Shadow-casted ultrathin surface coatings of titanium and titanium/silicon oxide sol particles via ultrasound-assisted deposition.

PubMed

Karahan, H Enis; Birer, Özgür; Karakuş, Kerem; Yıldırım, Cansu

2016-07-01

Ultrasound-assisted deposition (USAD) of sol nanoparticles enables the formation of uniform and inherently stable thin films. However, the technique still suffers in coating hard substrates and the use of fast-reacting sol-gel precursors still remains challenging. Here, we report on the deposition of ultrathin titanium and titanium/silicon hybrid oxide coatings using hydroxylated silicon wafers as a model hard substrate. We use acetic acid as the catalyst which also suppresses the reactivity of titanium tetraisopropoxide while increasing the reactivity of tetraethyl orthosilicate through chemical modifications. Taking the advantage of this peculiar behavior, we successfully prepared titanium and titanium/silicon hybrid oxide coatings by USAD. Varying the amount of acetic acid in the reaction media, we managed to modulate thickness and surface roughness of the coatings in nanoscale. Field-emission scanning electron microscopy and atomic force microscopy studies showed the formation of conformal coatings having nanoroughness. Quantitative chemical state maps obtained by x-ray photoelectron spectroscopy (XPS) suggested the formation of ultrathin (<10nm) coatings and thickness measurements by rotating analyzer ellipsometry supported this observation. For the first time, XPS chemical maps revealed the transport effect of ultrasonic waves since coatings were directly cast on rectangular substrates as circular shadows of the horn with clear thickness gradient from the center to the edges. In addition to the progress made in coating hard substrates, employing fast-reacting precursors and achieving hybrid coatings; this report provides the first visual evidence on previously suggested "acceleration and smashing" mechanism as the main driving force of USAD. Copyright © 2016 Elsevier B.V. All rights reserved.

RF magnetron sputtering of a hydroxyapatite target: A comparison study on polytetrafluorethylene and titanium substrates

NASA Astrophysics Data System (ADS)

Surmenev, Roman A.; Surmeneva, Maria A.; Grubova, Irina Yu.; Chernozem, Roman V.; Krause, Bärbel; Baumbach, Tilo; Loza, Kateryna; Epple, Matthias

2017-08-01

A pure hydroxyapatite (HA) target was used to prepare the biocompatible coating of HA on the surface of a polytetrafluorethylene (PTFE) substrate, which was placed on the same substrate holder with technically pure titanium (Ti) in the single deposition runs by radio-frequency (RF) magnetron sputtering. The XPS, XRD and FTIR analyses of the obtained surfaces showed that for all substrates, instead of the HA coating deposition, the coating of a mixture of calcium carbonate and calcium fluoride was grown. According to SEM investigations, the surface of PTFE was etched, and the surface topography of uncoated Ti was preserved after the depositions. The FTIR results reveal no phosphate bonds; only calcium tracks were observed in the EDX-spectra on the surface of the coated PTFE substrates. Phosphate oxide (V), which originated from the target, could be removed using a vacuum pump system, or no phosphate-containing bonds could be formed on the substrate surface because of the severe substrate bombardment process, which prevented the HA coating deposition. The observed results may be connected with the surface re-sputtering effect of the growing film by high-energy negatively charged ions (most probably oxygen or fluorine), which are accelerated in the cathode dark sheath.

In vitro apatite formation on nano-crystalline titania layer aligned parallel to Ti6Al4V alloy substrates with sub-millimeter gap.

PubMed

Hayakawa, Satoshi; Matsumoto, Yuko; Uetsuki, Keita; Shirosaki, Yuki; Osaka, Akiyoshi

2015-06-01

Pure titanium substrates were chemically oxidized with H2O2 and subsequent thermally oxidized at 400 °C in air to form anatase-type titania layer on their surface. The chemically and thermally oxidized titanium substrate (CHT) was aligned parallel to the counter specimen such as commercially pure titanium (cpTi), titanium alloy (Ti6Al4V) popularly used as implant materials or Al substrate with 0.3-mm gap. Then, they were soaked in Kokubo's simulated body fluid (SBF, pH 7.4, 36.5 °C) for 7 days. XRD and SEM analysis showed that the in vitro apatite-forming ability of the contact surface of the CHT specimen decreased in the order: cpTi > Ti6Al4V > Al. EDX and XPS surface analysis showed that aluminum species were present on the contact surface of the CHT specimen aligned parallel to the counter specimen such as Ti6Al4V and Al. This result indicated that Ti6Al4V or Al specimens released the aluminum species into the SBF under the spatial gap. The released aluminum species might be positively or negatively charged in the SBF and thus can interact with calcium or phosphate species as well as titania layer, causing the suppression of the primary heterogeneous nucleation and growth of apatite on the contact surface of the CHT specimen under the spatial gap. The diffusion and adsorption of aluminum species derived from the half-sized counter specimen under the spatial gap resulted in two dimensionally area-selective deposition of apatite particles on the contact surfaces of the CHT specimen.

Ultrasound assisted deposition of silica coatings on titanium

NASA Astrophysics Data System (ADS)

Kaş, Recep; Ertaş, Fatma Sinem; Birer, Özgür

2012-10-01

We present a novel ultrasound assisted method for silica coating of titanium surfaces. The coatings are formed by “smashing” silica nanoparticles onto activated titanium surface in solution using intense ultrasonic field. Homogeneous silica coatings are formed by deposition of dense multiple layers of silica nanoparticles. Since the nanoparticles also grow during the reaction, the layers of the coatings have smaller particles on the substrate and larger particles towards the surface. The thickness of the coatings can be controlled with several experimental parameters. Silica layers with thickness over 200 nm are readily obtained.

Oxygen plasma ashing effects on aluminum and titanium space protective coatings

NASA Technical Reports Server (NTRS)

Synowicki, R.; Kubik, R. D.; Hale, J. S.; Peterkin, Jane; Nafis, S.; Woollam, John A.; Zaat, S.

1991-01-01

Using variable angle spectroscopic ellipsometry and atomic force microscopy (AFM), the surface roughness and oxidation of aluminum and titanium thin films have been studied as a function of substrate deposition temperature and oxygen plasma exposure. Increasing substrate deposition temperatures affect film microstructure by greatly increasing grain size. Short exposures to an oxygen plasma environment produce sharp spikes rising rapidly above the surface as seen by AFM. Ellipsometric measurements were made over a wide range of plasma exposure times, and results at longer exposure times suggest that the surface is greater than 30% void. This is qualitatively verified by the AFM images.

Grafting strategy to develop single site titanium on an amorphous silica surface.

PubMed

Capel-Sanchez, M C; Blanco-Brieva, G; Campos-Martin, J M; de Frutos, M P; Wen, W; Rodriguez, J A; Fierro, J L G

2009-06-16

Titanium/silica systems were prepared by grafting a titanium alkoxide (titanium isopropoxide and titanium (triethanolaminate) isopropoxide) precursor onto amorphous silica. The grafting process, which consisted of the hydrolysis of the Ti precursor by the hydroxyl groups on the silica surface, yielded samples containing Ti-loadings of 1-1.6 wt %. The as synthesized and calcined TiO(2)-SiO(2) samples were characterized by UV-vis, FTIR, XPS, and XANES spectroscopic techniques. These systems were tested in the liquid-phase epoxidation of oct-1-ene with hydrogen peroxide reaction. Spectroscopic data indicated that titanium anchoring takes place by reaction between the alkoxide precursor and surface OH groups of the silica substrate. The nature of surface titanium species generated by chemical grafting depends largely on the titanium precursor employed. Thus, the titanium isopropoxide precursor yields tetrahedrally coordinated polymeric titanium species, which give rise to a low-efficiency catalyst. However, if an atrane precursor (titanium (triethanolaminate) isopropoxide) is employed, isolated titanium species are obtained. The fact that these species remain isolated even after calcination is due to the protective effect of the triethanolaminate ligand that avoids titanium polymerization. These differences in the titanium environment have a pivotal role in the performance of these systems in the epoxidation of alkenes with hydrogen peroxide.

Grafting Strategy to Develop Single Site Titanium on an Amorphous Silica Surface

DOE Office of Scientific and Technical Information (OSTI.GOV)

Capel-Sanchez, M.; Blanco-Brieva, G; Campos-Martin, J

2009-01-01

Titanium/silica systems were prepared by grafting a titanium alkoxide (titanium isopropoxide and titanium (triethanolaminate) isopropoxide) precursor onto amorphous silica. The grafting process, which consisted of the hydrolysis of the Ti precursor by the hydroxyl groups on the silica surface, yielded samples containing Ti-loadings of 1-1.6 wt %. The as synthesized and calcined TiO2-SiO2 samples were characterized by UV-vis, FTIR, XPS, and XANES spectroscopic techniques. These systems were tested in the liquid-phase epoxidation of oct-1-ene with hydrogen peroxide reaction. Spectroscopic data indicated that titanium anchoring takes place by reaction between the alkoxide precursor and surface OH groups of the silica substrate.more » The nature of surface titanium species generated by chemical grafting depends largely on the titanium precursor employed. Thus, the titanium isopropoxide precursor yields tetrahedrally coordinated polymeric titanium species, which give rise to a low-efficiency catalyst. However, if an atrane precursor (titanium (triethanolaminate) isopropoxide) is employed, isolated titanium species are obtained. The fact that these species remain isolated even after calcination is due to the protective effect of the triethanolaminate ligand that avoids titanium polymerization. These differences in the titanium environment have a pivotal role in the performance of these systems in the epoxidation of alkenes with hydrogen peroxide.« less

Surface XPS characterization of NiTi shape memory alloy after advanced oxidation processes in UV/H 2O 2 photocatalytic system

NASA Astrophysics Data System (ADS)

Wang, R. M.; Chu, C. L.; Hu, T.; Dong, Y. S.; Guo, C.; Sheng, X. B.; Lin, P. H.; Chung, C. Y.; Chu, P. K.

2007-08-01

Surface structure of NiTi shape memory alloy (SMA) was modified by advanced oxidation processes (AOP) in an ultraviolet (UV)/H 2O 2 photocatalytic system, and then systematically characterized with x-ray photoelectron spectroscopy (XPS). It is found that the AOP in UV/H 2O 2 photocatalytic system leads to formation of titanium oxides film on NiTi substrate. Depth profiles of O, Ni and Ti show such a film possesses a graded interface structure to NiTi substrate and there is no intermediate Ni-rich layer like that produced in conventional high temperature oxidation. Except TiO 2 phase, some titanium suboxides (TiO, Ti 2O 3) may also exist in the titanium oxides film. Oxygen mainly presents in metal oxides and some chemisorbed water and OH - are found in titanium oxides film. Ni nearly reaches zero on the upper surface and relatively depleted in the whole titanium oxides film. The work indicates the AOP in UV/H 2O 2 photocatalytic system is a promising way to favor the widespread application of biomedical NiTi SMA by improving its biocompatibility.

Microstructure and corrosion resistance of sputter-deposited titanium-chromium alloy coatings

DOE Office of Scientific and Technical Information (OSTI.GOV)

Landolt, D.; Robyr, C.; Mettraux, P.

1998-10-01

Titanium, chromium, and titanium-chromium alloy coatings were sputter-deposited to study their corrosion behaviors in relation to microstructure and composition. Silicon substrates were used to study the effect of alloying on intrinsic corrosion resistance of the coating materials, and brass substrates were used to study the effect of alloying on the penetrating porosity of the coatings. Corrosion behavior was characterized using linear sweep voltammetry. The crystal structure of the coatings was examined by x-ray diffraction (XRD) and the microstructure by scanning electron microscopy (SEM). Electrochemical impedance spectroscopy (EIS) was used to estimate the real surface area of the coatings. Results showedmore » alloying of titanium with chromium greatly influenced microstructure of the coatings. Alloying led to deposits of higher apparent density and, in some cases, to an x-ray amorphous structure. Alloy coatings showed significantly lower corrosion currents than the constituting metals. The effect was attributed to a smoother surface topography. When corrected of differences in real surface area, the intrinsic corrosion rate of the alloy coatings did not differ significantly from that of the constituting metals. Alloy coatings deposited on brass exhibited a lower porosity than titanium or chromium metal coatings produced under identical conditions.« less

Fundamental Study on One-Dimensional-Array Medical Ultrasound Probe with Piezoelectric Polycrystalline Film by Hydrothermal Method: Experimental Fabrication of One-Dimensional-Array Ultrasound Probe

NASA Astrophysics Data System (ADS)

Endo, Akito; Kawashima, Norimichi; Takeuchi, Shinichi; Ishikawa, Mutsuo; Kurosawa, Minoru Kuribayashi

2007-07-01

We deposited a lead zirconate titanete (PZT) polycrystalline film on a titanium substrate by the hydrothermal method and fabricated a transducer using the PZT film for use as an ultrasound probe. A 10 MHz miniature one-dimensional-array medical ultrasound probe containing the PZT film was developed. After sputtering titanium on the surface of a hydroxyapatite substrate, the titanium film on the substrate was etched by the photolithography to form a one-dimensional titanium film electrode array. We could thus fabricate a miniature one-dimensional-array ultrasound probe by the hydrothermal method. Transmitted ultrasound pulses from a 10 MHz commercial ultrasound probe were received by the newly fabricated one-dimensional-array ultrasound probe. The fabrication process of the probe and the results of experiments on receiving waveforms were reported in this paper.

Cleaning of titanium substrates after application in a bioreactor.

PubMed

Fingerle, Mathias; Köhler, Oliver; Rösch, Christina; Kratz, Fabian; Scheibe, Christian; Davoudi, Neda; Müller-Renno, Christine; Ziegler, Christiane; Huster, Manuel; Schlegel, Christin; Ulber, Roland; Bohley, Martin; Aurich, Jan C

2015-03-10

Plain and microstructured cp-titanium samples were studied as possible biofilm reactor substrates. The biofilms were grown by exposition of the titanium samples to bacteria in a flow cell. As bacteria the rod shaped gram negative Pseudomonas fluorescens and the spherical gram negative Paracoccus seriniphilus were chosen. Afterward, the samples were cleaned in subsequent steps: First, with a standard solvent based cleaning procedure with acetone, isopropanol, and ultrapure water and second by oxygen plasma sputtering. It will be demonstrated by means of x-ray photoelectron spectroscopy, fluorescence microscopy, and confocal laser scanning microscopy that oxygen plasma cleaning is a necessary and reliant tool to fully clean and restore titanium surfaces contaminated with a biofilm. The microstructured surfaces act beneficial to biofilm growth, while still being fully restorable after biofilm contamination. Scanning electron microscopy images additionally show, that the plasma process does not affect the microstructures. The presented data show the importance of the cleaning procedure. Just using solvents does not remove the biofilm and all its components reliably while a cleaning process by oxygen plasma regenerates the surfaces.

Formation of Titania Submicron-Scale Rod Arrays on Titanium Substrate and In Vitro Biocompatibility

DTIC Science & Technology

2005-01-01

vitro bioactivity. INTRODUCTION Commercially available pure titanium (c.p. Ti) and its alloys are widely used for dental and orthopedic implants because...days. DISCUSSION The submicron-scale rod arrays of rutile can be obtained on titanium surfaces after the heat treatment when the alkali- borate glass ...modification of titanium implants have been already developed or proposed to provide them with the ability of direct bonding to bone tissues. Note

The promotion of osseointegration of titanium surfaces by coating with silk protein sericin.

PubMed

Nayak, Sunita; Dey, Tuli; Naskar, Deboki; Kundu, Subhas C

2013-04-01

A promising strategy to influence the osseointegration process around orthopaedic titanium implants is the immobilization of bioactive molecules. This recruits appropriate interaction between the surface and the tissue by directing cells adhesion, proliferation, differentiation and active matrix remodelling. In this study, we aimed to investigate the functionalization of metallic implant titanium with silk protein sericin. Titanium surface was immobilized with non-mulberry Antheraea mylitta sericin using glutaraldehyde as crosslinker. To analyse combinatorial effects the sericin immobilized titanium was further conjugated with integrin binding peptide sequence Arg-Gly-Asp (RGD) using ethyl (dimethylaminopropyl) carbodiimide and N-hydroxysulfosuccinimide as coupling agents. The surface of sericin immobilized titanium was characterized biophysically. Osteoblast-like cells were cultured on sericin and sericin/RGD functionalized titanium and found to be more viable than those on pristine titanium. The enhanced adhesion, proliferation, and differentiation of osteoblast cells were observed. RT-PCR analysis showed that mRNA expressions of bone sialoprotein, osteocalcin and alkaline phosphatase were upregulated in osteoblast cells cultured on sericin and sericin/RGD immobilized titanium substrates. Additionally, no significant amount of pro-inflammatory cytokines TNF-α, IL-1β and nitric oxide production were recorded when macrophages cells and osteoblast-macrophages co culture cells were grown on sericin immobilized titanium. The findings demonstrate that the sericin immobilized titanium surfaces are potentially useful bioactive coated materials for titanium-based medical implants. Copyright © 2013 Elsevier Ltd. All rights reserved.

Titanium Surface Priming with Phase-Transited Lysozyme to Establish a Silver Nanoparticle-Loaded Chitosan/Hyaluronic Acid Antibacterial Multilayer via Layer-by-Layer Self-Assembly.

PubMed

Zhong, Xue; Song, Yunjia; Yang, Peng; Wang, Yao; Jiang, Shaoyun; Zhang, Xu; Li, Changyi

2016-01-01

The formation of biofilm around implants, which is induced by immediate bacterial colonization after installation, is the primary cause of post-operation infection. Initial surface modification is usually required to incorporate antibacterial agents on titanium (Ti) surfaces to inhibit biofilm formation. However, simple and effective priming methods are still lacking for the development of an initial functional layer as a base for subsequent coatings on titanium surfaces. The purpose of our work was to establish a novel initial layer on Ti surfaces using phase-transited lysozyme (PTL), on which multilayer coatings can incorporate silver nanoparticles (AgNP) using chitosan (CS) and hyaluronic acid (HA) via a layer-by-layer (LbL) self-assembly technique. In this study, the surfaces of Ti substrates were primed by dipping into a mixture of lysozyme and tris(2-carboxyethyl)phosphine (TCEP) to obtain PTL-functionalized Ti substrates. The subsequent alternating coatings of HA and chitosan loaded with AgNP onto the precursor layer of PTL were carried out via LbL self-assembly to construct multilayer coatings on Ti substrates. The results of SEM and XPS indicated that the necklace-like PTL and self-assembled multilayer were successfully immobilized on the Ti substrates. The multilayer coatings loaded with AgNP can kill planktonic and adherent bacteria to 100% during the first 4 days. The antibacterial efficacy of the samples against planktonic and adherent bacteria achieved 65%-90% after 14 days. The sustained release of Ag over 14 days can prevent bacterial invasion until mucosa healing. Although the AgNP-containing structure showed some cytotoxicity, the toxicity can be reduced by controlling the Ag release rate and concentration. The PTL priming method provides a promising strategy for fabricating long-term antibacterial multilayer coatings on titanium surfaces via the LbL self-assembly technique, which is effective in preventing implant-associated infections in the early stage.

Hydroxyapatite coating of titanium implants using hydroprocessing and evaluation of their osteoconductivity.

PubMed

Kuroda, Kensuke; Okido, Masazumi

2012-01-01

Many techniques for the surface modification of titanium and its alloys have been proposed from the viewpoint of improving bioactivity. This paper contains an overview of surface treatment methods, including coating with hydroxyapatite (HAp), an osteoconductive compound. There are two types of coating methods: pyroprocessing and hydroprocessing. In this paper, hydroprocessing for coating on the titanium substrate with HAp, carbonate apatite (CO(3)-Ap), a CO(3)-Ap/CaCO(3) composite, HAp/collagen, and a HAp/gelatin composite is outlined. Moreover, evaluation by implantation of surface-modified samples in rat tibiae is described.

