concentrations was contacted with a cationic polymer coated polymer membrane. The formation process of PIC was followed using a quartz crystal microbalance, and the PIC surfaces were analyzed by ζ-potential and X-ray photoelectron spectroscopy. The surface potential on the PIC was controllable from +20 to −16 mV, which increased in the amount of adsorbed anionic copolymer as the ζ-potential decreased toward the negative charge. The PIC surface in contact with human lymphocyte for 5 h was observed using a scanning electron microscopy and the density of the adherent human lymphocyte was determined by the lactate dehydrogenase method. The lymphocyte adhesion on the surface was gradually reduced with an increase in the negative value of the ζ-potential. The morphological change in the adherent lymphocytes was not observed on the polymer surfaces with MPC units. The adherent lymphocytes were not activated on the PIC surface. The lymphocyte adhesion with reduced activation could be controlled by changing the surface potential on the polymer with the MPC unit.     

Studies of calcium-precipitating oral bacterial adhesion on TiN,TiO2 single layer,and TiN/TiO2 multilayer-coated 316L SS

Titanium nitride (TiN), titanium oxide (TiO₂) single layer, and TiN/TiO₂ multilayer coatings were deposited on a 316L stainless steel substrate using reactive magnetron sputtering process with the aim of preventing bacterial adhesion. The crystal structures of as-prepared coatings were evaluated using X-ray diffraction analysis. The cubic structure of TiN, anatase, and rutile structure of TiO₂ was noticed. Atomic force microscopy images exhibited a relatively smooth surface for all coatings. The surface wettability studies confirmed that the coatings were hydrophilic in nature. The rate of bacterial adhesion was evaluated using scanning electron microscopy and epifluorescence microscopy. These results demonstrated that the coated substrates could help to effectively reduce the bacterial adhesion and biofilm formations.     

Polyetheretherketone and titanium surface treatments to modify roughness and wettability-Improvement of bioactivity and antibacterial properties

Among the materials available for implant production,titanium is the most used while polyetherether-ketone (PEEK) is emerging thanks to its stability and to the mechanical properties similar to the ones of the bone tissue.Material surface properties like roughness and wettability play a paramount role in cell adhesion,cell proliferation,osteointegration and implant stability.Moreover,the bacterial adhesion to the biomaterial and the biofilm formation depend on surface smoothness and hydrophobicity.In this work,two different treatments,sandblasting and air plasma,were used to increase respectively roughness and wettability of two materials:titanium and PEEK.Their effects were analyzed with profilometry and contact angle measurements.The biological properties of the material surfaces were also investigated in terms of cell adhesion and proliferation of NIH-3T3 cells,MG63 cells and human Dental Pulp Stem Cells.Moreover,the ability of Staphylococcus aureus to adhere and form a viable biofilm on the samples was evaluated.The biological properties of both treatments and both materials were compared with samples of Synthegra(R) titanium,which underwent laser ablation to obtain a porous micropatterning,character-ized by a smooth surface to discourage bacterial adhesion.All cell types used were able to adhere and proliferate on samples of the tested materials.Cell adhesion was higher on sandblasted PEEK samples for both MG63 and NIH-3T3 cell lines,on the contrary,the highest proliferation rate was observed on sandblasted titanium and was only slightly dependent on wettability;hDPSCs were able to proliferate similarly on sandblasted samples of both tested materials.The highest osteoblast differentiation was ob-served on laser micropatterned titanium samples,but similar effects,even if limited,were also observed on both sandblasted materials and air plasma treated titanium.The lowest bacterial adhesion and biofilm formation was observed on micropatterned titanium samples whereas,the highest biofilm formation was detected on sandblasted PEEK samples,and in particular on samples not treated with air-plasma,which displayed the highest hydrophobicity.The results of this work showed that all the tested materials were able to sustain osteoblast adhesion and promote cell proliferation;moreover,this work highlights the fea-sible PEEK treatments which allow to obtain surface properties similar to those of titanium.The results here reported,clearly show that cell behavior depends on a complex combination of surface properties like wettability and roughness and material nature,and while a rough surface is optimal for cell adhesion,a smooth and less hydrophilic surface is the best choice to limit bacterial adhesion and biofilm formation.     