Hydroxyapatite Coating of Titanium Implants Using Hydroprocessing and Evaluation of Their Osteoconductivity

PubMed Central

Kuroda, Kensuke; Okido, Masazumi

2012-01-01

Many techniques for the surface modification of titanium and its alloys have been proposed from the viewpoint of improving bioactivity. This paper contains an overview of surface treatment methods, including coating with hydroxyapatite (HAp), an osteoconductive compound. There are two types of coating methods: pyroprocessing and hydroprocessing. In this paper, hydroprocessing for coating on the titanium substrate with HAp, carbonate apatite (CO3–Ap), a CO3–Ap/CaCO3 composite, HAp/collagen, and a HAp/gelatin composite is outlined. Moreover, evaluation by implantation of surface-modified samples in rat tibiae is described. PMID:22400015

Inherent substrate-dependent growth initiation and selective-area atomic layer deposition of TiO{sub 2} using “water-free” metal-halide/metal alkoxide reactants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Atanasov, Sarah E.; Kalanyan, Berç; Parsons, Gregory N., E-mail: gnp@ncsu.edu

2016-01-15

Titanium dioxide atomic layer deposition (ALD) is shown to proceed selectively on oxidized surfaces with minimal deposition on hydrogen-terminated silicon using titanium tetrachloride (TiCl{sub 4}) and titanium tetra-isopropoxide [Ti(OCH(CH{sub 3}){sub 2}){sub 4}, TTIP] precursors. Ex situ x-ray photoelectron spectroscopy shows a more rapid ALD nucleation rate on both Si–OH and Si–H surfaces when water is the oxygen source. Eliminating water delays the oxidation of the hydrogen-terminated silicon, thereby impeding TiO{sub 2} film growth. For deposition at 170 °C, the authors achieve ∼2 nm of TiO{sub 2} on SiO{sub 2} before substantial growth takes place on Si–H. On both Si–H and Si–OH, themore » surface reactions proceed during the first few TiCl{sub 4}/TTIP ALD exposure steps where the resulting products act to impede subsequent growth, especially on Si–H surfaces. Insight from this work helps expand understanding of “inherent” substrate selective ALD, where native differences in substrate surface reaction chemistry are used to promote desired selective-area growth.« less

High power RF window deposition apparatus, method, and device

DOEpatents

Ives, Lawrence R.; Lucovsky, Gerald; Zeller, Daniel

2017-07-04

A process for forming a coating for an RF window which has improved secondary electron emission and reduced multipactor for high power RF waveguides is formed from a substrate with low loss tangent and desirable mechanical characteristics. The substrate has an RPAO deposition layer applied which oxygenates the surface of the substrate to remove carbon impurities, thereafter has an RPAN deposition layer applied to nitrogen activate the surface of the substrate, after which a TiN deposition layer is applied using Titanium tert-butoxide. The TiN deposition layer is capped with a final RPAN deposition layer of nitridation to reduce the bound oxygen in the TiN deposition layer. The resulting RF window has greatly improved titanium layer adhesion, reduced multipactor, and is able to withstand greater RF power levels than provided by the prior art.

Enhanced-Adhesion Multi-Walled Carbon Nanotubes on Titanium Substrates for Stray Light Control

NASA Technical Reports Server (NTRS)

Hagopian, John; Getty, Stephanie; Quijada, Manuel

2012-01-01

Carbon nanotubes previously grown on silicon have extremely low reflectance, making them a good candidate for stray light suppression. Silicon, however, is not a good structural material for stray light components such as tubes, stops, and baffles. Titanium is a good structural material and can tolerate the 700 C nanotube growth process. The ability to grow carbon nanotubes on a titanium substrate that are ten times blacker than the current NASA state-of-the-art paints in the visible to near infrared spectra has been achieved. This innovation will allow significant improvement of stray light performance in scientific instruments or any other optical system. This innovation is a refinement of the utilization of multiwalled carbon nano tubes for stray light suppression in spaceflight instruments. The innovation is a process to make the surface darker and improve the adhesion to the substrate, improving robustness for spaceflight use. Bright objects such as clouds or ice scatter light off of instrument structures and components and make it difficult to see dim objects in Earth observations. A darker material to suppress this stray light has multiple benefits to these observations, including enabling scientific observations not currently possible, increasing observational efficiencies in high-contrast scenes, and simplifying instruments and lowering their cost by utilizing fewer stray light components and achieving equivalent performance. The prior art was to use commercially available black paint, which resulted in approximately 4% of the light being reflected (hemispherical reflectance or total integrated scatter, or TIS). Use of multiwalled carbon nanotubes on titanium components such as baffles, entrance aperture, tubes, and stops, can decrease this scattered light by a factor of ten per bounce over the 200-nm to 2,500-nm wavelength range. This can improve system stray light performance by orders of magnitude. The purpose of the innovation is to provide an enhanced stray light control capability by making a blacker surface treatment for typical stray light control components. Since baffles, stops, and tubes used in scientific observations often undergo loads such as vibration, it was critical to develop this surface treatment on structural materials. The innovation is to optimize the carbon nanotube growth for titanium, which is a strong, lightweight structural material suitable for spaceflight use. The titanium substrate carbon nanotubes are more robust than those grown on silicon and allow for easier utilization. They are darker than current surface treatments over larger angles and larger wavelength range. The primary advantage of titanium substrate is that it is a good structural material, and not as brittle as silicon.

Thin sol-gel-derived silica coatings on dental pure titanium casting.

PubMed

Yoshida, K; Kamada, K; Sato, K; Hatada, R; Baba, K; Atsuta, M

1999-01-01

The sol-gel dipping process, in which liquid silicon alkoxide is transformed into a solid silicon-oxygen network, can produce a thin film coating of silica (SiO(2)). The features of this method are high homogeneity and purity of the thin SiO(2) film and a low sinter temperature, which are important in the preparation of coating films that can protect metallic ion release from the metal substrate and prevent attachment of dental plaque. We evaluated the surface properties of dental pure titanium casting coated with a thin SiO(2) or SiO(2)/F-hybrid film by the sol-gel dipping process. The metal specimens were pretreated by dipping in isopropylalcohol solution containing 10 wt% 3-aminopropyl trimethoxysilane and treated by dipping in the silica precursor solution for 5 min, withdrawal at a speed of 2 mm/min, air-drying for 20 min at room temperature, heating at 120 degrees C for 20 min, and then storing at room temperature. Both SiO(2) and SiO(2)/F films bonded strongly (above 55 MPa) to pure titanium substrate by a tensile test. SiO(2(-)) and SiO(2)/F-coated specimens immersed in 1 wt% of lactic acid solution for two weeks showed significantly less release of titanium ions (30. 5 ppb/cm(2) and 9.5 ppb/cm(2), respectively) from the substrate than noncoated specimens (235.2 ppb/cm(2)). Hydrophobilization of SiO(2(-)) and SiO(2)/F-coated surfaces resulted in significant increases of contact angle of water (81.6 degrees and 105.7 degrees, respectively) compared with noncoated metal specimens (62.1 degrees ). The formation of both thin SiO(2) and SiO(2)/F-hybrid films by the sol-gel dipping process on the surface of dental pure titanium casting may be useful clinically in enhancing the bond strength of dental resin cements to titanium, preventing titanium ions release from the substrate, and reducing the accumulation of dental plaque attaching to intraoral dental restorations. Copyright 1999 John Wiley & Sons, Inc.

The influence of surface roughness and high pressure torsion on the growth of anodic titania nanotubes on pure titanium

NASA Astrophysics Data System (ADS)

Hu, Nan; Gao, Nong; Starink, Marco J.

2016-11-01

Anodic titanium dioxide nanotube (TNT) arrays have wide applications in photocatalytic, catalysis, electronics, solar cells and biomedical implants. When TNT coatings are combined with severe plastic deformation (SPD), metal processing techniques which efficiently improve the strength of metals, a new generation of biomedical implant is made possible with both improved bulk and surface properties. This work investigated the effect of processing by high pressure torsion (HPT) and different mechanical preparations on the substrate and subsequently on the morphology of TNT layers. HPT processing was applied to refine the grain size of commercially pure titanium samples and substantially improved their strength and hardness. Subsequent anodization at 30 V in 0.25 wt.% NH4F for 2 h to form TNT layers on sample surfaces prepared with different mechanical preparation methods was carried out. It appeared that the local roughness of the titanium surface on a microscopic level affected the TNT morphology more than the macroscopic surface roughness. For HPT-processed sample, the substrate has to be pre-treated by a mechanical preparation finer than 4000 grit for HPT to have a significant influence on TNTs. During the formation of TNT layers the oxide dissolution rate was increased for the ultrafine-grained microstructure formed due to HPT processing.

Spontaneous Differentiation of Dental Pulp stem cells on Dental polymers

NASA Astrophysics Data System (ADS)

Bherwani, Aneel; Suarato, Giulia; Qin, Sisi; Chang, Chung-Cheh; Akhavan, Aaron; Spiegel, Joseph; Jurukovski, Vladimir; Rafailovich, Miriam; Simon, Marcia

2012-02-01

Dental pulp stem cells were plated on two dentally relevant materials i.e. PMMA commonly used for denture and Titanium used for implants. In both cases, we probed for the role of surface interaction and substrate morphology. Different films of PMMA were spun cast directly onto Si wafers; PMMA fibers of different diameters were electro spun onto some of these substrates. Titanium metal was evaporated onto Si surfaces using an electron beam evaporator. In addition, on some surfaces, P4VP nanofibers were spun cast. DPSC were grown in alpha-MEM supplemented with 10% fetal bovine serum, 0.2mM L-ascorbic acid 2-phosphate, 2mm glutamine and 10mM beta-glycerol phosphate either with or without 10nM dexamethasone. After 21 days samples were examined using confocal microscopy of cells and by scanning electron microscopy (SEM) and Energy dispersive X-ray Analysis (EDAX). In the case of Titanium biomineralization was observed independent of dexamethasone, where the deposits were templated along the fibers. Minimal biomineralization was observed on flat Titanium and PMMA samples. Markers of osteogenesis and specific signaling pathways are being evaluated by RT-PCR, which are up regulated on each surface, to understand the fundamental manner in which surfaces interact with cell differentiation.

Femtosecond laser-induced periodic surface structures on titanium nitride coatings for tribological applications

NASA Astrophysics Data System (ADS)

Bonse, J.; Kirner, S. V.; Koter, R.; Pentzien, S.; Spaltmann, D.; Krüger, J.

2017-10-01

Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces.

Self-organized nickel nanoparticles on nanostructured silicon substrate intermediated by a titanium oxynitride (TiNxOy) interface

NASA Astrophysics Data System (ADS)

Morales, M.; Droppa, R., Jr.; de Mello, S. R. S.; Figueroa, C. A.; Zanatta, A. R.; Alvarez, F.

2018-01-01

In this work we report an experimental approach by combining in situ sequential top-down and bottom-up processes to induce the organization of nanosized nickel particles. The top-down process consists in xenon ion bombardment of a crystalline silicon substrate to generate a pattern, followed by depositing a ˜15 nm titanium oxynitride thin film to act as a metallic diffusion barrier. Then, metallic nanoparticles are deposited by argon ion sputtering a pure nickel target, and the sample is annealed to promote the organization of the nickel nanoparticles (a bottom-up process). According to the experimental results, the surface pattern and the substrate biaxial surface strain are the driving forces behind the alignment and organization of the nickel nanoparticles. Moreover, the ratio between the F of metallic atoms arriving at the substrate relative to its surface diffusion mobility determines the nucleation regime of the nickel nanoparticles. These features are presented and discussed considering the existing technical literature on the subject.

Pulsed Laser Deposition Processing of Improved Titanium Nitride Coatings for Implant Applications

NASA Astrophysics Data System (ADS)

Haywood, Talisha M.

Recently surface coating technology has attracted considerable attention of researchers to develop novel coatings with enhanced functional properties such as hardness, biocompatibility, wear and corrosion resistance for medical devices and surgical tools. The materials currently being used for surgical implants include predominantly stainless steel (316L), cobalt chromium (Co-Cr), titanium and its alloys. Some of the limitations of these implants include improper mechanical properties, corrosion resistance, cytotoxicity and bonding with bone. One of the ways to improve the performance and biocompatibility of these implants is to coat their surfaces with biocompatible materials. Among the various coating materials, titanium nitride (TiN) shows excellent mechanical properties, corrosion resistance and low cytotoxicity. In the present work, a systematic study of pulsed laser ablation processing of TiN coatings was conducted. TiN thin film coatings were grown on commercially pure titanium (Ti) and stainless steel (316L) substrates at different substrate temperatures and different nitrogen partial pressures using the pulsed laser deposition (PLD) technique. Microstructural, surface, mechanical, chemical, corrosion and biological analysis techniques were applied to characterize the TiN thin film coatings. The PLD processed TiN thin film coatings showed improvements in mechanical strength, corrosion resistance and biocompatibility when compared to the bare substrates. The enhanced performance properties of the TiN thin film coatings were a result of the changing and varying of the deposition parameters.

Fretting Wear-Resistant, Micro-Arc Oxidation Coatings for Aluminum and Titanium Alloy Bearings (Preprint)

DTIC Science & Technology

2007-03-01

Cushman, Infoscitex Corporation, 303 Bear Hill Road, Waltham, MA 02451 Aluminum and titanium alloys are used as replacements for steel in gear...assess the susceptibility of selected substrates to wear. Initial testing utilized M50 steel rings as the counter surface to uncoated aluminum and...were recorded and plotted over the 4500 cycles, as shown in the right of Figure 3, depicting results of the best performing test substrate, M50 Steel

On the Electrodeposition of Ca-P Coatings on Nitinol Alloy: A Comparison Between Different Surface Modification Methods

NASA Astrophysics Data System (ADS)

Etminanfar, M. R.; Khalil-Allafi, J.

2016-02-01

In this study, a combination of surface modification process and the electrochemical deposition of Ca-P coatings was used for the modification of the Nitinol shape memory alloy. DSC, SEM, GIB-XRD, FT-Raman, XPS, and FTIR measurements were performed for the characterization of the samples. Results indicated that chemical etching and boiling of the samples in distilled water formed TiO film on the surface. After the chemical modification, subsequent aging of the sample, at 470 °C for 30 min, converted the oxide film to a stable structure of titanium dioxide. In that case, the treated substrate indicated a superelastic behavior. At the same electrochemical condition, the treated substrate revealed more stable and uniform Ca-P coatings in comparison with the abraded Nitinol substrate. This difference was attributed to the presence of hydroxyl groups on the titanium dioxide surface. Also, after soaking the sample in SBF, the needle-like coating on the treated substrate was completely covered with the hydroxyapatite phase which shows a good bioactivity of the coating.

Microstructures of plasma-sprayed hydroxyapatite-coated Ti-6Al-4V dental implants.

PubMed

Tufekci, E; Brantley, W A; Mitchell, J C; McGlumphy, E A

1997-01-01

The purpose of this study was to investigate the microstructure of plasma-sprayed hydroxyapatite coatings and the elemental composition near the coating-substrate interface for two commercial implants, using the scanning electron microscope. Both coating surfaces and cross-sectioned specimens were examined. The results indicated that while the surface microstructures of both implants were consistent with the plasma-spraying process, the scale of the constituents was much finer for one product. In cross-section, both coatings exhibited minimal porosity and intimate contact with the titanium alloy substrate. It was found that limited interdiffusion of titanium and calcium occurred near the interface.

Influence of microstructure and chemical composition of sputter deposited TiO2 thin films on in vitro bioactivity.

PubMed

Lilja, Mirjam; Genvad, Axel; Astrand, Maria; Strømme, Maria; Enqvist, Håkan

2011-12-01

Functionalisation of biomedical implants via surface modifications for tailored tissue response is a growing field of research. Crystalline TiO(2) has been proven to be a bone bioactive, non-resorbable material. In contact with body fluids a hydroxyapaptite (HA) layer forms on its surface facilitating the bone contact. Thus, the path of improving biomedical implants via deposition of crystalline TiO(2) on the surface is interesting to follow. In this study we have evaluated the influence of microstructure and chemical composition of sputter deposited titanium oxide thin films on the in vitro bioactivity. We find that both substrate bias, topography and the flow ratio of the gases used during sputtering affect the HA layer formed on the films after immersion in simulated body fluid at 37°C. A random distribution of anatase and rutile crystals, formed at negative substrate bias and low Ar to O(2) gas flow ratios, are shown to favor the growth of flat HA crystal structures whereas higher flow ratios and positive substrate bias induced growth of more spherical HA structures. These findings should provide valuable information when optimizing the bioactivity of titanium oxide coatings as well as for tailoring process parameters for sputtered-based production of bioactive titanium oxide implant surfaces.

Wettability of Thin Silicate-Containing Hydroxyapatite Films Formed by RF-Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Gorodzha, S. N.; Surmeneva, M. A.; Surmenev, R. A.; Gribennikov, M. V.; Pichugin, V. F.; Sharonova, A. A.; Pustovalova, A. A.; Prymack, O.; Epple, M.; Wittmar, A.; Ulbricht, M.; Gogolinskii, K. V.; Kravchuk, K. S.

2014-02-01

Using the methods of electron and atomic force microscopy, X-ray structural analysis and measurements of the wetting angle, the features of morphology, structure, contact angle and free surface energy of silicon-containing calcium-phosphate coatings formed on the substrates made from titanium VT1-0 and stainless steel 12Cr18Ni10Ti are investigated. It is shown that the coating - substrate system possesses bimodal roughness formed by the substrate microrelief and coating nanostructure, whose principal crystalline phase is represented by silicon-substituted hydroxiapatite with the size of the coherent scattering region (CSR) 18-26 nm. It is found out that the formation of a nanostructured coating on the surface of rough substrates makes them hydrophilic. The limiting angle of water wetting for the coatings formed on titanium and steel acquires the values in the following ranges: 90-92 and 101-104°, respectively, and decreases with time.

[Cr-Ti-Al-N complex coating on titanium to strengthen Ti/porcelain bonding].

PubMed

Zhang, Hui; Guo, Tian-wen; Li, Jun-ming; Pan, Jing-guang; Dang, Yong-gang; Tong, Yu

2006-02-01

To study the feasibility of magnetron sputtering Cr-Ti-Al-N complex coating as an interlayer on titanium to enhance the titanium-ceramic binding strength. With a three-point bending test according to ISO 9693, the binding strength of Duceratin (Degussa) to titanium substrate prepared with 4 different surface treatments (polishing, polishing and megnetron sputtering Cr, Ti, Al, and N complex coating, sandblasting, sandblasting and coating) was evaluated. Ti/porcelain interface and fractured Ti surface were examined using scanning electron microscopy with energy-dispersive spectrometry (EDS). The binding strength of polished and coated titanium/Duceratin was significantly higher than polished titanium group (P<0.05). The binding strength of sandblasted and coated titanium/Duceratin did not differ significantly from that of sandblasted titanium group (P>0.05), and the strength in the two sandblasted titanium groups was significantly higher than that in polished and coated titanium group (P<0.05). Megnetron sputtering Cr-Ti-Al-N complex on polished titanium can increase the titanium/porcelain binding strength. Megnetron sputtering coating is a promising Ti/porcelain interlayer.

Carbon Nanotubes on Titanium Substrates for Stray Light Suppression

NASA Technical Reports Server (NTRS)

Hagopian, John; Getty, Stephanie; Quijada, Manuel

2011-01-01

A method has been developed for growing carbon nanotubes on a titanium substrate, which makes the nano tubes ten times blacker than the current state-of-the-art paints in the visible to near infrared. This will allow for significant improvement of stray light performance in scientific instruments, or any other optical system. Because baffles, stops, and tubes used in scientific observations often undergo loads such as vibration, it is critical to develop this surface treatment on structural materials. This innovation optimizes the carbon nano - tube growth for titanium, which is a strong, lightweight structural material suitable for spaceflight use. The steps required to grow the nanotubes require the preparation of the surface by lapping, and the deposition of an iron catalyst over an alumina stiction layer by e-beam evaporation. In operation, the stray light controls are fabricated, and nanotubes (multi-walled 100 microns in length) are grown on the surface. They are then installed in the instruments or other optical devices.

Effect of substrate surface treatment on electrochemically assisted photocatalytic activity of N-S co-doped TiO2 films

NASA Astrophysics Data System (ADS)

Parada-Gamboa, N. J.; Pedraza-Avella, J. A.; Meléndez, A. M.

2017-01-01

To investigate whether different metal surface treatments, performed on meshes of stainless steel 304 and titanium, affect the photocatalytic activity (PCA) of supported modified anodic TiO2 films, metallic substrates were coated with titanium isopropoxide sol-gel precursor modified with thiourea. Substrates were pretreated by some of the following techniques: a) sandblasting, b) pickling, c) hydroxylation and d) passivation. The as-prepared electrode materials were characterized by X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), and voltammetry in the dark and under light UVA irradiation. PCA of modified N-S-TiO2 electrodes was evaluated by electrochemically assisted photocatalytic degradation of methyl orange. The results of XPS revealed that N and S were incorporated into the lattice of TiO2. FESEM showed that surface roughness and thickness of films varies depending on surface treatment. Voltammetric and XPS characterization of N-S co-doped TiO2 films supported on stainless steel revealed that their surface contains alpha-Fe2O3/FeOOH. Accordingly, iron contamination of the films coming from stainless steel was detrimental to the degradation of methyl orange. Prior to sol-gel coating process, sandblasting followed by nitric acid passivation for stainless steel or hydrofluoric acid pickling process in the case of titanium improved the PCA of N-S co-doped TiO2 films.

Laser induced single spot oxidation of titanium

NASA Astrophysics Data System (ADS)

Jwad, Tahseen; Deng, Sunan; Butt, Haider; Dimov, S.

2016-11-01

Titanium oxides have a wide range of applications in industry, and they can be formed on pure titanium using different methods. Laser-induced oxidation is one of the most reliable methods due to its controllability and selectivity. Colour marking is one of the main applications of the oxidation process. However, the colourizing process based on laser scanning strategies is limited by the relative large processing area in comparison to the beam size. Single spot oxidation of titanium substrates is proposed in this research in order to increase the resolution of the processed area and also to address the requirements of potential new applications. The method is applied to produce oxide films with different thicknesses and hence colours on titanium substrates. High resolution colour image is imprinted on a sheet of pure titanium by converting its pixels' colours into laser parameter settings. Optical and morphological periodic surface structures are also produced by an array of oxide spots and then analysed. Two colours have been coded into one field and the dependencies of the reflected colours on incident and azimuthal angles of the light are discussed. The findings are of interest to a range of application areas, as they can be used to imprint optical devices such as diffusers and Fresnel lenses on metallic surfaces as well as for colour marking.

Controlled release of chlorhexidine antiseptic from microporous amorphous silica applied in open porosity of an implant surface.

PubMed

Verraedt, Els; Braem, Annabel; Chaudhari, Amol; Thevissen, Karin; Adams, Erwin; Van Mellaert, Lieve; Cammue, Bruno P A; Duyck, Joke; Anné, Jozef; Vleugels, Jef; Martens, Johan A

2011-10-31

Amorphous microporous silica (AMS) serving as a reservoir for controlled release of a bioactive agent was applied in the open porosity of a titanium coating on a Ti-6Al-4V metal substrate. The pores of the AMS emptied by calcination were loaded with chlorhexidine diacetate (CHX) via incipient wetness impregnation with CHX solution, followed by solvent evaporation. Using this CHX loaded AMS system on titanium substrate sustained release of CHX into physiological medium was obtained over a 10 day-period. CHX released from the AMS coating was demonstrated to be effective in killing planktonic cultures of the human pathogens Candida albicans and Staphylococcus epidermidis. This surface modification of titanium bodies with AMS controlled release functionality for a bioactive compound potentially can be applied on dental and orthopaedic implants to abate implant-associated microbial infection. Copyright © 2011 Elsevier B.V. All rights reserved.

Thin calcium phosphate coatings on titanium by electrochemical deposition in modified simulated body fluid.

PubMed

Peng, Ping; Kumar, Sunil; Voelcker, Nicolas H; Szili, Endre; Smart, Roger St C; Griesser, Hans J

2006-02-01

Adherent and optically semitransparent thin calcium phosphate (CaP) films were electrochemically deposited on titanium substrates in a modified simulated body fluid at 37 degrees C. Coatings deposited by using periodic pulsed potentials showed better adhesion and better mechanical properties than coatings deposited with use of a constant potential. Scanning electron microscopy was used to study the morphology of the coatings. The coatings displayed a polydispersed porous structure with pores in the range of a few nanometers to 1 mum. Furthermore, X-ray diffractometry and the O(1s) satellite peaks in X-ray photoelectron spectroscopy indicated that the coatings possessed a similar surface chemistry to that of natural bone minerals. These results were confirmed by inductively coupled plasma optical emission spectrometry, which yielded a Ca:P ratio of 1.65, close to that of hydroxyapatite. Contact mode atomic force microscopy (AFM) showed the average thickness of the coatings was in the order of 200 nm. Root-mean-square (RMS) roughness values, also derived by AFM, were shown to be much higher on the titanium-CaP surfaces in comparison with untreated titanium substrates, with RMS values of about 300 and 110 nm, respectively. Cell culture experiments showed that the CaP surfaces are nontoxic to MG63 osteoblastic cells in vitro and were able to support cell growth for up to 4 days, outperforming the untreated titanium surface in a direct comparison. These easily prepared coatings show promise for hard-tissue biomaterials. (c) 2005 Wiley Periodicals, Inc.

Ultraviolet-Diode Pump Solid State Laser Removal of Titanium Aluminium Nitride Coating from Tungsten Carbide Substrate

NASA Astrophysics Data System (ADS)

See, Tian Long; Chantzis, Dimitrios; Royer, Raphael; Metsios, Ioannis; Antar, Mohammad; Marimuthu, Sundar

2017-09-01

This paper presents an investigation on the titanium aluminium nitride (TiAlN) coating removal from tungsten carbide (WC-Co) substrate using a diode pump solid state (DPSS) ultraviolet (UV) laser with maximum average power of 90 W, wavelength of 355 nm and pulse width of 50 ns. The TiAlN coating of 1.5 μm thickness is removed from the WC-Co substrate with laser fluence of 2.71 J/cm2 at 285.6 number of pulses (NOP) and with NOP of 117.6 at 3.38 J/cm2 fluence. Titanium oxide formation was observed on the ablated surface due to the re-deposition of ablated titanium residue and also attributed to the high temperature observed during the laser ablation process. Crack width of around 0.2 μm was observed over both TiAlN coating and WC-Co substrate. The crack depth ranging from 1 to 10 μm was observed and is related to the thickness of the melted carbide. The crack formation is a result of the thermal induced stresses caused by the laser beam interaction with the material as well as the higher thermal conductivity of cobalt compared to WC. Two cleaning regions are observed and is a consequence of the Gaussian distribution of the laser beam energy. The surface roughness of the ablated WC-Co increased with increasing laser fluence and NOP.

In vitro study of electrodeposited fluoridated hydroxyapatite coating on G-II titanium with a nanostructured TiO2 interlayer.

PubMed

Lin, Jin-Shyong; Tsai, Tzung-Bau; Say, Wen-Ching; Chiu, Chun; Chen, Shih-Hsun

2017-04-04

Titanium and its alloys have been widely used as orthopedic and dental implants for several decades due to their superior mechanical properties, corrosion resistance and biocompatibility. Recently, many researches revealed that the hydroxyapatite coatings on biomedical materials can further improve their biocompatibility and bioactivity. However, hydroxyapatite coatings are easily decomposed, weakening the bonding between implants and bone tissues and resulting in a high dissolution rate in the biological environment. Prolonging the lifetime of hydroxyapatite in implants is valuable for improving postoperative quality. Hydroxyapatite is the primary inorganic component of bones and teeth. A suitable amount of fluoride ions would be beneficial for the formation of fluoridated hydroxyapatite, which can enhance bone-cell response and the acid resistance of enamel. In this study, G-II titanium substrate was anodized to form a TiO 2 interlayer with a nanotube structure. An electrolyte composed of fluoride, calcium and phosphorus ions was prepared for electroplating fluoridated hydroxyapatite (FHA) coatings onto anodized G-II titanium substrates at a constant voltage. The obtained coatings were examined for their microstructure, mechanical properties; moreover, the changes of apatite structure, surface morphology and corrosion resistance were further investigated after immersion in simulated body fluid (SBF) for a number of weeks. The results show that FHA coatings have a higher surface roughness and hardness than plain hydroxyapatite. After immersion in SBF, the FHA coatings induced the nucleation and growth of apatite on the surface and increased their crystallinity. In a potentiodynamic polarization test, FHA coatings exhibited a better anti-corrosion ability than bare G-II titanium substrate in SBF. Additionally, the anodized TiO 2 nanotube improved the adhesion and corrosion resistance of FHA as well.

Detonation nanodiamonds biofunctionalization and immobilization to titanium alloy surfaces as first steps towards medical application.

PubMed

Gonçalves, Juliana P L; Shaikh, Afnan Q; Reitzig, Manuela; Kovalenko, Daria A; Michael, Jan; Beutner, René; Cuniberti, Gianaurelio; Scharnweber, Dieter; Opitz, Jörg

2014-01-01

Due to their outstanding properties nanodiamonds are a promising nanoscale material in various applications such as microelectronics, polishing, optical monitoring, medicine and biotechnology. Beyond the typical diamond characteristics like extreme hardness or high thermal conductivity, they have additional benefits as intrinsic fluorescence due to lattice defects without photobleaching, obtained during the high pressure high temperature process. Further the carbon surface and its various functional groups in consequence of the synthesis, facilitate additional chemical and biological modification. In this work we present our recent results on chemical modification of the nanodiamond surface with phosphate groups and their electrochemically assisted immobilization on titanium-based materials to increase adhesion at biomaterial surfaces. The starting material is detonation nanodiamond, which exhibits a heterogeneous surface due to the functional groups resulting from the nitrogen-rich explosives and the subsequent purification steps after detonation synthesis. Nanodiamond surfaces are chemically homogenized before proceeding with further functionalization. Suspensions of resulting surface-modified nanodiamonds are applied to the titanium alloy surfaces and the nanodiamonds subsequently fixed by electrochemical immobilization. Titanium and its alloys have been widely used in bone and dental implants for being a metal that is biocompatible with body tissues and able to bind with adjacent bone during healing. In order to improve titanium material properties towards biomedical applications the authors aim to increase adhesion to bone material by incorporating nanodiamonds into the implant surface, namely the anodically grown titanium dioxide layer. Differently functionalized nanodiamonds are characterized by infrared spectroscopy and the modified titanium alloys surfaces by scanning and transmission electron microscopy. The process described shows an adsorption and immobilization of modified nanodiamonds on titanium; where aminosilanized nanodiamonds coupled with O-phosphorylethanolamine show a homogeneous interaction with the titanium substrate.

Nanotubular topography enhances the bioactivity of titanium implants.

PubMed

Huang, Jingyan; Zhang, Xinchun; Yan, Wangxiang; Chen, Zhipei; Shuai, Xintao; Wang, Anxun; Wang, Yan

2017-08-01

Surface modification on titanium implants plays an important role in promoting mesenchymal stem cell (MSC) response to enhance osseointegration persistently. In this study, nano-scale TiO 2 nanotube topography (TNT), micro-scale sand blasted-acid etched topography (SLA), and hybrid sand blasted-acid etched/nanotube topography (SLA/TNT) were fabricated on the surfaces of titanium implants. Although the initial cell adherence at 60 min among TNT, SLA and TNT/SLA was not different, SLA and SLA/TNT presented to be rougher and suppressed the proliferation of MSC. TNT showed hydrophilic surface and balanced promotion of cellular functions. After being implanted in rabbit femur models, TNT displayed the best osteogenesis inducing ability as well as strong bonding strength to the substrate. These results indicate that nano-scale TNT provides favorable surface topography for improving the clinical performance of endosseous implants compared with micro and hybrid micro/nano surfaces, suggesting a promising and reliable surface modification strategy of titanium implants for clinical application. Copyright © 2017 Elsevier Inc. All rights reserved.

Titanium oxide as substrate for neural cell growth.

PubMed

Carballo-Vila, Mónica; Moreno-Burriel, Berta; Chinarro, Eva; Jurado, José R; Casañ-Pastor, Nieves; Collazos-Castro, Jorge E

2009-07-01

Titanium oxide has antiinflammatory activity and tunable electrochemical behavior that make it an attractive material for the fabrication of implantable devices. The most stable composition is TiO2 and occurs mainly in three polymorphs, namely, anatase, rutile, and brookite, which differ in its crystallochemical properties. Here, we report the preparation of rutile surfaces that permit good adherence and axonal growth of cultured rat cerebral cortex neurons. Rutile disks were obtained by sinterization of TiO2 powders of commercial origin or precipitated from hydrolysis of Ti(IV)-isopropoxide. Commercial powders sintered at 1300-1600 degrees C produced rutile surfaces with abnormal grain growth, probably because of impurities of the powders. Neurons cultured on those surfaces survived in variable numbers and showed fewer neurites than on control materials. On the other hand, rutile sintered from precipitated powders had less contaminants and more homogenous grain growth. By adjusting the thermal treatment it was possible to obtain surfaces performing well as substrate for neuron survival for at least 10 days. Some surfaces permitted normal axonal elongation, whereas dendrite growth was generally impaired. These findings support the potential use of titanium oxide in neuroprostheses and other devices demanding materials with enhanced properties in terms of biocompatibility and axon growth promotion.

Effect of Ti Substrate Ion Implantation on the Physical Properties of Anodic TiO2 Nanotubes

NASA Astrophysics Data System (ADS)

Jedi-Soltanabadi, Zahra; Ghoranneviss, Mahmood; Ghorannevis, Zohreh; Akbari, Hossein

2018-03-01

The influence of nitrogen-ion implantation on the titanium (Ti) surface is studied. The nontreated Ti and the Ti treated with ion implantation were anodized in an ethylene-glycol-based electrolyte solution containing 0.3 wt% ammonium fluoride (NH4F) and 3 vol% deionized (DI) water at a potential of 60 V for 1 h at room temperature. The current density during the growth of the TiO2 nanotubes was monitored in-situ. The surface roughnesses of the Ti substrates before and after the ion implantation were investigated with atomic force microscopy (AFM). The surface roughness was lower for the treated Ti substrate. The morphology of the anodic TiO2 nanotubes was studied by using field-emission scanning electron microscopy (FESEM). Clearly, the titanium nanotubes grown on the treated substrate were longer. In addition, some ribs were observed on their walls. The optical band gap of the anodic TiO2 nanotubes was characterized by using a diffuse reflection spectral (DRS) analysis. The anodic TiO2 nanotubes grown on the treated Ti substrate revealed a band gap energy of approximately 3.02 eV.

Structural characterization of oxidized titanium surfaces

NASA Astrophysics Data System (ADS)

Jobin, M.; Taborelli, M.; Descouts, P.

1995-05-01

Oxidized titanium surfaces resulting from various processes have been structurally characterized by means of scanning force microscopy, x-ray photoemission spectroscopy (XPS), x-ray diffraction, and electron energy-loss spectroscopy (EELS) with losses in the 0-100 eV range. It has been found that the surface morphology has a granular structure for electropolished titanium and for titanium evaporated on mica at low substrate temperature (570 K), but changes to flat terraces for the films evaporated at higher temperature (770 K). Angular-dependent XPS has revealed the presence of a Ti2O3 suboxide at the Ti/TiO2 interface for electropolished titanium. Dry oxidation has been performed at 770 and 970 K on both weakly and highly crystallized evaporated titanium films oriented along (0001). In the case of underlying crystallized metallic titanium, the resulting TiO2 films are crystallized with the anatase (004) orientation for oxidation at 770 K and with rutile (200) orientation for oxidation at 970 K. EELS spectra interpreted in terms of the molecular orbitals of a (TiO6)8- cluster show that the local octahedral environment of titanium atoms is preserved on native oxides, even if these oxides are not crystallized.

Characterization of poly(Sodium Styrene Sulfonate) Thin Films Grafted from Functionalized Titanium Surfaces

PubMed Central

Zorn, Gilad; Baio, Joe E.; Weidner, Tobias; Migonney, Veronique; Castner, David G.

2011-01-01

Biointegration of titanium implants in the body is controlled by their surface properties. Improving surface properties by coating with a bioactive polymer is a promising approach to improve the biological performance of titanium implants. To optimize the grafting processes, it is important to fully understand the composition and structure of the modified surfaces. The main focus of this study is to provide a detailed, multi-technique characterization of a bioactive poly(sodium styrene sulfonate) (pNaSS) thin film grafted from titanium surfaces via a two-step procedure. Thin titanium films (~50 nm thick with an average surface roughness of 0.9±0.2nm) prepared by evaporation onto silicon wafers were used as smooth model substrates. X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) showed that the titanium film was covered with a TiO2 layer that was at least 10nm thick and contained hydroxyl groups present at the outermost surface. These hydroxyl groups were first modified with a 3-methacryloxypropyltrimethoxysilane (MPS) cross linker. XPS and ToF-SIMS showed that a monolayer of the MPS molecules were successfully attached onto the titanium surfaces. The pNaSS film was grafted from the MPS modified titanium through atom transfer radical polymerization. Again, XPS and ToF-SIMS were used to verify that the pNaSS molecules were successfully grafted onto the modified surfaces. Atomic force microscopy analysis showed that the film was smooth and uniformly covered the surface. Fourier transform infrared spectroscopy indicated an ordered array of grafted NaSS molecules were present on the titanium surfaces. Sum frequency generation vibration spectroscopy and near edge X-ray absorption fine structure spectroscopy illustrated that the NaSS molecules were grafted onto the titanium surface with a substantial degree of orientational order in the styrene rings. PMID:21892821

Sol-gel-derived hydroxyapatite-carbon nanotube/titania coatings on titanium substrates.

PubMed

Ji, Xiaoli; Lou, Weiwei; Wang, Qi; Ma, Jianfeng; Xu, Haihong; Bai, Qing; Liu, Chuantong; Liu, Jinsong

2012-01-01

In this paper, hydroxyapatite-carbon nanotube/titania (HA-CNT/TiO(2)) double layer coatings were successfully developed on titanium (Ti) substrates intended for biomedical applications. A TiO(2) coating was firstly developed by anodization to improve bonding between HA and Ti, and then the layer of HA and CNTs was coated on the surface by the sol-gel process to improve the biocompatibility and mechanical properties of Ti. The surfaces of double layer coatings were uniform and crack-free with a thickness of about 7 μm. The bonding strength of the HA-CNT/TiO(2) coating was higher than that of the pure HA and HA-CNT coatings. Additionally, in vitro cell experiments showed that CNTs promoted the adhesion of preosteoblasts on the HA-CNT/TiO(2) double layer coatings. These unique surfaces combined with the osteoconductive properties of HA exhibited the excellent mechanical properties of CNTs. Therefore, the developed HA-CNT/TiO(2) coatings on Ti substrates might be a promising material for bone replacement.

Laser-driven high-frequency vibrations of metal blister surface

NASA Astrophysics Data System (ADS)

Kononenko, T. V.; Sinyavsky, M. N.; Konov, V. I.; Sentis, M.

2013-09-01

Time-resolved interferometric microscopy was applied to investigate laser-induced blistering of a titanium film on a silica substrate. Ablation of the titanium/silica interface by single 0.7 ns pulses within a certain fluence range results in local exfoliation of the metal film from the substrate avoiding, however, complete film destruction. Time-dependent transformation of the metal surface profile was reconstructed from the interference patterns within 0-13 ns time delay range. Transverse annular waves with typical amplitude of one hundred of nanometers and estimated traveling speed of few kilometers per second were revealed on the blister surface. The wave occurrence was attributed to fast inhomogeneous bending of the film covering the expanding blister. The resultant high-frequency (˜1 GHz) vibrations of the metal surface provide intensive inertial forces when such metalized target is used for blister-based laser-induced forward transfer of nanopowders and organic molecules.

Bioactive borate glass coatings for titanium alloys.

PubMed

Peddi, Laxmikanth; Brow, Richard K; Brown, Roger F

2008-09-01

Bioactive borate glass coatings have been developed for titanium and titanium alloys. Glasses from the Na(2)O-CaO-B(2)O(3) system, modified by additions of SiO(2), Al(2)O(3), and P(2)O(5), were characterized and compositions with thermal expansion matches to titanium were identified. Infrared and X-ray diffraction analyses indicate that a hydroxyapatite surface layer forms on the borate glasses after exposure to a simulated body fluid for 2 weeks at 37 degrees C; similar layers form on 45S5 Bioglass((R)) exposed to the same conditions. Assays with MC3T3-E1 pre-osteoblastic cells show the borate glasses exhibit in vitro biocompatibility similar to that of the 45S5 Bioglass((R)). An enameling technique was developed to form adherent borate glass coatings on Ti6Al4V alloy, with adhesive strengths of 36 +/- 2 MPa on polished substrates. The results show these new borate glasses to be promising candidates for forming bioactive coatings on titanium substrates.

Oxygen-implanted induced formation of oxide layer enhances blood compatibility on titanium for biomedical applications.