A controlled release of antibiotics from calcium phosphate-coated poly(lactic-co-glycolic acid) particles and their in vitro efficacy against Staphylococcus aureus biofilm

Ceramic-polymer hybrid particles, intended for osteomyelitis treatment, were fabricated by preparing poly(lactic-co-glycolic acid) particles through an emulsion solvent evaporation technique, followed by calcium phosphate (CaP) coating via a surface adsorption-nucleation method. The presence of CaP coating on the surface of the particles was confirmed by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. Subsequently, two antibiotics for treating bone infection, nafcillin (hydrophilic) and levofloxacin (amphiphilic), were loaded into these hybrid particles and their in vitro drug release studies were investigated. The CaP coating was shown to reduce burst release, while providing sustained release of the antibiotics for up to 4 weeks. In vitro bacterial study against Staphylococcus aureus demonstrated the capability of these antibiotic-loaded hybrid particles to inhibit biofilm formation as well as deteriorate established biofilm, making this hybrid system a potential candidate for further investigation for osteomyelitis treatment.     

Assessment of the Cytocompatibility of Poly‐(N‐hexylvinylpyridinium) Used as an Antibacterial Implant Coating

Medical implants made of titanium have a wide variety of applications, ranging from replacement of a single tooth to extraoral maxillofacial prosthetic rehabilitation or hip endoprosthesis. The long‐term success of such osseointegrated titanium implants is endangered by inflammation of periimplant hard or soft tissues caused by a bacterial infection. Therefore, implants should ideally inhibit bacterial adhesion and growth, but allows strong attachment of connective tissues or epithelium at the same time. Antimicrobial polymers like poly(vinyl‐N‐hexylpyridinium bromide) (hexyl‐PVP) are a promising approach as implant coatings to inhibit bacterial adhesion, but little is known about the biocompatibility of these polymers. The aim of the present study was to develop a method for evaluation of the cell acceptance of hexyl‐PVP or copolymers of vinyl‐N‐hexylpyridinium bromide and (4‐vinylbenzyl)phosphonic acid diethylester (poly((hexyl‐VP)‐co‐VBP)) as coating on titanium disks. Primary human gingival fibroblasts were used and biocompatibility was assessed by cell adhesion and proliferation. The cell morphology of the fibroblasts on these surfaces was analyzed by scanning electron microscopy (SEM) and was used as additional criterion. The results indicate no significant differences in adhesion or proliferation rate between primary human gingival fibroblasts seeded on polymer‐coated titanium disks and uncoated titanium disks as a control. Although SEM micrographs displayed moderate differences in cell morphology between the two groups, application of hexyl‐PVP or the corresponding copolymers as antibacterial coatings for medical implants or devices appears to be promising.     

In Vivo and In Vitro investigation of titanium oxide layers coated on LTI-carbon by IBED

A layer of titanium oxide layer was coated on low temperature isotropic pyrolytic carbon (LTI-carbon), a prevailing material used for artificial heart valves' fabrication, by ion beam enhanced deposition (IBED). Glancing angle x-ray diffraction (GAXRD), X-ray photoelectron spectroscopy (XPS), Rutherford backscattering spectroscopy (RBS), atomic force microscopy (AFM) and transmission electronic microscopy (TEM) were used to characterize the deposited titanium oxide layer. The results show that the layer is polycrystalline with TiO, Ti₂O₃ and TiO₂ coexisting and the root-mean-square (RMS) roughness of the surface is measured to be 8.7 nm. Platelet adhesion experiments show that the adherent platelet on titanium oxide layer is about four times less than that on LTI-carbon. In vivo investigation was performed by implanting LTI-carbon and a titanium oxide layer coated LTI-carbon into the femoral artery of a dog for 4 weeks. By means of scan electron microscopy, coagulation, fibrin, deformed blood red cells and aggregation of adherent platelet were found on the surface of the uncoated LTI-carbon, whereas, nothing but a few normal-shaped blood red cells were found on the titanium oxide coated LTI-carbon. It can be concluded that titanium oxide coated LTI-carbon has a much better blood compatibility than that of the LTI-carbon.     