PubMed

Hung, Wei-Chiang; Chang, Fang-Mo; Yang, Tzu-Sen; Ou, Keng-Liang; Lin, Che-Tong; Peng, Pei-Wen

2016-11-01

Titanium dioxide (TiO2) layers were prepared on a Ti substrate by using oxygen plasma immersion ion implantation (oxygen PIII). The surface chemical states, structure, and morphology of the layers were studied using X-ray photoelectron spectroscopy, X-ray diffraction, Raman microscopy, atomic force microscopy and scanning electron microscope. The mechanical properties, such as the Young's modulus and hardness, of the layers were investigated using nanoindentation testing. The Ti(4+) chemical state was determined to be present on oxygen-PIII-treated surfaces, which consisted of nanocrystalline TiO2 with a rutile structure. Compared with Ti substrates, the oxygen-PIII-treated surfaces exhibited decreased Young's moduli and hardness. Parameters indicating the blood compatibility of the oxygen-PIII-treated surfaces, including the clotting time and platelet adhesion and activation, were studied in vitro. Clotting time assays indicated that the clotting time of oxygen-PIII-treated surfaces was longer than that of the Ti substrate, which was associated with decreased fibrinogen adsorption. In conclusion, the surface characteristics and the blood compatibility of Ti implants can be modified and improved using oxygen PIII. Copyright © 2016 Elsevier B.V. All rights reserved.

Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

PubMed

Catauro, M; Papale, F; Bollino, F

2016-01-01

The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0

In vitro response to alkaline phosphatase coatings immobilized onto titanium implants using electrospray deposition or polydopamine-assisted deposition.

PubMed

Nijhuis, Arnold W G; van den Beucken, Jeroen J J P; Jansen, John A; Leeuwenburgh, Sander C G

2014-04-01

Immobilization of biomolecules onto implant surfaces is one of the most straightforward strategies to control the interaction between an implant and its biological environment. Recently, it was shown that the enzyme alkaline phosphatase (ALP) could be efficiently immobilized onto titanium implants in a single step using polydopamine. We hypothesized that such polydopamine-ALP coatings can enhance the early attachment of cells and increase mineralization. Therefore, the current study aimed at immobilization of ALP onto titanium by means of either one- or two-step polydopamine-assisted immobilization or electrospray deposition, the comparative characterization of these experimental substrates and subsequent cell behavioral analysis using primary osteoblast-like cells. Uncoated titanium and ALP-free polydopamine coatings served as controls. Despite significant ALP surface activity and lower water contact for angles ALP-containing surface modifications, only marginal effects on early cell behavior (i.e., cell spreading) and osteogenic differentiation (i.e., proliferation, differentiation and mineralization) were observed in comparison to uncoated titanium. Copyright © 2013 Wiley Periodicals, Inc.

Wear evaluation of flank in burins of high speed steel modified with titanium ions

NASA Astrophysics Data System (ADS)

E Caballero, J.; V-Niño, E. D.

2017-12-01

This report shows the results obtained researching the flank wearing resistance performed by the high-speed steel (HSS) burins without any surface treatment (reference substrate) and others with surface treatment based on Titanium ions. The flank wearing was carried out by means of an industrial process by chip removal with repetitive tests of dry finished turning of AISI/SAE 1045 steel bars. The useful service life of the burins was evaluated according to ISO 3685:1993, and it was found that the burins treated with Titanium ions showed an increase in the flank wearing resistance with respect to the ones used as reference.

Fe-C-Si ternary composite coating on CP-titanium and its tribological properties

NASA Astrophysics Data System (ADS)

Maleque, M. A.; Saffina, W.; Ahmed, A. S.; Ali, M. Y.

2017-03-01

This study focused on the development of ternary composite coating through incorporation of Fe-C-Si ternary powder mixtures on CP-Ti substrate and characterizes the microstructure, hardness and wears behavior in presence of Jatropha oil. In this work, the surface of commercial purity titanium (CP-Ti) was modified using a tungsten inert gas (TIG) surface melting technique. The wear behavior of coated CP-titanium was performed using pin-on-disk machine. The results showed that the melt track has dendritic microstructure which was homogenously distributed throughout the melt pool. This Fe-C-Si ternary composite coating enhanced the surface hardness of CP-Ti significantly from 175 HV for the untreated substrate to ∼800 HV for the Fe-C-Si coated CP-Ti due to the formation of intermetallic compounds.. The wear results showed that less wear volume loss was observed on the composite coated CP-Ti in presence of Jatropha-biodiesel compared to uncoated CP-Ti. The achievement of this hard Fe-C-Si composite coating on the surface of CP-Ti can broadened new prospect for many engineering applications that use biodiesel under different tribological variables.

Waterless TiO{sub 2} atomic layer deposition using titanium tetrachloride and titanium tetraisopropoxide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anderson, Virginia R.; Cavanagh, Andrew S.; Abdulagatov, Aziz I.

2014-01-15

The surface chemistry for TiO{sub 2} atomic layer deposition (ALD) typically utilizes water or other oxidants that can oxidize underlying substrates such as magnetic disks or semiconductors. To avoid this oxidation, waterless or oxidant-free surface chemistry can be used that involves titanium halides and titanium alkoxides. In this study, waterless TiO{sub 2} ALD was accomplished using titanium tetrachloride (TiCl{sub 4}) and titanium tetraisopropoxide (TTIP). In situ transmission Fourier transform infrared (FTIR) studies were employed to study the surface species and the reactions during waterless TiO{sub 2} ALD. At low temperatures between 125 and 225  °C, the FTIR absorbance spectra revealed thatmore » the isopropoxide species remained on the surface after TTIP exposures. The TiCl{sub 4} exposures then removed the isopropoxide species and deposited additional titanium species. At high temperatures between 250 and 300  °C, the isopropoxide species were converted to hydroxyl species by β-hydride elimination. The observation of propene gaseous reaction product by quadrupole mass spectrometry (QMS) confirmed the β-hydride elimination reaction pathway. The TiCl{sub 4} exposures then easily reacted with the hydroxyl species. QMS studies also observed the 2-chloropropane and HCl gaseous reaction products and monitored the self-limiting nature of the TTIP reaction. Additional studies examined the waterless TiO{sub 2} ALD growth at low and high temperature. Quartz crystal microbalance measurements observed growth rates of ∼3 ng/cm{sup 2} at a low temperature of 150  °C. Much higher growth rates of ∼15 ng/cm{sup 2} were measured at a higher temperature of 250  °C under similar reaction conditions. X-ray reflectivity analysis measured a growth rate of 0.55 ± 0.05 Å/cycle at 250  °C. X-ray photoelectron depth-profile studies showed that the TiO{sub 2} films contained low Cl concentrations <1 at. %. This waterless TiO{sub 2} ALD process using TiCl{sub 4} and TTIP should be valuable to prevent substrate oxidation during TiO{sub 2} ALD on oxygen-sensitive substrates.« less

Influence of laser cladding regimes on structural features and mechanical properties of coatings on titanium substrates

NASA Astrophysics Data System (ADS)

Malyutina, Yulia N.; Lazurenko, Daria V.; Bataev, Ivan A.; Movtchan, Igor A.

2015-10-01

In this paper an influence of the tantalum content on the structure and properties of surface layers of the titanium alloy doped using a laser treatment technology was investigated. It was found that an increase of a quantity of filler powder per one millimeter of a track length contributed to a rise of the content of undissolved particles in coatings. The maximum thickness of a cladded layer was reached at the mass of powder per the length unit equaled to 5.5 g/cm. Coatings were characterized by the formation of a dendrite structure with attributes of segregation. The width of a quenched fusion zone grew with an increase in the rate of powder feed to the treated area. Significant strengthening of the titanium surface layer alloyed with tantalum was not observed; however, the presence of undissolved tantalum particles can decrease the hardness of titanium surface layers.

Adhesion enhancement of titanium nitride coating on aluminum casting alloy by intrinsic microstructures

NASA Astrophysics Data System (ADS)

Nguyen, Chuong L.; Preston, Andrew; Tran, Anh T. T.; Dickinson, Michelle; Metson, James B.

2016-07-01

Aluminum casting alloys have excellent castability, high strength and good corrosion resistance. However, the presence of silicon in these alloys prevents surface finishing with conventional methods such as anodizing. Hard coating with titanium nitride can provide wear and corrosion resistances, as well as the aesthetic finish. A critical factor for a durable hard coating is its bonding with the underlying substrate. In this study, a titanium nitride layer was coated on LM25 casting alloy and a reference high purity aluminum substrate using Ion Assisted Deposition. Characterization of the coating and the critical interface was carried out by a range of complementing techniques, including SIMS, XPS, TEM, SEM/EDS and nano-indentation. It was observed that the coating on the aluminum alloy is stronger compared to that on the pure aluminum counterpart. Silicon particles in the alloy offers the reinforcement though mechanical interlocking at microscopic level, even with nano-scale height difference. This reinforcement overcomes the adverse effect caused by surface segregation of magnesium in aluminum casting alloys.

Electronic and Optical Properties of Titanium Nitride Bulk and Surfaces from First Principles Calculations (Postprint)

DTIC Science & Technology

2015-11-18

thickness of the film, or substrate. In this work, we report calculations for titanium nitride ( TiN ), a promising material for plasmonic applications...stoichiometric bulk TiN , as well as of the TiN (100), TiN (110), and TiN (111) outermost surfaces. Density functional theory (DFT) and many-body GW methods...and the band structure for bulk TiN were shown to be consistent with previous work. Calculated dielectric functions, plasma frequencies, reflectivity

Characterization of surface roughness of laser deposited titanium alloy and copper using AFM

NASA Astrophysics Data System (ADS)

Erinosho, M. F.; Akinlabi, E. T.; Johnson, O. T.

2018-03-01

Laser Metal Deposition (LMD) is the process of using the laser beam of a nozzle to produce a melt pool on a metal surface usually the substrate and metal powder is been deposited into it thereby creating a fusion bond with the substrate to form a new material layer against the force gravity. A good metal laminate is formed when the wettability between the dropping metal powder and the substrate adheres. This paper reports the surface roughness of laser deposited titanium alloy and copper (Ti6Al4V + Cu) using the Atomic Force Microscopy (AFM). This AFM is employed in order to sense the surface and produce different manipulated images using the micro-fabricated mechanical tip under a probe cartridge of high resolution. The process parameters employed during the deposition routine determines the output of the deposit. A careful attention is given to the laser deposited Ti6Al4V + Cu samples under the AFM probe because of their single tracked layers with semi-circular pattern of deposition. This research work can be applicable in the surface modification of laser deposited samples for the marine industry.

Characterization of ion beam modified ceramic wear surfaces using Auger electron spectroscopy

NASA Technical Reports Server (NTRS)

Wei, W.; Lankford, J.

1987-01-01

An investigation of the surface chemistry and morphology of the wear surfaces of ceramic material surfaces modified by ion beam mixing has been conducted using Auger electron spectroscopy and secondary electron microscopy. Studies have been conducted on ceramic/ceramic friction and wear couples made up of TiC and NiMo-bonded TiC cermet pins run against Si3N4 and partially stabilized zirconia disc surfaces modified by the ion beam mixing of titanium and nickel, as well as ummodified ceramic/ceramic couples in order to determine the types of surface changes leading to the improved friction and wear behavior of the surface modified ceramics in simulated diesel environments. The results of the surface analyses indicate that the formation of a lubricating oxide layer of titanium and nickel, is responsible for the improvement in ceramic friction and wear behavior. The beneficial effect of this oxide layer depends on several factors, including the adherence of the surface modified layer or subsequently formed oxide layer to the disc substrate, the substrate materials, the conditions of ion beam mixing, and the environmental conditions.

Molybdeno-Aluminizing of Powder Metallurgy and Wrought Ti and Ti-6Al-4V alloys by Pack Cementation process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tsipas, Sophia A., E-mail: stsipas@ing.uc3m.es; Go

Wear and high temperature oxidation resistance of some titanium-based alloys needs to be enhanced, and this can be effectively accomplished by surface treatment. Molybdenizing is a surface treatment where molybdenum is introduced into the surface of titanium alloys causing the formation of wear-resistant surface layers containing molybdenum, while aluminizing of titanium-based alloys has been reported to improve their high temperature oxidation properties. Whereas pack cementation and other surface modification methods have been used for molybdenizing or aluminizing of wrought and/or cast pure titanium and titanium alloys, such surface treatments have not been reported on titanium alloys produced by powder metallurgymore » (PM). Also a critical understanding of the process parameters for simultaneous one step molybdeno-aluminizing of titanium alloys by pack cementation and the predominant mechanism for this process have not been reported. The current research work describes the surface modification of titanium and Ti-6Al-4V prepared by PM by molybdeno-aluminizing and analyzes thermodynamic aspects of the deposition process. Similar coatings are also deposited to wrought Ti-6Al-4V and compared. Characterization of the coatings was carried out using scanning electron microscopy and x-ray diffraction. For both titanium and Ti-6Al-4V, the use of a powder pack containing ammonium chloride as activator leads to the deposition of molybdenum and aluminium into the surface but also introduces nitrogen causing the formation of a thin titanium nitride layer. In addition, various titanium aluminides and mixed titanium aluminium nitrides are formed. The appropriate conditions for molybdeno-aluminizing as well as the phases expected to be formed were successfully determined by thermodynamic equilibrium calculations. - Highlights: •Simultaneous co-deposition of Mo-Al onto powder metallurgy and wrought Ti alloy •Thermodynamic calculations were used to optimize deposition conditions •External TiN and internal a Mo-rich layer on all alloy substrates •Titanium aluminides and Ti-Al mixed nitrides are formed on Ti-6Al-4V •The presence of Al and V alloying elements modifies the diffusion of Mo.« less

Biomimetic Deposition of Hydroxyapatite by Mixed Acid Treatment of Titanium Surfaces.

PubMed

Zhao, J M; Park, W U; Hwang, K H; Lee, J K; Yoon, S Y

2015-03-01

A simple chemical method was established for inducing bioactivity of Ti metal. In the present study, two kinds of mixed acid solutions were used to treat Ti specimens to induce Ca-P formation. Following a strong mixed acid activation process, Ca-P coatings successfully formed on the Ti surfaces in the simulated body fluid. Strong mixed acid etching was used to increase the roughness of the metal surface, because the porous and rough surfaces allow better adhesion between Ca-P coatings and substrate. Nano-scale modification of titanium surfaces can alter cellular and tissue responses, which may benefit osseointegration and dental implant therapy. Some specimens were treated with a 5 M NaOH aqueous solution, and then heat treated at 600 °C in order to form an amorphous sodium titanate layer on their surface. This treated titanium metal is believed to form a dense and uniform bone-like apatite layer on its surface in a simulated body fluid (SBF). This study proved that mixed acid treatment is not only important for surface passivation but is also another bioactive treatment for titanium surfaces, an alternative to alkali treatment. In addition, mixed acid treatment uses a lower temperature and shorter time period than alkali treatment.

Substrate-insensitive atomic layer deposition of plasmonic titanium nitride films

DOE PAGES

Yu, Ing-Song; Cheng, Hsyi-En; Chang, Chun-Chieh; ...

2017-02-06

The plasmonic properties of titanium nitride (TiN) films depend on the type of substrate when using typical deposition methods such as sputtering. We show atomic layer deposition (ALD) of TiN films with very weak dependence of plasmonic properties on the substrate, which also suggests the prediction and evaluation of plasmonic performance of TiN nanostructures on arbitrary substrates under a given deposition condition. Our results also observe that substrates with more nitrogen-terminated (N-terminated) surfaces will have significant impact on the deposition rate as well as the film plasmonic properties. Furthermore, we illustrate that the plasmonic properties of ALD TiN films canmore » be tailored by simply adjusting the deposition and/or post-deposition annealing temperatures. These characteristics and the capability of conformal coating make ALD TiN films on templates ideal for applications that require the fabrication of complex 3D plasmonic nanostructures.« less

Fabrication of biomimetic resorption lacunae-like structure on titanium surface and its osteoblast responses

NASA Astrophysics Data System (ADS)

Huo, Fangjun; Guo, Weihua; Wu, Hao; Wang, Yueting; He, Gang; Xie, Li; Tian, Weidong

2018-04-01

Biomimetic specific surface structure could improve biological behaviors of specific cells and eventual tissue integration. Featuring titanium surface with structures resembling bone resorption lacunae (RL) can be a promising approach to improve the osteoblast responses and osseointegration of implants. As a most common used dental implant surface, sandblasting and acid etching (SLA) surface has micro-sized structures with dimensions similar to RL, but great differences exist when it comes to shape and contour. In this work, by anodizing titanium substrate in a novel HCOONa/CH3COONa electrolyte, RL-like crater structures were fabricated with highly similar size, shape and contour. Compared with SLA, it was much more similar to RL structure in shape and contour. Furthermore, through subsequent alkali-heat treatment, nano-sized structures that overlaid the whole surface were obtained, which further mimic undercuts features inside the RL. The as-prepared surface was consisted of crystalline titania and exhibited super-hydrophilicity with good stability. In vitro evaluation results showed that the surface could significantly improve adhesion, proliferation and differentiation of MG63 cells in comparison with SLA. This new method may be a promising candidate for biomimetic modification of titanium implant to promote osseointegration.

Rutile titanium dioxide films deposited with a vacuum arc at different temperatures

NASA Astrophysics Data System (ADS)

Arias, L. Franco; Kleiman, A.; Heredia, E.; Márquez, A.

2012-06-01

Rutile crystalline phase of TiO2 has been one of the most investigated materials for medical applications. Its implementation as a surface layer on biomedical implants has shown to improve hemocompatibility and biocompatibility. In this work, titanium dioxide coatings were deposited on glass and steel 316L substrates using cathodic arc deposition. The coatings were obtained at different substrate temperatures; varying from room temperature to 600°C. The crystalline structure of the films was identified by glancing angle X-ray diffraction. Depending on the substrate material and on its temperature during the deposition process, anatase, anatse+rutile and rutile structures were observed. It was determined that rutile films can be obtained below 600 °C with this deposition method.

Structure and mechanical properties of a two-layered material produced by the E-beam surfacing of Ta and Nb on the titanium base after multiple rolling

NASA Astrophysics Data System (ADS)

Bataev, V. A.; Golkovski, M. G.; Samoylenko, V. V.; Ruktuev, A. A.; Polyakov, I. A.; Kuksanov, N. K.

2018-04-01

The study has been conducted in line with the current approach to investigation of materials obtained by considerably deep surface alloying of the titanium substrate with Ta, Nb, and Zr. The thickness of the resulting alloyed layer was equal to 2 mm. The coating was formed through weld deposition of a powder with the use of a high-voltage electron beam in the air. It has been lately demonstrated that manufactured such a way alloyed layers possess corrosion resistance which is significantly higher than the resistance of titanium substrates. It has already been shown that such two-layered materials are weldable. The study objective is to investigate the feasibility of rolling for necking the sheets with the Ti-Ta-Nb anticorrosion coating with further fourfold decrease in their thickness. The research is also aimed at investigation of the material properties after rolling. Anticorrosion layers were formed both on CP-titanium and on VT14 (Ti-4Al-3Mo-1 V) durable titanium alloy. The results of chemical composition determination, structure examination, X-ray phase analysis and mechanical properties observations (including bending properties of the alloyed layers) are presented in the paper. The combination of welding, rolling, and bending enables the manufacture of corrosion-resistant vessels and process pipes which are made from the developed material and find technological application.

Precision replenishable grinding tool and manufacturing process

DOEpatents

Makowiecki, D.M.; Kerns, J.A.; Blaedel, K.L.; Colella, N.J.; Davis, P.J.; Juntz, R.S.

1998-06-09

A reusable grinding tool consisting of a replaceable single layer of abrasive particles intimately bonded to a precisely configured tool substrate, and a process for manufacturing the grinding tool are disclosed. The tool substrate may be ceramic or metal and the abrasive particles are preferably diamond, but may be cubic boron nitride. The manufacturing process involves: coating a configured tool substrate with layers of metals, such as titanium, copper and titanium, by physical vapor deposition (PVD); applying the abrasive particles to the coated surface by a slurry technique; and brazing the abrasive particles to the tool substrate by alloying the metal layers. The precision control of the composition and thickness of the metal layers enables the bonding of a single layer or several layers of micron size abrasive particles to the tool surface. By the incorporation of an easily dissolved metal layer in the composition such allows the removal and replacement of the abrasive particles, thereby providing a process for replenishing a precisely machined grinding tool with fine abrasive particles, thus greatly reducing costs as compared to replacing expensive grinding tools. 11 figs.

Precision replenishable grinding tool and manufacturing process

DOEpatents

Makowiecki, Daniel M.; Kerns, John A.; Blaedel, Kenneth L.; Colella, Nicholas J.; Davis, Pete J.; Juntz, Robert S.

1998-01-01

A reusable grinding tool consisting of a replaceable single layer of abrasive particles intimately bonded to a precisely configured tool substrate, and a process for manufacturing the grinding tool. The tool substrate may be ceramic or metal and the abrasive particles are preferably diamond, but may be cubic boron nitride. The manufacturing process involves: coating a configured tool substrate with layers of metals, such as titanium, copper and titanium, by physical vapor deposition (PVD); applying the abrasive particles to the coated surface by a slurry technique; and brazing the abrasive particles to the tool substrate by alloying the metal layers. The precision control of the composition and thickness of the metal layers enables the bonding of a single layer or several layers of micron size abrasive particles to the tool surface. By the incorporation of an easily dissolved metal layer in the composition such allows the removal and replacement of the abrasive particles, thereby providing a process for replenishing a precisely machined grinding tool with fine abrasive particles, thus greatly reducing costs as compared to replacing expensive grinding tools.

Fabrication, ultra-structure characterization and in vitro studies of RF magnetron sputter deposited nano-hydroxyapatite thin films for biomedical applications

NASA Astrophysics Data System (ADS)

Surmeneva, Maria A.; Surmenev, Roman A.; Nikonova, Yulia A.; Selezneva, Irina I.; Ivanova, Anna A.; Putlyaev, Valery I.; Prymak, Oleg; Epple, Matthias

2014-10-01

A series of nanostructured low-crystalline hydroxyapatite (HA) coatings averaging 170, 250, and 440 nm in thickness were deposited onto previously etched titanium substrates through radio-frequency (RF) magnetron sputtering. The HA coatings were analyzed using infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM). Cross sections of the thin specimens were prepared by FIB to study the microstructure of the coatings by TEM. The deposition process formed nano-scale grains, generating an amorphous layer at the substrate/coating interface and inducing the growth of a columnar grain structure perpendicular to the substrate surface. A microstructural analysis of the film confirmed that the grain size and crystallinity increased when increasing the deposition time. The nanostructured HA coatings were not cytotoxic, as proven by in vitro assays using primary dental pulp stem cells and mouse fibroblast NCTC clone L929 cells. Low-crystallinity HA coatings with different thicknesses stimulated cells to attach, proliferate and form mineralized nodules on the surface better than uncoated titanium substrates.

Surface Modification Enhanced Reflection Intensity of Quartz Crystal Microbalance Sensors upon Molecular Adsorption.

PubMed

Kojima, Taisuke

2018-01-01

Molecular adsorption on a sensing surface involves molecule-substrate and molecule-molecule interactions. Combining optical systems and a quartz crystal microbalance (QCM) on the same sensing surface allows the quantification of such interactions and reveals the physicochemical properties of the adsorbed molecules. However, low sensitivity of the current reflection-based techniques compared to the QCM technique hinders the quantitative analysis of the adsorption events. Here, a layer-by-layer surface modification of a QCM sensor is studied to increase the optical sensitivity. The intermediate layers of organic-inorganic molecules and metal-metal oxide were explored on a gold (Au) surface of a QCM sensor. First, polyhedral oligomeric silsesquioxane-derivatives that served as the organic-inorganic intermediate layer were synthesized and modified on the Au-QCM surface. Meanwhile, titanium oxide, fabricated by anodic oxidation of titanium, was used as a metal-metal oxide intermediate layer on a titanium-coated QCM surface. The developed technique enabled interrogation of the molecular adsorption owing to the enhanced optical sensitivity.

Functionalization of Titanium with Chitosan via Silanation: Evaluation of Biological and Mechanical Performances

PubMed Central

Renoud, Pauline; Toury, Bérangère; Benayoun, Stéphane; Attik, Ghania; Grosgogeat, Brigitte

2012-01-01

Complications in dentistry and orthopaedic surgery are mainly induced by peri-implant bacterial infections and current implant devices do not prevent such infections. The coating of antibacterial molecules such as chitosan on its surface would give the implant bioactive properties. The major challenge of this type of coating is the attachment of chitosan to a metal substrate. In this study, we propose to investigate the functionalization of titanium with chitosan via a silanation. Firstly, the surface chemistry and mechanical properties of such coating were evaluated. We also verified if the coated chitosan retained its biocompatibility with the peri-implant cells, as well as its antibacterial properties. FTIR and Tof-SIMS analyses confirmed the presence of chitosan on the titanium surface. This coating showed great scratch resistance and was strongly adhesive to the substrate. These mechanical properties were consistent with an implantology application. The Chitosan-coated surfaces showed strong inhibition of Actinomyces naeslundii growth; they nonetheless showed a non significant inhibition against Porphyromonas gingivalis after 32 hours in liquid media. The chitosan-coating also demonstrated good biocompatibility to NIH3T3 fibroblasts. Thus this method of covalent coating provides a biocompatible material with improved bioactive properties. These results proved that covalent coating of chitosan has significant potential in biomedical device implantation. PMID:22859940

Structure, composition and morphology of bioactive titanate layer on porous titanium surfaces

NASA Astrophysics Data System (ADS)

Li, Jinshan; Wang, Xiaohua; Hu, Rui; Kou, Hongchao

2014-07-01

A bioactive coating was produced on pore surfaces of porous titanium samples by an amendatory alkali-heat treatment method. Porous titanium was prepared by powder metallurgy and its porosity and average size were 45% and 135 μm, respectively. Coating morphology, coating structure and phase constituents were examined by SEM, XPS and XRD. It was found that a micro-network structure with sizes of <200 nm mainly composed of bioactive sodium titanate and rutile phases of TiO2 covered the interior and exterior of porous titanium cells, and redundant Ca ion was detected in the titanate layer. The concentration distribution of Ti, O, Ca and Na in the coating showed a compositional gradient from the intermediate layer toward the outer surface. These compositional gradients indicate that the coating bonded to Ti substrate without a distinct interface. After immersion into the SBF solution for 3 days, a bone-like carbonate-hydroxylapatite showing a good biocompatibility was detected on the coating surface. And the redundant Ca advanced the bioactivity of the coating. Thus, the present modification is expected to allow the use of the bioactive porous titanium as artificial bones even under load-bearing conditions.

Protein adsorption and biomimetic mineralization behaviors of PLL-DNA multilayered films assembled onto titanium

NASA Astrophysics Data System (ADS)

Gao, Wenli; Feng, Bo; Ni, Yuxiang; Yang, Yongli; Lu, Xiong; Weng, Jie

2010-11-01

Titanium and its alloys are frequently used as surgical implants in load bearing situations, such as hip prostheses and dental implants, owing to their biocompatibility, mechanical and physical properties. In this paper, a layer-by-layer (LBL) self-assembly technique, based on the polyelectrolyte-mediated electrostatic adsorption of poly-L-lysine (PLL) and DNA, was used to the formation of multilayer on titanium surfaces. Then bovine serum albumin (BSA) adsorption and biomimetic mineralization of modified surfaces were studied. The chemical composition and wettability of assembled substrates were investigated by X-ray photoelectron spectroscopy (XPS), fluorescence microscopy and water contact angle measurement, respectively. The XPS analysis indicated that the layers were assembled successfully through electrostatic attractions. The measurement with ultraviolet (UV) spectrophotometer revealed that the LBL films enhanced ability of BSA adsorption onto titanium. The adsorption quantity of BSA on the surface terminated with PLL was higher than that of the surface terminated with DNA, and the samples of TiOH/P/D/P absorbed BSA most. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) showed that samples of assembled PLL or/and DNA had better bioactivity in inducing HA formation. Thus the assembling of PLL and DNA onto the surface of titanium in turn via a layer-by-layer self-assembly technology can improve the bioactivity of titanium.

Titanium disilicide formation by sputtering of titanium on heated silicon substrate

NASA Astrophysics Data System (ADS)

Tanielian, M.; Blackstone, S.

1984-09-01

We have sputter deposited titanium on bare silicon substrates at elevated temperatures. We find that at a substrate temperature of about 515 °C titanium silicide is formed due to the reaction of the titanium with the Si. The resistivity of the silicide is about 15 μΩ cm and it is not etchable in a selective titanium etch. This process can have applications in low-temperature, metal-oxide-semiconductor self-aligned silicide formation for very large scale integrated

Rapid prototyped porous nickel–titanium scaffolds as bone substitutes

PubMed Central

Hoffmann, Waldemar; Bormann, Therese; Rossi, Antonella; Müller, Bert; Schumacher, Ralf; Martin, Ivan; Wendt, David

2014-01-01

While calcium phosphate–based ceramics are currently the most widely used materials in bone repair, they generally lack tensile strength for initial load bearing. Bulk titanium is the gold standard of metallic implant materials, but does not match the mechanical properties of the surrounding bone, potentially leading to problems of fixation and bone resorption. As an alternative, nickel–titanium alloys possess a unique combination of mechanical properties including a relatively low elastic modulus, pseudoelasticity, and high damping capacity, matching the properties of bone better than any other metallic material. With the ultimate goal of fabricating porous implants for spinal, orthopedic and dental applications, nickel–titanium substrates were fabricated by means of selective laser melting. The response of human mesenchymal stromal cells to the nickel–titanium substrates was compared to mesenchymal stromal cells cultured on clinically used titanium. Selective laser melted titanium as well as surface-treated nickel–titanium and titanium served as controls. Mesenchymal stromal cells had similar proliferation rates when cultured on selective laser melted nickel–titanium, clinically used titanium, or controls. Osteogenic differentiation was similar for mesenchymal stromal cells cultured on the selected materials, as indicated by similar gene expression levels of bone sialoprotein and osteocalcin. Mesenchymal stromal cells seeded and cultured on porous three-dimensional selective laser melted nickel–titanium scaffolds homogeneously colonized the scaffold, and following osteogenic induction, filled the scaffold’s pore volume with extracellular matrix. The combination of bone-related mechanical properties of selective laser melted nickel–titanium with its cytocompatibility and support of osteogenic differentiation of mesenchymal stromal cells highlights its potential as a superior bone substitute as compared to clinically used titanium. PMID:25383165

Construction of a multifunctional coating consisting of phospholipids and endothelial progenitor cell-specific peptides on titanium substrates

NASA Astrophysics Data System (ADS)

Chen, Huiqing; Li, Xiaojing; Zhao, Yuancong; Li, Jingan; Chen, Jiang; Yang, Ping; Maitz, Manfred F.; Huang, Nan

2015-08-01

A phospholipid/peptide polymer (PMMDP) with phosphorylcholine groups, endothelial progenitor cell (EPC)-specific peptides and catechol groups was anchored onto a titanium (Ti) surface to fabricate a biomimetic multifunctional surface. The PMMDP coating was characterized by X-ray photoelectron spectroscopy (XPS), water contact angle measurements and atomic force microscopy (AFM), respectively. The amount of PMMDP coating on the Ti surface was quantified by using the quartz crystal microbalance with dissipation (QCM-D). Interactions between blood components and the coated and bare Ti substrates were evaluated by platelet adhesion and activation assays and fibrinogen denaturation test using platelet rich plasma (PRP). The results revealed that the PMMDP-modified surface inhibited fibrinogen denaturation and reduced platelet adhesion and activation. EPC cell culture on the PMMDP-modified surface showed increased adhesion and proliferation of EPCs when compared to the cells cultured on untreated Ti surface. The inhibition of fibrinogen denaturation and platelet adhesion and support of EPCs attachment and proliferation indicated that this coating might be beneficial for future applications in blood-contacting implants, such as vascular stents.

Influence of laser cladding regimes on structural features and mechanical properties of coatings on titanium substrates

DOE Office of Scientific and Technical Information (OSTI.GOV)

Malyutina, Yulia N., E-mail: iuliiamaliutina@gmail.ru; Lazurenko, Daria V., E-mail: pavlyukova-87@mail.ru; Bataev, Ivan A., E-mail: ivanbataev@ngs.ru

2015-10-27

In this paper an influence of the tantalum content on the structure and properties of surface layers of the titanium alloy doped using a laser treatment technology was investigated. It was found that an increase of a quantity of filler powder per one millimeter of a track length contributed to a rise of the content of undissolved particles in coatings. The maximum thickness of a cladded layer was reached at the mass of powder per the length unit equaled to 5.5 g/cm. Coatings were characterized by the formation of a dendrite structure with attributes of segregation. The width of a quenchedmore » fusion zone grew with an increase in the rate of powder feed to the treated area. Significant strengthening of the titanium surface layer alloyed with tantalum was not observed; however, the presence of undissolved tantalum particles can decrease the hardness of titanium surface layers.« less

Corrosion resistance of nanostructured titanium.

PubMed

Garbacz, H; Pisarek, M; Kurzydłowski, K J

2007-11-01

The present work reports results of studies of corrosion resistance of pure nano-Ti-Grade 2 after hydrostatic extrusion. The grain size of the examined samples was below 90 nm. Surface analytical technique including AES combined with Ar(+) ion sputtering, were used to investigate the chemical composition and thicknesses of the oxides formed on nano-Ti. It has been found that the grain size of the titanium substrate did not influence the thickness of oxide formed on the titanium. The thickness of the oxide observed on the titanium samples before and after hydrostatic extrusion was about 6 nm. Tests carried out in a NaCl solution revealed a slightly lower corrosion resistance of nano-Ti in comparison with the titanium with micrometric grain size.

Calcium phosphate-based coatings on titanium and its alloys.

PubMed

Narayanan, R; Seshadri, S K; Kwon, T Y; Kim, K H

2008-04-01

Use of titanium as biomaterial is possible because of its very favorable biocompatibility with living tissue. Titanium implants having calcium phosphate coatings on their surface show good fixation to the bone. This review covers briefly the requirements of typical biomaterials and narrowly focuses on the works on titanium. Calcium phosphate ceramics for use in implants are introduced and various methods of producing calcium phosphate coating on titanium substrates are elaborated. Advantages and disadvantages of each type of coating from the view point of process simplicity, cost-effectiveness, stability of the coatings, coating integration with the bone, cell behavior, and so forth are highlighted. Taking into account all these factors, the efficient method(s) of producing these coatings are indicated finally.

Scratch and wear behaviour of plasma sprayed nano ceramics bilayer Al2O3-13 wt%TiO2/hydroxyapatite coated on medical grade titanium substrates in SBF environment

NASA Astrophysics Data System (ADS)

Palanivelu, R.; Ruban Kumar, A.

2014-10-01

Among the various coating techniques, plasma spray coating is an efficient technique to protect the metal surface from the various surface problems like wear and corrosion. The aim of this present work is to design and produce a bilayer coating on the non- toxic commercially pure titanium (denoted as CP-Ti) implant substrate in order to improve the biocompatibility and surface properties. To achieve that, Al2O3-13 wt%TiO2 (AT13) and hydroxyapatite (HAP) were coated on CP-Ti implant substrate using plasma spray coating technique. Further, the coated substrates were subjected to various characterization techniques. The crystallite size of coated HAP and its morphological studies were carried out using X-ray diffractometer (XRD) and scanning electron microscopy (SEM) respectively. The wear test on the bilayer (AT13/HAP) coated CP-Ti implant surface was conducted using ball-on-disc tester under SBF environment at 37 °C, in order to determine the wear rate and the coefficient of friction. The adhesion strength of the bilayer coated surface was evaluated by micro scratch tester under the ramp load conditions with load range of 14-20 N. The above said studies were repeated on the single layer coated HAP and AT13 implant surfaces. The results reveal that the bilayer (AT13/HAP) coated CP-Ti surface has the improved wear rate, coefficient of friction in compared to single layer coated HAP and AT13 surfaces.

Effects of the micro-nano surface topography of titanium alloy on the biological responses of osteoblast.

PubMed

Yin, Chengcheng; Zhang, Yanjing; Cai, Qing; Li, Baosheng; Yang, Hua; Wang, Heling; Qi, Hua; Zhou, Yanmin; Meng, Weiyan

2017-03-01

In clinical applications, osseointegration is essential for the long-term stability of dental implants. Inspired by the hierarchical structure of natural bone, we applied the electrochemical etching (EC) technique to form a micro-nano structure on a titanium alloy (Ti6Al4V) substrate, called EC surface. Sand blasting and acid etching (SLA) and machined (M) methods were employed to generate micro and smooth textures, respectively, as the control groups. The surface topographies of the three substrates were characterized using scanning electron microscopy (SEM). Then, human osteoblast-like cells (MG63) were cultured on substrates, and adhesion, proliferation, morphology, alkaline phosphatase activity (ALP), and gene expression levels of Runt-related transcription factor 2 (RUNX2), osteocalcin (OCN), osteopontin (OPN), and type I collagen (COLIA 1) were analyzed. MG63 cells cultured on the EC Ti alloy substrates displayed better cell adhesion, significant proliferation, and a higher production level of ALP, gene expressions of RUNX2, OCN, OPN and COLIA 1 (p < 0.01 or p < 0.05) compared with those of SLA and M substrates. These results indicate that the micro-nano structure fabricated by electrochemical etching method is beneficial for the biological functions of MG63 cells and may be a promising candidate in dental implants. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 757-769, 2017. © 2016 Wiley Periodicals, Inc.

An in vitro assessment of titanium functionalized with polysaccharides conjugated with vascular endothelial growth factor for enhanced osseointegration and inhibition of bacterial adhesion.

PubMed

Hu, Xuefeng; Neoh, Koon-Gee; Shi, Zhilong; Kang, En-Tang; Poh, Chyekhoon; Wang, Wilson

2010-12-01

The long-term success of orthopedic implants may be compromised by defective osseointegration and bacterial infection. An effective approach to minimize implant failure would be to modify the surface of the implant to make it habitable for bone-forming cells and anti-infective at the same time. In this in vitro study, the surfaces of titanium (Ti) substrates were functionalized by first covalently grafting either dopamine followed by carboxymethyl chitosan (CMCS) or hyaluronic acid-catechol (HAC). Vascular endothelial growth factor (VEGF) was then conjugated to the polysaccharide-grafted surface. Antibacterial assay with Staphylococcus aureus (S. aureus) showed that the polysaccharide-modified substrates significantly decrease bacterial adhesion. The CMCS-functionalized Ti demonstrated better antibacterial property than the HAC-functionalized Ti since CMCS is bactericidal while HA only inhibits the adhesion of bacteria without killing them. Osteoblast attachment, as well as alkaline phosphatase (ALP) activity and calcium deposition were enhanced by the immobilized VEGF on the polysaccharide-grafted Ti. Thus, Ti substrates modified with polysaccharides conjugated with VEGF can promote osteoblast functions and concurrently reduce bacterial adhesion. Since VEGF is also known to enhance angiogenesis, the VEGF-polysaccharide functionalized substrates will have promising applications in the orthopedic field. Copyright © 2010 Elsevier Ltd. All rights reserved.

Surface enhanced raman spectroscopy technique in rapid detection of live and dead salmonella cells

USDA-ARS?s Scientific Manuscript database

Many research proved that Surface Enhanced Raman Spectroscopy (SERS) can detect pathogens rapidly and accurately. In this study, a silver metal substrate was used for the selected common food pathogen Salmonella typhimurium bacteria. Nano silver rods were deposited on a thin titanium coating over t...

Biological Behavior of Osteoblast Cell and Apatite Forming Ability of the Surface Modified Ti Alloys.

PubMed

Zhao, Jingming; Hwang, K H; Choi, W S; Shin, S J; Lee, J K

2016-02-01

Titanium as one kind of biomaterials comes in direct contact with the body, making evaluation of biocompatibility an important aspect to biomaterials development. Surface chemistry of titanium plays an important role in osseointegration. Different surface modification alters the surface chemistry and result in different biological response. In this study, three kinds of mixed acid solutions were used to treat Ti specimens to induce Ca-P formation. Following a strong mixed acid activation process, Ca-P coating successfully formed on the Ti surfaces in simulated body fluid. Strong mixed acid increased the roughness of the metal surface, because the porous and rough surface allows better adhesion between Ca-P coatings and substrates. After modification of titanium surface by mixed acidic solution and subsequently H2O2/HCL treatment evaluation of biocompatibility was conducted from hydroxyapatite formation by biomimetic process and cell viability on modified titanium surface. Nano-scale modification of titanium surfaces can alter cellular and tissue responses, which may benefit osseointegration and dental implant therapy. Results from this study indicated that surface treatment methods affect the surface morphology, type of TiO2 layer formed and subsequent apatite deposition and biological responses. The thermo scientific alamarblue cell viability assay reagent is used to quantitatively measure the viability of mammalian cell lines, bacteria and fungi by incorporating a rapid, sensitive and reliable fluorometric/colorimetric growth indicator, without any toxic and side effect to cell line. In addition, mixed acid treatment uses a lower temperature and shorter time period than widely used alkali treatment.