Laser surface modification of titanium substrate for pulsed laser deposition of highly adherent hydroxyapatite

Biomedical implant devices made out of titanium and its alloys are benefited by a modified surface or a bioactive coating to enhance bone bonding ability and to function effectively in vivo for the intended period of time. In this respect hydroxyapatite coating developed through pulsed laser deposition is a promising approach. Since the success of the bioactive ceramic coated implant depends mainly on the substrate-coating strength; an attempt has been made to produce micro patterned surface structure on titanium substrate for adherent hydroxyapatite coating. A pulsed Nd-YAG laser beam (355 nm) with 10 Hz repetition rate was used for surface treatment of titanium as well as hydroxyapatite deposition. The unfocussed laser beam was used to modify the substrate surface with 500–18,000 laser pulses while keeping the polished substrate in water. Hydroxyapatite deposition was done in a vacuum deposition chamber at 400°C with the focused laser beam under 1 × 10⁻³ mbar oxygen pressure. Deposits were analyzed to understand the physico-chemical, morphological and mechanical characteristics. The obtained substrate and coating surface morphology indicates that laser treatment method can provide controlled micro-topography. Scratch test analysis and microindentation hardness values of coating on laser treated substrate indicate higher mechanical adhesion with respect to coatings on untreated substrates.     

The effects of polishing methods on surface morphology,roughness and bacterial colonisation of titanium abutments

Bacterial colonisation of exposed implant and abutment surfaces can lead to peri-implantitis, a common cause of oral implant failure. When an abutment becomes exposed in the oral environment the typical recommendation is to debride it, to obtain a smoother surface which might be expected to reduce bacterial colonisation. The aim of this study was to evaluate, in vitro, a conventional polishing protocol (PP1) and a simplified polishing protocol (PP2), suggested to have advantages over PP1. The surface morphology and roughness of titanium abutments were characterised at each stage of polishing, and adhesion of oral bacteria was evaluated, using atomic force microscopy, environmental scanning electron microscopy and optical profilometry. PP1 and PP2 methodologies resulted in indistinguishable surface finishes, with fewer scratches than the unmodified surface, and equal roughness values. PP2 resulted in less disruption and less removal of surface material. Early biofilm formation by Streptococcus mutans was reduced on surfaces polished using PP2, but not PP1. Biofilms of Actinomyces naeslundii were more extensive on polished abutment surfaces. Simplified protocol PP2 may be preferable to conventional protocol PP1, since less material is removed, and there is less chance of rough areas remaining. Polishing, however, does not necessarily reduce oral bacterial colonisation.     

Corrosion behaviour of single (Ti) and duplex (Ti–TiO2) coating on 304L stainless steel in nitric acid medium

Sputter deposited single titanium (Ti) layer, and duplex Ti–TiO₂ coating on austenitic type 304L stainless steel (SS) was prepared, and the corrosion performance was evaluated in nitric acid medium using surface morphological and electrochemical techniques. Morphological analysis using atomic force microscope of the duplex Ti–TiO₂ coated surface showed minimization of structural heterogeneities as compared to single Ti layer coating. The electrochemical corrosion results revealed that, titanium coated 304L SS showed moderate to marginal improvement in corrosion resistance in 1 M, and 8 M nitric acid, respectively. Duplex Ti–TiO₂ coated 304L SS specimens showed improved corrosion resistance as compared to Ti coating from dilute (1 M) to concentrated medium (8 M). The percentage of protection efficiency for base material increases significantly for duplex Ti–TiO₂ coating as compared to single Ti layer coating. The oxidizing ability of nitric acid on both the coatings as well as factors responsible for improvement in protection efficiency are discussed and highlighted in this paper.