Titanium based flat heat pipes for computer chip cooling

NASA Astrophysics Data System (ADS)

Soni, Gaurav; Ding, Changsong; Sigurdson, Marin; Bozorgi, Payam; Piorek, Brian; MacDonald, Noel; Meinhart, Carl

2008-11-01

We are developing a highly conductive flat heat pipe (called Thermal Ground Plane or TGP) for cooling computer chips. Conventional heat pipes have circular cross sections and thus can't make good contact with chip surface. The flatness of our TGP will enable conformal contact with the chip surface and thus enhance cooling efficiency. Another limiting factor in conventional heat pipes is the capillary flow of the working fluid through a wick structure. In order to overcome this limitation we have created a highly porous wick structure on a flat titanium substrate by using micro fabrication technology. We first etch titanium to create very tall micro pillars with a diameter of 5 μm, a height of 40 μm and a pitch of 10 μm. We then grow a very fine nano structured titania (NST) hairs on all surfaces of the pillars by oxidation in H202. In this way we achieve a wick structure which utilizes multiple length scales to yield high performance wicking of water. It's capable of wicking water at an average velocity of 1 cm/s over a distance of several cm. A titanium cavity is laser-welded onto the wicking substrate and a small quantity of water is hermetically sealed inside the cavity to achieve a TGP. The thermal conductivity of our preliminary TGP was measured to be 350 W/m-K, but has the potential to be several orders of magnitude higher.

Osteoconductive phosphoserine-modified poly(ε-lysine) dendrons: synthesis, titanium oxide surface functionalization and response of osteoblast-like cell lines

PubMed Central

Meikle, S. T.; Bianchi, G.; Olivier, G.; Santin, M.

2013-01-01

The lack of direct bonding between the surface of an implant and the mineralized bony tissue is among the main causes of aseptic loosening in titanium-based implants. Surface etching and ceramic coatings have led to improved osteointegration, but their clinical performance is still limited either by partial bonding or by coating delamination. In this work, a solid-phase synthesis method has been optimized to produce poly(ε-lysine) dendrons, the outermost branching generation of which is functionalized by phosphoserine (PS), a known catalyst of the biomineralization process. The dendrons were deposited onto etched titanium oxide surfaces as a near-to-monolayer film able to induce the formation of a homogeneous calcium phosphate phase in a simulated body fluid over 3 days. The dendron films also stimulated MG63 and SAOS-2 osteoblast-like cells to proliferate at a rate significantly higher than etched titanium, with SAOS-2 also showing a higher degree of differentiation over 14 days. PS-tethered dendron films were not affected by various sterilization methods and UV treatment appeared to improve the cell substrate potential of these films, thus suggesting their potential as a surface functionalization method for bone implants. PMID:23193106

Adhesion of Porphyromonas gingivalis and Tannerella forsythia to dentin and titanium with sandblasted and acid etched surface coated with serum and serum proteins - An in vitro study.

PubMed

Eick, Sigrun; Kindblom, Christian; Mizgalska, Danuta; Magdoń, Anna; Jurczyk, Karolina; Sculean, Anton; Stavropoulos, Andreas

2017-03-01

To evaluate the adhesion of selected bacterial strains incl. expression of important virulence factors at dentin and titanium SLA surfaces coated with layers of serum proteins. Dentin- and moderately rough SLA titanium-discs were coated overnight with human serum, or IgG, or human serum albumin (HSA). Thereafter, Porphyromonas gingivalis, Tannerella forsythia, or a six-species mixture were added for 4h and 24h. The number of adhered bacteria (colony forming units; CFU) was determined. Arg-gingipain activity of P. gingivalis and mRNA expressions of P. gingivalis and T. forsythia proteases and T. forsythia protease inhibitor were measured. Coating specimens never resulted in differences exceeding 1.1 log10 CFU, comparing to controls, irrespective the substrate. Counts of T. forsythia were statistically significantly higher at titanium than dentin, the difference was up to 3.7 log10 CFU after 24h (p=0.002). No statistically significant variation regarding adhesion of the mixed culture was detected between surfaces or among coatings. Arg-gingipain activity of P. gingivalis was associated with log10 CFU but not with the surface or the coating. Titanium negatively influenced mRNA expression of T. forsythia protease inhibitor at 24h (p=0.026 uncoated, p=0.009 with serum). The present findings indicate that: a) single bacterial species (T. forsythia) can adhere more readily to titanium SLA than to dentin, b) low expression of T. forsythia protease inhibitor may influence the virulence of the species on titanium SLA surfaces in comparison with teeth, and c) surface properties (e.g. material and/or protein layers) do not appear to significantly influence multi-species adhesion. Copyright © 2016 Elsevier Ltd. All rights reserved.

Topography and nanostructural evaluation of chemically and thermally modified titanium substrates.

PubMed

Salemi, Hoda; Behnamghader, Aliasghar; Afshar, Abdollah

2016-10-01

In this research, the effects of chemical and thermal treatment on the morphological and compositional aspects of titanium substrates and so, potentially, on development of biomimetic bone like layers formation during simulated body fluid (SBF) soaking was investigated. The HF, HF/HNO3 and NaOH solutions were used for chemical treatment and some of alkali-treated samples followed a heat treatment at 600°C. The treated samples before and after soaking were subjected to material characterization tests using scanning electron microscopy (SEM), X-ray diffraction (XRD) and atomic force microscopy (AFM). White light interferometry (WLI) was used to determine the roughness parameters such as Ra, Rq, RKu and Rsk. The significance of the obtained data was assessed using ANOVA variance analysis between all samples. It was observed that the reaction at grain boundaries and sodium titanate intermediate layers play a great role in the nucleation of calcium phosphate layers. Based on the obtained results in this work, the calcium phosphate microstructure deposited on titanium substrates was more affected by chemical modification than surface topography.

Microstructure, nickel suppression and mechanical characteristics of electropolished and photoelectrocatalytically oxidized biomedical nickel titanium shape memory alloy.

PubMed

Chu, C L; Guo, C; Sheng, X B; Dong, Y S; Lin, P H; Yeung, K W K; Chu, Paul K

2009-07-01

A new surface modification protocol encompassing an electropolishing pretreatment (EP) and subsequent photoelectrocatalytic oxidation (PEO) has been developed to improve the surface properties of biomedical nickel titanium (NiTi) shape memory alloy (SMA). Electropolishing is a good way to improve the resistance to localized breakdown of NiTi SMA whereas PEO offers the synergistic effects of advanced oxidation and electrochemical oxidation. Our results indicate that PEO leads to the formation of a sturdy titania film on the EP NiTi substrate. There is an Ni-free zone near the top surface and a graded interface between the titania layer and NiTi substrate, which bodes well for both biocompatibility and mechanical stability. In addition, Ni ion release from the NiTi substrate is suppressed, as confirmed by the 10-week immersion test. The modulus and hardness of the modified NiTi surface increase with larger indentation depths, finally reaching plateau values of about 69 and 3.1GPa, respectively, which are slightly higher than those of the NiTi substrate but much lower than those of a dense amorphous titania film. In comparison, after undergoing only EP, the mechanical properties of NiTi exhibit an inverse change with depth. The deformation mechanism is proposed and discussed. Our results indicate that surface modification by dual EP and PEO can notably suppress Ni ion release and improve the biocompatibility of NiTi SMA while the surface mechanical properties are not compromised, making the treated materials suitable for hard tissue replacements.

Porous TiO₂ surface formed on nickel-titanium alloy by plasma electrolytic oxidation: a prospective polymer-free reservoir for drug eluting stent applications.

PubMed

Huan, Zhiguang; Fratila-Apachitei, Lidy E; Apachitei, Iulian; Duszczyk, Jurek

2013-07-01

In this study, a porous oxide layer was formed on the surface of nickel-titanium alloy (NiTi) by plasma electrolytic oxidation (PEO) with the aim to produce a polymer-free drug carrier for drug eluting stent (DES) applications. The oxidation was performed galvanostatically in concentrated phosphoric acid electrolyte at low temperature. It was found that the response of NiTi substrate during the PEO process was different from that of bulk Ti, since the presence of large amount of Ni delayed the initial formation of a compact oxide layer that is essential for the PEO to take place. Under optimized PEO conditions, the resultant surface showed porosity, pore density and oxide layer thickness of 14.11%, 2.40 × 10⁵ pores/mm² and 0.8 μm, respectively. It was additionally noted that surface roughness after PEO did not significantly increase as compared with that of original NiTi substrate and the EDS analyses revealed a decrease in Ni/Ti ratio on the surface after PEO. The cross-section morphology showed no discontinuity between the PEO layer and the NiTi substrate. Furthermore, wettability and surface free energy of the NiTi substrate increased significantly after PEO treatment. The PEO process could be successfully translated to NiTi stent configuration proving for the first time its feasibility for such a medical device and offering potential for development of alternative, polymer-free drug carriers for NiTi DES. Copyright © 2013 Wiley Periodicals, Inc.

Characterization and evaluation of femtosecond laser-induced sub-micron periodic structures generated on titanium to improve osseointegration of implants

NASA Astrophysics Data System (ADS)

Lee, Bryan E. J.; Exir, Hourieh; Weck, Arnaud; Grandfield, Kathryn

2018-05-01

Reproducible and controllable methods of modifying titanium surfaces for dental and orthopaedic applications are of interest to prevent poor implant outcomes by improving osseointegration. This study made use of a femtosecond laser to generate laser-induced periodic surface structures with periodicities of 300, 620 and 760 nm on titanium substrates. The reproducible rippled patterns showed consistent submicron scale roughness and relatively hydrophobic surfaces as measured by atomic force microscopy and contact angle, respectively. Transmission electron microscopy and Auger electron spectroscopy identified a thicker oxide layer on ablated surfaces compared to controls. In vitro testing was conducted using osteosarcoma Saos-2 cells. Cell metabolism on the laser-ablated surfaces was comparable to controls and alkaline phosphatase activity was notably increased at late time points for the 620 and 760 nm surfaces compared to controls. Cells showed a more elongated shape on laser-ablated surfaces compared to controls and showed perpendicular alignment to the periodic structures. This work has demonstrated the feasibility of generating submicron features on an implant material with the ability to influence cell response and improve implant outcomes.

Optimization of Oxidation Temperature for Commercially Pure Titanium to Achieve Improved Corrosion Resistance

NASA Astrophysics Data System (ADS)

Bansal, Rajesh; Singh, J. K.; Singh, Vakil; Singh, D. D. N.; Das, Parimal

2017-03-01

Thermal oxidation of commercially pure titanium (cp-Ti) was carried out at different temperatures, ranging from 200 to 900 °C to achieve optimum corrosion resistance of the thermally treated surface in simulated body fluid. Scanning electron microscopy, x-ray diffraction, Raman spectroscopy and electrochemical impedance spectroscopy techniques were used to characterize the oxides and assess their protective properties exposed in the test electrolyte. Maximum resistance toward corrosion was observed for samples oxidized at 500 °C. This was attributed to the formation of a composite layer of oxides at this temperature comprising Ti2O3 (titanium sesquioxide), anatase and rutile phases of TiO2 on the surface of cp-Ti. Formation of an intact and pore-free oxide-substrate interface also improved its corrosion resistance.

PEM Anchorage on Titanium Using Catechol Grafting

PubMed Central

Marie, Hélène; Barrere, Amélie; Schoentstein, Frédérique; Chavanne, Marie-Hélène; Grosgogeat, Brigitte; Mora, Laurence

2012-01-01

Background This study deals with the anchorage of polyelectrolyte films onto titanium surfaces via a cathecol-based linker for biomedical applications. Methodology The following study uses a molecule functionalized with a catechol and a carboxylic acid: 3-(3,4-dihydroxyphenyl)propanoic acid. This molecule is anchored to the TiO2 substrate via the catechol while the carboxylic acid reacts with polymers bearing amine groups. By providing a film anchorage of chemisorption type, it makes possible to deposit polyelectrolytes on the surface of titanium. Principal Findings Infrared spectroscopy (ATR-FTIR), X-ray photoelectron spectroscopy (XPS), contact angle and atomic force microscopy (AFM) measurements show that the different steps of grafting have been successfully performed. Conclusions This method based on catechol anchorage of polyelectrolytes open a window towards large possibilities of clinical applications. PMID:23226262

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, S. K.; Mohan, S.; Bysakh, S.

The formation of surface oxide layer as well as compositional changes along the thickness for NiTi shape memory alloy thin films deposited by direct current magnetron sputtering at substrate temperature of 300 °C in the as-deposited condition as well as in the postannealed (at 600 °C) condition have been thoroughly studied by using secondary ion mass spectroscopy, x-ray photoelectron spectroscopy, and scanning transmission electron microscopy-energy dispersive x-ray spectroscopy techniques. Formation of titanium oxide (predominantly titanium dioxide) layer was observed in both as-deposited and postannealed NiTi films, although the oxide layer was much thinner (8 nm) in as-deposited condition. The depletionmore » of Ti and enrichment of Ni below the oxide layer in postannealed films also resulted in the formation of a graded microstructure consisting of titanium oxide, Ni{sub 3}Ti, and B2 NiTi. A uniform composition of B2 NiTi was obtained in the postannealed film only below a depth of 200–250 nm from the surface. Postannealed film also exhibited formation of a ternary silicide (Ni{sub x}Ti{sub y}Si) at the film–substrate interface, whereas no silicide was seen in the as-deposited film. The formation of silicide also caused a depletion of Ni in the film in a region ∼250–300 nm just above the film substrate interface.« less

Characterization of a Surface-Flashover Ion Source with 10-250 ns Pulse Widths

NASA Astrophysics Data System (ADS)

Falabella, S.; Guethlein, G.; Kerr, P. L.; Meyer, G. A.; Morse, J. D.; Sampayan, S.; Tang, V.

2009-03-01

As a step towards developing an ultra compact D-D neutron source for various defense and homeland security applications, a compact ion source is needed. Towards that end, we are testing a pulsed, surface flashover source, with deuterated titanium films deposited on alumina substrates as the electrodes. An electrochemically-etched mask was used to define the electrode areas on the substrate during the sputtered deposition of the titanium films. Deuterium loading of the films was performed in an all metal-sealed vacuum chamber containing a heated stage. Deuterium ion current from the source was determined by measuring the neutrons produced when the ions impacted a deuterium-loaded target held at -90 kV. As the duration of the arc current is varied, it was observed that the integrated deuteron current per pulse initially increases rapidly, then reaches a maximum near a pulse length of 100 ns.

In situ fabrication of silver nanoparticle-filled hydrogen titanate nanotube layer on metallic titanium surface for bacteriostatic and biocompatible implantation

PubMed Central

Wang, Zheng; Sun, Yan; Wang, Dongzhou; Liu, Hong; Boughton, Robert I

2013-01-01

A silver nanoparticle (AgNP)-filled hydrogen titanate nanotube layer was synthesized in situ on a metallic titanium substrate. In the synthesis approach, a layer of sodium titanate nanotubes is first prepared on the titanium surface by using a hydrothermal method. Silver nitrate solution is absorbed into the nanotube channels by immersing a dried nanotube layer in silver nitrate solution. Finally, silver ions are reduced by glucose, leading to the in situ growth of AgNPs in the hydrogen titanate nanotube channels. Long-term silver release and bactericidal experiments demonstrated that the effective silver release and effective antibacterial period of the titanium foil with a AgNP-filled hydrogen titanate nanotube layer on the surface can extend to more than 15 days. This steady and prolonged release characteristic is helpful to promote a long-lasting antibacterial capability for the prevention of severe infection after surgery. A series of antimicrobial and biocompatible tests have shown that the sandwich nanostructure with a low level of silver loading exhibits a bacteriostatic rate as high as 99.99%, while retaining low toxicity for cells and possessing high osteogenic potential. Titanium foil with a AgNP-filled hydrogen titanate nanotube layer on the surface that is fabricated with low-cost surface modification methods is a promising implantable material that will find applications in artificial bones, joints, and dental implants. PMID:23966780

Thin Bioactive Zn Substituted Hydroxyapatite Coating Deposited on Ultrafine Grained Titanium Substrate: Structure Analysis

NASA Astrophysics Data System (ADS)

Prosolov, Konstantin A.; Belyavskaya, Olga A.; Muehle, Uwe; Sharkeev, Yurii P.

2018-02-01

Nanocrystalline Zn substituted hydroxyapatite coatings were deposited by radiofrequency magnetron sputtering on the surface of ultrafine-grained titanium substrates. Cross section transmission electron microscopy provided information about the morphology and texture of the thin film while in-column energy dispersive X-ray analysis confirmed the presence of Zn in the coating. The Zn substituted hydroxyapatite coating was formed by an equiaxed polycrystalline grain structure. Effect of substrate crystallinity on the structure of deposited coating is discussed. An amorphous TiO2 sublayer of 8 nm thickness was detected in the interface between the polycrystalline coating and the Ti substrate. Its appearance in the amorphous state is attributed to prior to deposition etching of the substrate and subsequent condensation of oxygen-containing species sputtered from the target. This layer contributes to the high coating-to-substrate adhesion. The major P-O vibrational modes of high intensity were detected by Raman spectroscopy. The Zn substituted hydroxyapatite could be a material of choice when antibacterial osteoconductive coating with a possibility of withstanding mechanical stress during implantation and service is needed.

Surface and corrosion characteristics of carbon plasma implanted and deposited nickel-titanium alloy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poon, R.W.Y.; Liu, X.Y.; Chung, C.Y.

2005-05-01

Nickel-titanium shape memory alloys (NiTi) are potentially useful in orthopedic implants on account of their super-elastic and shape memory properties. However, the materials are prone to surface corrosion and the most common problem is out-diffusion of harmful Ni ions from the substrate into body tissues and fluids. In order to improve the corrosion resistance and related surface properties, we used the technique of plasma immersion ion implantation and deposition to deposit an amorphous hydrogenated carbon coating onto NiTi and implant carbon into NiTi. Both the deposited amorphous carbon film and carbon plasma implanted samples exhibit much improved corrosion resistances andmore » surface mechanical properties and possible mechanisms are suggested.« less

Surface properties, crystallinity and optical properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chuan, Lee Te, E-mail: gd130079@siswa.uthm.edu.my; Abdullah, Hasan Zuhudi, E-mail: hasan@uthm.edu.my; Idris, Maizlinda Izwana, E-mail: izwana@uthm.edu.my

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. This method has been widely used in surface modification of biomaterials especially for dental implants. In this study, the surface morphology, crystallinity and optical properties of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (5 and 10 minutes) and current density (10-70 mA.cm{sup −2}) at room temperature. Anodisedmore » titanium was characterised by using field emission scanning electron microscopy (FESEM), X-ray diffractometer (XRD), and UV-Vis spectrometry. The result of the experiment showed that surface morphology, crystallinity and optical properties depended strongly on the current density and anodising time. More porous surface and large amount of anatase and rutile was produced at higher current density and longer anodising time. Apart from that, it is also revealed that the energy band gap of anodised titanium increases as the increase in current density due to the presence of anatase and rutile TiO{sub 2}.« less

Surface properties, crystallinity and optical properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

NASA Astrophysics Data System (ADS)

Chuan, Lee Te; Abdullah, Hasan Zuhudi; Idris, Maizlinda Izwana

2015-07-01

Anodic oxidation is an electrochemical method for the production of ceramic films on a metallic substrate. It had been widely used to deposit the ceramic coatings on the metals surface. This method has been widely used in surface modification of biomaterials especially for dental implants. In this study, the surface morphology, crystallinity and optical properties of titanium foil was modified by anodising in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA). The experiments were carried out at high voltage (350 V), different anodising time (5 and 10 minutes) and current density (10-70 mA.cm-2) at room temperature. Anodised titanium was characterised by using field emission scanning electron microscopy (FESEM), X-ray diffractometer (XRD), and UV-Vis spectrometry. The result of the experiment showed that surface morphology, crystallinity and optical properties depended strongly on the current density and anodising time. More porous surface and large amount of anatase and rutile was produced at higher current density and longer anodising time. Apart from that, it is also revealed that the energy band gap of anodised titanium increases as the increase in current density due to the presence of anatase and rutile TiO2.

Co-blasting of titanium surfaces with an abrasive and hydroxyapatite to produce bioactive coatings: substrate and coating characterisation.

PubMed

Dunne, Conor F; Twomey, Barry; O'Neill, Liam; Stanton, Kenneth T

2014-01-01

The aim of this work is to assess the influence of two blast media on the deposition of hydroxyapatite onto a titanium substrate using a novel ambient temperature coating technique named CoBlast. CoBlast was developed to address the problems with high temperature coating techniques. The blasting media used in this study were Al2O3 and a sintered apatite powder. The prepared and coated surfaces were compared to plasma sprayed hydroxyapatite on the same substrates using the same hydroxyapatite feedstock powder. X-ray diffraction analysis revealed the coating crystallinity was the same as the original hydroxyapatite feedstock powder for the CoBlast samples while evidence of amorphous hydroxyapatite phases and β-TCP was observed in the plasma sprayed samples. The blast media type significantly influences the adhesive strength of the coating, surface roughness of both the substrate and coating and the microstructure of the substrate. The coating adhesion increased for the CoBlasted samples from 50 MPa to 60 MPa for sintered apatite powder and alumina, respectively, while plasma spray samples were significantly lower (5 MPa) when tested using a modified pull-test. In conclusion, the choice of blast medium is shown to be a key parameter in the CoBlast process. This study indicates that sintered apatite powder is the most suitable candidate for use as a blast medium in the coating of medical devices.

Preparation and in vitro evaluation of plasma-sprayed Mg(2)SiO(4) coating on titanium alloy.

PubMed

Xie, Youtao; Zhai, Wanyin; Chen, Lei; Chang, Jiang; Zheng, Xuebin; Ding, Chuanxian

2009-07-01

In this paper, chemically synthesized Mg(2)SiO(4) (MS) powder was plasma-sprayed onto a titanium alloy substrate to evaluate its application potentials in biomedicine. The phase composition and surface morphology of the MS coating were analyzed. Results showed that the MS coating was composed mainly of Mg(2)SiO(4) phase, with a small amount of MgO and glass phases. Mechanical testing showed that the coating exhibited good adhesion strength to the substrate due to the close thermal expansion coefficient between the MS ceramic and the titanium alloy substrate. The measured bonding strength was as high as 41.5+/-5.3MPa, which is much higher than the traditional HA coating. In vitro cytocompatibility evaluation of the MS coating was performed using canine bone marrow stem cells (MSCs). The MSCs exhibited good adhesion, proliferation and differentiation behavior on the MS coating surface, which can be explained by the high protein adsorption capability of the MS coating, as well as the stimulatory effects of Mg and Si ions released from the coating. The proliferation rate of the MSCs on MS coating was very close to that on the hydroxylapatite (HA) coating. Alkaline phosphatase (ALP) activity analysis demonstrated that the ALP level of the MSCs on the MS coating remained high even after 21days, implying that the surface characteristics of the coating are beneficial for the differentiation of MSCs. In summary, our results suggest that MS coating might be a new approach to prepare bone implants.

Thin films and uses

DOEpatents

Baskaran, Suresh; Graff, Gordon L.; Song, Lin

1998-01-01

The invention provides a method for synthesizing a titanium oxide-containing film comprising the following steps: (a) preparing an aqueous solution of a titanium chelate with a titanium molarity in the range of 0.01M to 0.6M. (b) immersing a substrate in the prepared solution, (c) decomposing the titanium chelate to deposit a film on the substrate. The titanium chelate maybe decomposed acid, base, temperature or other means. A preferred method provides for the deposit of adherent titanium oxide films from C2 to C5 hydroxy carboxylic acids. In another aspect the invention is a novel article of manufacture having a titanium coating which protects the substrate against ultraviolet damage. In another aspect the invention provides novel semipermeable gas separation membranes, and a method for producing them.

Modification of Titanium Substrates with Chimeric Peptides Comprising Antimicrobial and Titanium-Binding Motifs Connected by Linkers To Inhibit Biofilm Formation.

PubMed

Liu, Zihao; Ma, Shiqing; Duan, Shun; Xuliang, Deng; Sun, Yingchun; Zhang, Xi; Xu, Xinhua; Guan, Binbin; Wang, Chao; Hu, Meilin; Qi, Xingying; Zhang, Xu; Gao, Ping

2016-03-02

Bacterial adhesion and biofilm formation are the primary causes of implant-associated infection, which is difficult to eliminate and may induce failure in dental implants. Chimeric peptides with both binding and antimicrobial motifs may provide a promising alternative to inhibit biofilm formation on titanium surfaces. In this study, chimeric peptides were designed by connecting an antimicrobial motif (JH8194: KRLFRRWQWRMKKY) with a binding motif (minTBP-1: RKLPDA) directly or via flexible/rigid linkers to modify Ti surfaces. We evaluated the binding behavior of peptides using quartz crystal microbalance (QCM) and atomic force microscopy (AFM) techniques and investigated the effect of the modification of titanium surfaces with these peptides on the bioactivity of Streptococcus gordonii (S. gordonii) and Streptococcus sanguis (S. sanguis). Compared with the flexible linker (GGGGS), the rigid linker (PAPAP) significantly increased the adsorption of the chimeric peptide on titanium surfaces (p < 0.05). Concentration-dependent adsorption is consistent with a single Langmuir model, whereas time-dependent adsorption is in line with a two-domain Langmuir model. Additionally, the chimeric peptide with the rigid linker exhibited more effective antimicrobial ability than the peptide with the flexible linker. This finding was ascribed to the ability of the rigid linker to separate functional domains and reduce their interference to the maximum extent. Consequently, the performance of chimeric peptides with specific titanium-binding motifs and antimicrobial motifs against bacteria can be optimized by the proper selection of linkers. This rational design of chimeric peptides provides a promising alternative to inhibit the formation of biofilms on titanium surfaces with the potential to prevent peri-implantitis and peri-implant mucositis.

Characterization and cell behavior of titanium surfaces with PLL/DNA modification via a layer-by-layer technique.

PubMed

Gao, Wenli; Feng, Bo; Lu, Xiong; Wang, Jianxin; Qu, Shuxin; Weng, Jie

2012-08-01

This study describes the fabrication of two types of multilayered films onto titanium by layer-by-layer (LBL) self-assembly, using poly-L-lysine (PLL) as the cationic polyelectrolyte and deoxyribonucleic acid (DNA) as the anionic polyelectrolyte. The assembling process of each component was studied using atomic force microscopy (AFM) and quartz crystal balance (QCM). Zeta potential of the LBL-coated microparticles was measured by dynamic light scattering. Titanium substrates with or without multilayered films were used in osteoblast cell culture experiments to study cell proliferation, viability, differentiation, and morphology. Results of AFM and QCM indicated the progressive build-up of the multilayered coatings. The surface morphology of three types of multilayered films showed elevations in the nanoscale range. The data of zeta potential showed that the surface terminated with PLL displayed positive charge while the surface terminated with DNA displayed negative charge. The proliferation of osteoblasts on modified titanium films was found to be greater than that on control (p < 0.05) after 3 and 7 days culture, respectively. Alamar blue measurement showed that the PLL/DNA-modified films have higher cell viability (p < 0.05) than the control. Still, the alkaline phosphatase activity assay revealed a better differentiated phenotype on three types of multilayered surfaces compared to noncoated controls. Collectively our results suggest that PLL/DNA were successfully used to surface engineer titanium via LBL technique, and enhanced its cell biocompatibility. Copyright © 2012 Wiley Periodicals, Inc.

Microstructure and high-temperature oxidation resistance of TiN/Ti3Al intermetallic matrix composite coatings on Ti6Al4V alloy surface by laser cladding

NASA Astrophysics Data System (ADS)

Zhang, Xiaowei; Liu, Hongxi; Wang, Chuanqi; Zeng, Weihua; Jiang, Yehua

2010-11-01

A high-temperature oxidation resistant TiN embedded in Ti3Al intermetallic matrix composite coating was fabricated on titanium alloy Ti6Al4V surface by 6kW transverse-flow CO2 laser apparatus. The composition, morphology and microstructure of the laser clad TiN/Ti3Al intermetallic matrix composite coating were characterized by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometer (EDS). In order to evaluate the high-temperature oxidation resistance of the composite coatings and the titanium alloy substrate, isothermal oxidation test was performed in a conventional high-temperature resistance furnace at 600°C and 800°C respectively. The result shows that the laser clad intermetallic composite coating has a rapidly solidified fine microstructure consisting of TiN primary phase (granular-like, flake-like, and dendrites), and uniformly distributed in the Ti3Al matrix. It indicates that a physical and chemical reaction between the Ti powder and AlN powder occurred completely under the laser irradiation. In addition, the microhardness of the TiN/Ti3Al intermetallic matrix composite coating is 844HV0.2, 3.4 times higher than that of the titanium alloy substrate. The high-temperature oxidation resistance test reveals that TiN/Ti3Al intermetallic matrix composite coating results in the better modification of high-temperature oxidation behavior than the titanium substrate. The excellent high-temperature oxidation resistance of the laser cladding layer is attributed to the formation of the reinforced phase TiN and Al2O3, TiO2 hybrid oxide. Therefore, the laser cladding TiN/Ti3Al intermetallic matrix composite coating is anticipated to be a promising oxidation resistance surface modification technique for Ti6Al4V alloy.

Methods of Antimicrobial Coating of Diverse Materials

NASA Technical Reports Server (NTRS)

Akse, James R.; Holtsnider, John T.; Kliestik, Helen

2011-01-01

Methods of coating diverse substrate materials with antimicrobial agents have been developed. Originally intended to reduce health risks to astronauts posed by pathogenic microorganisms that can grow on surfaces in spacecraft, these methods could also be used on Earth for example, to ensure sterility of surgical inserts and other medical equipment. The methods involve, generally, chemical preparation of substrate surfaces to enable attachment of antimicrobial molecules to the substrate surfaces via covalent bonds. Substrate materials that have been treated successfully include aluminum, glass, a corrosion-resistant nickel alloy, stainless steel, titanium, and poly(tetrafluoroethylene). Antimicrobial agents that have been successfully immobilized include antibiotics, enzymes, bacteriocins, bactericides, and fungicides. A variety of linkage chem istries were employed. Activity of antimicrobial coatings against gram-positive bacteria, gram-negative bacteria, and fungi was demonstrated. Results of investigations indicate that the most suitable combination of antimicrobial agent, substrate, and coating method depends upon the intended application.

Direct growth of cerium oxide nanorods on diverse substrates for superhydrophobicity and corrosion resistance

NASA Astrophysics Data System (ADS)

Cho, Young Jun; Jang, Hanmin; Lee, Kwan-Soo; Kim, Dong Rip

2015-06-01

Superhydrophobic surfaces with anti-corrosion properties have attracted great interest in many industrial fields, particularly to enhance the thermal performance of offshore applications such as heat exchangers, pipelines, power plants, and platform structures. Nanostructures with hydrophobic materials have been widely utilized to realize superhydrophobicity of surfaces, and cerium oxide has been highlighted due to its good corrosion resistive and intrinsically hydrophobic properties. However, few studies of direct growth of cerium oxide nanostructures on diverse substrates have been reported. Herein we report a facile hydrothermal method to directly grow cerium oxide nanorods on diverse substrates, such as aluminum alloy, stainless steel, titanium, and silicon. Diverse substrates with cerium oxide nanorods exhibited superhydrophobicity with no hydrophobic modifiers on their surfaces, and showed good corrosion resistive properties in corrosive medium. We believe our method could pave the way for realization of scalable and sustainable corrosion resistive superhydrophobic surfaces in many industrial fields.

Highly efficient TiO2-based microreactor for photocatalytic applications.

PubMed

Krivec, Matic; Žagar, Kristina; Suhadolnik, Luka; Čeh, Miran; Dražić, Goran

2013-09-25

A photocatalytic, TiO2-based microreactor is designed and fabricated on a metal-titanium foil. The microchannel is mechanically engraved in the substrate foil, and a double-layered TiO2 anatase film is immobilized on its inner walls with a two-step synthesis, which included anodization and a hydrothermal treatment. X-ray diffraction (XRD) and scanning electron microscopy (SEM) confirm the presence of an approximately 10-μm-thick layer of titania nanotubes and anatase nanoparticles. The SEM and transmission electron microscopy (TEM) of the cross sections show a dense interface between the titanium substrate and the TiO2 nanotubes. An additional layer of TiO2-anatase nanoparticles on the top of the film provides a large, photocatalytic surface area. The metal-titanium substrate with a functionalized serpentine channel is sealed with UV-transparent Plexiglas, and four 0.8-mW UV LEDs combined with a power controller on a small printed-circuit board are fixed over the substrate. The photocatalytic activity and the kinetic properties for the degradation of caffeine are provided, and the longer-term stability of the TiO2 film is evaluated. The results show that after 6 months of use and 3600 working cycles the microreactor still exhibits 60% of its initial efficiency.

Effect of hot water and heat treatment on the apatite-forming ability of titania films formed on titanium metal via anodic oxidation in acetic acid solutions.

PubMed

Cui, Xinyu; Kim, Hyun-Min; Kawashita, Masakazu; Wang, Longbao; Xiong, Tianying; Kokubo, Tadashi; Nakamura, Takashi

2008-04-01

Titanium and its alloys have been widely used for orthopedic implants because of their good biocompatibility. We have previously shown that the crystalline titania layers formed on the surface of titanium metal via anodic oxidation can induce apatite formation in simulated body fluid, whereas amorphous titania layers do not possess apatite-forming ability. In this study, hot water and heat treatments were applied to transform the titania layers from an amorphous structure into a crystalline structure after titanium metal had been anodized in acetic acid solution. The apatite-forming ability of titania layers subjected to the above treatments in simulated body fluid was investigated. The XRD and SEM results indicated hot water and/or heat treatment could greatly transform the crystal structure of titania layers from an amorphous structure into anatase, or a mixture of anatase and rutile. The abundance of Ti-OH groups formed by hot water treatment could contribute to apatite formation on the surface of titanium metals, and subsequent heat treatment would enhance the bond strength between the apatite layers and the titanium substrates. Thus, bioactive titanium metals could be prepared via anodic oxidation and subsequent hot water and heat treatment that would be suitable for applications under load-bearing conditions.

Anodized porous titanium coated with Ni-CeO2 deposits for enhancing surface toughness and wear resistance

NASA Astrophysics Data System (ADS)

Zhou, Xiaowei; Ouyang, Chun

2017-05-01

In order to make large improvements of surface toughness and wear resistance for pure titanium (Ti) substrate, anodic titanium oxide (ATO) surface with nanoporous structure was coated with the Ni-CeO2 nanocomposite coatings. Regarding TiO2 barrier layer on Ti surface to inhibit its electrochemical activity, pre-treatments were successively processed with anodizing, sensitizing, activating, and then followed by electroless Ni-P film to be acted as an activated layer for electroplating Ni-CeO2 deposits. The existing Pd atoms around ATO nanopores were expected as the heterogeneous nucleation sites for supporting the growing locations of electroless Ni-P film. The innovative of interface design using porous structure was introduced for bonding pinholes to achieve a metallurgical adhesion interface between Ti substrate and surface coatings. Besides the objectives of this work were to elucidate how effects by the adding CeO2 nanoparticles on modifying microstructures and wear mechanisms of Ni-CeO2 nanocomposite coatings. Many efforts of XRD, FE-SEM, TEM and Nanoindentation tests were devoted to comparing different wear behaviors of Ni-CeO2 coatings relative to pure nickel. Results indicated that uniform-distributed Ti nanopores with an average diameter size of ∼200 nm was achieved using the Phosphate-type anodizing solution at DC 150 V. A worn surface without fatigue cracks was observed for TAO surface coated with Ni-CeO2 deposits, showing the existing Ce-rich worn products to be acted as a solid lubricant phase for making a self-healing effect on de-lamination failures. More important, this finding will be the guidelines for Ce-rich precipitations to be expected as the strengthening phase in anodized porous of Ti, Al and Mg alloys for intensifying their surface properties.

The Interface Structure of High-Temperature Oxidation-Resistant Aluminum-Based Coatings on Titanium Billet Surface

NASA Astrophysics Data System (ADS)

Xu, Zhefeng; Rong, Ju; Yu, Xiaohua; Kun, Meng; Zhan, Zhaolin; Wang, Xiao; Zhang, Yannan

2017-10-01

A new type of high-temperature oxidation-resistant aluminum-based coating, on a titanium billet surface, was fabricated by the cold spray method, at a high temperature of 1050°C, for 8 h, under atmospheric pressure. The microstructure of the exposed surface was analyzed via optical microscopy, the microstructure of the coating and elemental diffusion was analyzed via field emission scanning electron microscopy, and the interfacial phases were identified via x-ray diffraction. The Ti-Al binary phase diagram and Gibbs free energy of the stable phase were calculated by Thermo-calc. The results revealed that good oxidation resistant 50-μm-thick coatings were successfully obtained after 8 h at 1050°C. Two layers were obtained after the coating process: an Al2O3 oxidation layer and a TiAl3 transition layer on the Ti-based substrate. The large and brittle Al2O3 grains on the surface, which can be easily spalled off from the surface after thermal processing, protected the substrate against oxidation during processing. In addition, the thermodynamic calculation results were in good agreement with the experimental data.

Effect of power and type of substrate on calcium-phosphate coating morphology and microhardness

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kulyashova, Ksenia, E-mail: kseniya@ispms.tsc.ru; Glushko, Yurii, E-mail: glushko@ispms.tsc.ru; Sharkeev, Yurii, E-mail: sharkeev@ispms.tsc.ru

2015-10-27

As known, the influence of the different sputtering process parameters and type of substrate on structure of the deposited coating is important to identify, because these parameters are significantly affected on structure of coating. The studies of the morphology and microhardness of calcium-phosphate (CaP) coatings formed and obtained on the surface of titanium, zirconium, titanium and niobium alloy for different values of the power of radio frequency discharge are presented. The increase in the radio frequency (rf) magnetron discharge leads to the formation of a larger grain structure of the coating. The critical depths of indentation for coatings determining themore » value of their microhardness have been estimated. Mechanical properties of the composite material on the basis of the bioinert substrate metal and CaP coatings are superior to the properties of the separate components that make up this composite material.« less

Construction of surface HA/TiO2 coating on porous titanium scaffolds and its preliminary biological evaluation.

PubMed

Chen, Hongjie; Wang, Chunli; Yang, Xiao; Xiao, Zhanwen; Zhu, Xiangdong; Zhang, Kai; Fan, Yujiang; Zhang, Xingdong

2017-01-01

A simple approach to fabricating hydroxyxapatite/titanium dioxide (HA/TiO 2 ) coating on porous titanium (Ti) scaffolds was developed in the present study. Surface TiO 2 layer was firstly formed on porous Ti scaffolds with multi-scale pores by acid-alkali (AA) treatment. The outer HA layer was then formed on the TiO 2 layer by subsequent pulse electrochemical deposition (ED) technique. All the three main process parameters, i.e. deposition times, current density and mass transfer mode affected the properties of the HA coating notably. Under the conditions of 90 deposition cycles, -10mA/cm 2 of pulse current density and stirring, a thin layer of homogeneous and nanorod-like HA sediments was formed on the substrate surface of porous Ti scaffolds. The results of protein adsorption and cellular experiments showed that compared to the single TiO 2 surface, the HA/TiO 2 surface allowed more adsorption of serum proteins and further enhanced the alkaline phosphatase (ALP) activity of MC3T3-E1 osteoblasts. Copyright © 2016 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Korol, A.A.; Korol, Y.A.; Kasich-Pilipenko, I.Y.

Melted slip coatings were obtained and the structural changes in the coatings and their substrates upon simultaneous heating by concentrated solar radiant energy fluxes were studied. Well known wear and corrosion resistant TiC-Ni-B and WC-Ni-B coatings 50 to 300 microns thick applied by the slip method to flat or cylindrical stainless steel and titanium specimens were examined. The specimens were heated in an SGU-5 solar heating installation with a 2 m diameter parabolic mirror concentrator in a process chamber with a quartz window under a vacuum. Metallographic analysis revealed a finely dispersed heterogeneous structure with no visible porosity, good bondingmore » of coating to substrate, and uniform distribution of carbide phase in the metal matrix of the TiC-Ni-B coatings on titanium. Results were similar for the other coatings, indicating that concentrated solar energy can produce coatings with satisfactory surface quality, good density, and a framework structure. The coating interacted with the substrate by diffusion. Most of the volume of the substrate underwent no significant changes, indicating good bond strength between coatings and substrate.« less

The relationship between substrate morphology and biological performances of nano-silver-loaded dopamine coatings on titanium surfaces

PubMed Central

Zhang, Weibo; Wang, Shuang; Ge, Shaohua; Ji, Ping

2018-01-01

Biomedical device-associated infection (BAI) and lack of osseointegration are the main causes of implant failure. Therefore, it is imperative for implants not only to depress microbial activity and biofilm colonization but also to prompt osteoblast functions and osseointegration. As part of the coating development for implants, the interest of in vitro studies on the interaction between implant substrate morphology and the coating's biological performances is growing. In this study, by harnessing the adhesion and reactivity of bioinspired polydopamine, nano-silver was successfully anchored onto micro/nanoporous as well as smooth titanium surfaces to analyse the effect of substrate morphology on biological performances of the coatings. Compared with the smooth surface, a small size of nano-silver and high silver content was found on the micro/nanoporous surface. More mineralization happened on the coating on the micro/nanoporous structure than on the smooth surface, which led to a more rapid decrease of silver release from the micro/nanoporous surface. Antimicrobial tests indicated that both surfaces with resulting coating inhibit microbial colonization on them and growth around them, indicating that the coating eliminates the shortcoming of the porous structure which render the implant extremely susceptible to BAI. Besides, the multiple osteoblast responses of nano-silver-loaded dopamine coatings on both surfaces, i.e. attachment, proliferation and differentiation, have deteriorated, however the mineralized surfaces of these coatings stimulated osteoblast proliferation and differentiation, especially for the micro/nanoporous surface. Therefore, nano-silver-loaded dopamine coatings on micro/nanoporous substratum may not only reduce the risk of infection but also facilitate mineralization during the early post-operative period and then promote osseointegration owing to the good osteoblast-biocompatibility of the mineralized surface. These results clearly highlight the influence of the substrate morphology on the biological performances of implant coating. PMID:29765680

Experimental design and analysis of activators regenerated by electron transfer-atom transfer radical polymerization experimental conditions for grafting sodium styrene sulfonate from titanium substrates.

PubMed

Foster, Rami N; Johansson, Patrik K; Tom, Nicole R; Koelsch, Patrick; Castner, David G

2015-09-01

A 2 4 factorial design was used to optimize the activators regenerated by electron transfer-atom transfer radical polymerization (ARGET-ATRP) grafting of sodium styrene sulfonate (NaSS) films from trichlorosilane/10-undecen-1-yl 2-bromo-2-methylpropionate (ester ClSi) functionalized titanium substrates. The process variables explored were: (1) ATRP initiator surface functionalization reaction time; (2) grafting reaction time; (3) CuBr 2 concentration; and (4) reducing agent (vitamin C) concentration. All samples were characterized using x-ray photoelectron spectroscopy (XPS). Two statistical methods were used to analyze the results: (1) analysis of variance with [Formula: see text], using average [Formula: see text] XPS atomic percent as the response; and (2) principal component analysis using a peak list compiled from all the XPS composition results. Through this analysis combined with follow-up studies, the following conclusions are reached: (1) ATRP-initiator surface functionalization reaction times have no discernable effect on NaSS film quality; (2) minimum (≤24 h for this system) grafting reaction times should be used on titanium substrates since NaSS film quality decreased and variability increased with increasing reaction times; (3) minimum (≤0.5 mg cm -2 for this system) CuBr 2 concentrations should be used to graft thicker NaSS films; and (4) no deleterious effects were detected with increasing vitamin C concentration.

Medical equipment bio-capability processes using the atmospheric plasma-sprayed titanium coating

NASA Astrophysics Data System (ADS)

Rezaei, F.; Saviz, S.; Ghoranneviss, M.

2017-12-01

Antibacterial surfaces such as titanium coatings are able to have capability in the human body environment. In this study, titanium coatings are deposited on the 316 stainless steel substrates by a handmade plasma spray system. Some mechanical, chemical properties and microstructure of the created titanium layer are determined to evaluate the quality of coating. The XRD, SEM, adhesion tests from cross cut and corrosion test by potentiodynamic are used. During the different stages, some of the parameters are changed in different samples to achieve the best quality in the coating. It is shown that by increasing the spray time, the production of nanoparticles begins. On the other hand, the best layers are created when the spray main gas flow rate has a certain amount.

Properties of ordered titanium templates covered with Au thin films for SERS applications

NASA Astrophysics Data System (ADS)

Grochowska, Katarzyna; Siuzdak, Katarzyna; Sokołowski, Michał; Karczewski, Jakub; Szkoda, Mariusz; Śliwiński, Gerard

2016-12-01

Currently, roughened metal nanostructures are widely studied as highly sensitive Raman scattering substrates that show application potential in biochemistry, food safety or medical diagnostic. In this work the structural properties and the enhancement effect due to surface enhanced Raman scattering (SERS) of highly ordered nano-patterned titanium templates covered with thin (5-20 nm) gold films are reported. The templates are formed by preparation of a dense structure of TiO2 nanotubes on a flat Ti surface (2 × 2 cm2) and their subsequent etching down to the substrate. SEM images reveal the formation of honeycomb nanostructures with the cavity diameter of 80 nm. Due to the strongly inhomogeneous distribution of the electromagnetic field in the vicinity of the Au film discontinuities the measured average enhancement factor (107-108) is markedly higher than observed for bare Ti templates. The enhancement factor and Raman signal intensity can be optimized by adjusting the process conditions and thickness of the deposited Au layer. Results confirm that the obtained structures can be used in surface enhanced sensing.

Correlation between surface properties and wettability of multi-scale structured biocompatible surfaces

NASA Astrophysics Data System (ADS)

Gorodzha, S. N.; Surmeneva, M. A.; Prymak, O.; Wittmar, A.; Ulbricht, M.; Epple, M.; Teresov, A.; Koval, N.; Surmenev, R. A.

2015-11-01

The influence of surface properties of radio-frequency (RF) magnetron deposited hydroxyapatite (HA) and Si-containing HA coatings on wettability was studied. The composition and morphology of the coatings fabricated on titanium (Ti) were characterized using atomic force microscopy (AFM) and X-ray diffraction (XRD). The surface wettability was studied using contact angle analysis. Different geometric parameters of acid-etched (AE) and pulse electron beam (PEB)-treated Ti substrates and silicate content in the HA films resulted in the different morphology of the coatings at micro- and nano- length scales. Water contact angles for the HA coated Ti samples were evaluated as a combined effect of micro roughness of the substrate and nano-roughness of the HA films resulting in higher water contact angles compared with acid-etched (AE) or pulse electron beam (PEB) treated Ti substrates.

Electric Arc and Electrochemical Surface Texturing Technologies

NASA Technical Reports Server (NTRS)

Banks, Bruce A.; Rutledge, Sharon K.; Snyder, Scott A.

1997-01-01

Surface texturing of conductive materials can readily be accomplished by means of a moving electric arc which produces a plasma from the environmental gases as well as from the vaporized substrate and arc electrode materials. As the arc is forced to move across the substrate surface, a condensate from the plasma re-deposits an extremely rough surface which is intimately mixed and attached to the substrate material. The arc textured surfaces produce greatly enhanced thermal emittance and hold potential for use as high temperature radiator surfaces in space, as well as in systems which use radiative heat dissipation such as computer assisted tomography (CAT) scan systems. Electrochemical texturing of titanium alloys can be accomplished by using sodium chloride solutions along with ultrasonic agitation to produce a random distribution of craters on the surface. The crater size and density can be controlled to produce surface craters appropriately sized for direct bone in-growth of orthopaedic implants. Electric arc texturing and electrochemical texturing techniques, surface properties and potential applications will be presented.

The effect of stem surface treatment and material on pistoning of ulnar components in linked cemented elbow prostheses.

PubMed

Hosein, Yara K; King, Graham J W; Dunning, Cynthia E

2013-09-01

The ulnar component of a total elbow replacement can fail by "pistoning." Stem surface treatments have improved stability at the stem-cement interface but with varied success. This study investigated the role of surface treatment and stem substrate material on implant stability under axial loading. Sixty circular stems (diameter, 8 mm) made of cobalt chrome (n = 30) or titanium (n = 30) had different surfaces: smooth, sintered beads, and plasma spray. The surface treatment length was either 10 mm or 20 mm. Stems were potted in bone cement, allowed to cure for 24 hours, and tested in a materials testing machine under a compressive staircase loading protocol. Failure was defined as 2 mm of push-out or completion of the protocol. Two-way analyses of variance compared the effects of surface treatment and substrate material on interface strength and motion. Significant interactions were found between surface treatment and substrate material for both interface strength and motion (P < .05). For titanium, the 20-mm beaded stems had greater interface strength than all other stems (P < .05) and had less motion than the 10-mm plasma-spray and smooth stems (P < .05). For cobalt chrome, the 20-mm beaded stems showed greater interface strength (P < .05) and similar motion (P > .05) to the 20-mm plasma-spray stems (P < .05), which outperformed all other stems (P < .05). Mechanisms of catastrophic failure varied: smooth stems debonded at the stem-cement interface, beaded stems experienced debonding of the beads from the stem, and plasma-spray stems showed loss of frictional force between the surface treatment and cement. Stem surface treatment can enhance ulnar component stability but is dependent on substrate material. Copyright © 2013 Journal of Shoulder and Elbow Surgery Board of Trustees. Published by Mosby, Inc. All rights reserved.

Fabrication and Physical Properties of Titanium Nitride/Hydroxyapatite Composites on Polyether Ether Ketone by RF Magnetron Sputtering Technique

NASA Astrophysics Data System (ADS)

Nupangtha, W.; Boonyawan, D.

2017-09-01

Titanium nitride (TiN) coatings have been used very successfully in a variety of applications because of their excellent properties, such as the high hardness meaning good wear resistance and also used for covering medical implants. Hydroxyapatite is a bioactive ceramic that contributes to the restoration of bone tissue, which together with titanium nitride may contribute to obtaining a superior composite in terms of mechanical and bone tissue interaction matters. This paper aims to explain how to optimize deposition conditions for films synthesis on PEEK by varying sputtering parameters such as nitrogen flow rate and direction, deposition time, d-s (target-to-substrate distance) and 13.56 MHz RF power. The plasma conditions used to deposit films were monitored by the optical emission spectroscopy (OES). Titanium nitride/Hydroxyapatite composite films were performed by gas mixture with nitrogen and argon ratio of 1:3 and target-to-substrate distance at 8 cm. The gold colour, as-deposited film was found on PEEK with high hardness and higher surface energy than uncoated PEEK. X-ray diffraction characterization study was carried to study the crystal structural properties of these composites.

Optimization of amino group density on surfaces of titanium dioxide nanoparticles covalently bonded to a silicone substrate for antibacterial and cell adhesion activities.

PubMed

Okada, Masahiro; Yasuda, Shoji; Kimura, Tsuyoshi; Iwasaki, Mitsunobu; Ito, Seishiro; Kishida, Akio; Furuzono, Tsutomu

2006-01-01

A composite consisting of titanium dioxide (TiO2) particle, the surface of which was modified with amino groups, and a silicone substrate through covalent bonding at their interface was developed, and antibacterial and cell adhesion activities of the composite were evaluated. The density of the amino groups on the TiO2 particle surface was controlled by the reaction time of the modification reaction. The degradation rate of CH3CHO in the presence of the TiO2 particles under UV irradiation decreased with an increase in the amino group density on the TiO2 surface. On the other hand, the number of L929 cells adhering on the TiO2/silicone composite increased with an increase in the amino group density. From the above two results, the optimum density of amino groups for both photoreactivity and cell adhesiveness was estimated to be 2.0-4.0 molecules/nm2. The optimum amino group-modified TiO2/silicone composite sheet (amino group density, 3.0 molecules/nm2) showed an effective antibacterial activity for Escherichia coli bacteria under UV irradiation. (c) 2005 Wiley Periodicals, Inc

Thickness Influence on In Vitro Biocompatibility of Titanium Nitride Thin Films Synthesized by Pulsed Laser Deposition

PubMed Central

Duta, Liviu; Stan, George E.; Popa, Adrian C.; Husanu, Marius A.; Moga, Sorin; Socol, Marcela; Zgura, Irina; Miculescu, Florin; Urzica, Iuliana; Popescu, Andrei C.; Mihailescu, Ion N.

2016-01-01

We report a study on the biocompatibility vs. thickness in the case of titanium nitride (TiN) films synthesized on 410 medical grade stainless steel substrates by pulsed laser deposition. The films were grown in a nitrogen atmosphere, and their in vitro cytotoxicity was assessed according to ISO 10993-5 [1]. Extensive physical-chemical analyses have been carried out on the deposited structures with various thicknesses in order to explain the differences in biological behavior: profilometry, scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction and surface energy measurements. XPS revealed the presence of titanium oxynitride beside TiN in amounts that vary with the film thickness. The cytocompatibility of films seems to be influenced by their TiN surface content. The thinner films seem to be more suitable for medical applications, due to the combined high values of bonding strength and superior cytocompatibility. PMID:28787846

Combinatorial Characterization of TiO2 Chemical Vapor Deposition Utilizing Titanium Isopropoxide.

PubMed

Reinke, Michael; Ponomarev, Evgeniy; Kuzminykh, Yury; Hoffmann, Patrik

2015-07-13

The combinatorial characterization of the growth kinetics in chemical vapor deposition processes is challenging because precise information about the local precursor flow is usually difficult to access. In consequence, combinatorial chemical vapor deposition techniques are utilized more to study functional properties of thin films as a function of chemical composition, growth rate or crystallinity than to study the growth process itself. We present an experimental procedure which allows the combinatorial study of precursor surface kinetics during the film growth using high vacuum chemical vapor deposition. As consequence of the high vacuum environment, the precursor transport takes place in the molecular flow regime, which allows predicting and modifying precursor impinging rates on the substrate with comparatively little experimental effort. In this contribution, we study the surface kinetics of titanium dioxide formation using titanium tetraisopropoxide as precursor molecule over a large parameter range. We discuss precursor flux and temperature dependent morphology, crystallinity, growth rates, and precursor deposition efficiency. We conclude that the surface reaction of the adsorbed precursor molecules comprises a higher order reaction component with respect to precursor surface coverage.

Calcium Phosphate Growth at Electropolished Titanium Surfaces

PubMed Central

Ajami, Elnaz; Aguey-Zinsou, Kondo-Francois

2012-01-01

This work investigated the ability of electropolished Ti surface to induce Hydroxyapatite (HA) nucleation and growth in vitro via a biomimetic method in Simulated Body Fluid (SBF). The HA induction ability of Ti surface upon electropolishing was compared to that of Ti substrates modified with common chemical methods including alkali, acidic and hydrogen peroxide treatments. Our results revealed the excellent ability of electropolished Ti surfaces in inducing the formation of bone-like HA at the Ti/SBF interface. The chemical composition, crystallinity and thickness of the HA coating obtained on the electropolished Ti surface was found to be comparable to that achieved on the surface of alkali treated Ti substrate, one of the most effective and popular chemical treatments. The surface characteristics of electropolished Ti contributing to HA growth were discussed thoroughly. PMID:24955535

Influence of substrate metal alloy type on the properties of hydroxyapatite coatings deposited using a novel ambient temperature deposition technique.

PubMed

Barry, J N; Cowley, A; McNally, P J; Dowling, D P

2014-03-01

Hydroxyapatite (HA) coatings are applied widely to enhance the level of osteointegration onto orthopedic implants. Atmospheric plasma spray (APS) is typically used for the deposition of these coatings; however, HA crystalline changes regularly occur during this high-thermal process. This article reports on the evaluation of a novel low-temperature (<47°C) HA deposition technique, called CoBlast, for the application of crystalline HA coatings. To-date, reports on the CoBlast technique have been limited to titanium alloy substrates. This study addresses the suitability of the CoBlast technique for the deposition of HA coatings on a number of alternative metal alloys utilized in the fabrication of orthopedic devices. In addition to titanium grade 5, both cobalt chromium and stainless steel 316 were investigated. In this study, HA coatings were deposited using both the CoBlast and the plasma sprayed techniques, and the resultant HA coating and substrate properties were evaluated and compared. The CoBlast-deposited HA coatings were found to present similar surface morphologies, interfacial properties, and composition irrespective of the substrate alloy type. Coating thickness however displayed some variation with the substrate alloy, ranging from 2.0 to 3.0 μm. This perhaps is associated with the electronegativity of the metal alloys. The APS-treated samples exhibited evidence of both coating, and significantly, substrate phase alterations for two metal alloys; titanium grade 5 and cobalt chrome. Conversely, the CoBlast-processed samples exhibited no phase changes in the substrates after depositions. The APS alterations were attributed to the brief, but high-intensity temperatures experienced during processing. Copyright © 2013 Wiley Periodicals, Inc.

Surface Modifications with Laser Synthesized Mo Modified Coating

NASA Astrophysics Data System (ADS)

Sun, Lu; Chen, Hao; Liu, Bo

2013-01-01

Mg-Cu-Al was first used to improve the surface performance of TA15 titanium alloys by means of laser cladding technique. The synthesis of hard composite coating on TA15 titanium alloy by laser cladding of Mg-Cu-Al-B4C/Mo pre-placed powders was investigated by means of scanning electron microscope, energy dispersive spectrometer and high resolution transmission electron microscope. Experimental results indicated that such composite coating mainly consisted of TiB2, TiB, TiC, Ti3Al and AlCuMg. Compared with TA15 alloy substrate, an improvement of wear resistance was observed for this composite coating due to the actions of fine grain, amorphous and hard phase strengthening.

Laser bioengineering of glass-titanium implants surface

NASA Astrophysics Data System (ADS)

Lusquiños, F.; Arias-González, F.; Penide, J.; del Val, J.; Comesaña, R.; Quintero, F.; Riveiro, A.; Boutinguiza, M.; Pascual, M. J.; Durán, A.; Pou, J.

2013-11-01

Osseointegration is the mean challenge when surgical treatments fight against load-bearing bone diseases. Absolute bone replacement by a synthetic implant has to be completed not only from the mechanics point of view, but also from a biological approach. Suitable strength, resilience and stress distribution of titanium alloy implants are spoiled by the lack of optimal biological characteristics. The inert quality of extra low interstitial titanium alloy, which make it the most attractive metallic alloy for biomedical applications, oppose to an ideal surface with bone cell affinity, and capable to stimulate bone attachment bone growth. Diverse laser treatments have been proven as effective tools to modify surface properties, such as wettability in contact to physiological fluids, or osteoblast guided and slightly enhanced attachment. The laser surface cladding can go beyond by providing titanium alloy surfaces with osteoconduction and osteoinduction properties. In this research work, the laser radiation is used to produce bioactive glass coatings on Ti6Al4V alloy substrates. Specific silicate bioactive glass compositions has been investigated to achieve suitable surface tension and viscosity temperature behavior during processing, and to provide with the required release of bone growth gene up regulation agents in the course of resorption mediated by physiological fluids. The produced coatings and interfaces, the surface osteoconduction properties, and the chemical species release in simulated physiological fluid were characterized by scanning electron microscopy (SEM), hot stage microscopy (HSM), X-ray diffraction (XRD), X ray fluorescence (XRF), and Fourier transform infrared spectroscopy (FTIR).

Investigation of boundary conditions for biomimetic HA deposition on titanium oxide surfaces.

PubMed

Lindgren, M; Astrand, M; Wiklund, U; Engqvist, H

2009-07-01

To improve the clinical outcome of metal implants, i.e. earlier loading and reduction of the incidence of revision surgery, better bone bonding ability is wanted. One method to achieve this is to change the surface chemistry to give a surface that facilitates bone bonding in vivo, i.e. a bioactive surface. Crystalline titanium oxide has recently been proven to be bioactive in vitro and is an interesting option to the more common hydroxylapatite (HA) coatings on implants. A materials possible in vitro bioactivity is tested through soaking in simulated body fluid and studies of possible HA formation on the surface. For bioactive materials, the formed HA layer can also be used as a coating. The aim of the current paper is to investigate some boundary conditions for HA formation on crystalline titanium oxide surfaces regarding influence from coating thickness, soaking time and soaking temperature. The influence from soaking time and temperature on the HA growth were investigated on oxidised Ti samples, (24 h at 800 degrees C) resulting in a rutile surface structure. The oxidised samples were tested at three temperatures (4, 37 and 65 degrees C) and four times (1 h, 1 day, 1 week and 4 weeks). The influence from titanium coating thickness on the HA growth was investigated via depositing thin films of crystalline titanium dioxide on Ti plates using a reactive magnetron sputtering process. Four different PVD runs with coating thicknesses between 19 and 74 nm were tested. The soaking temperature had an effect on the HA formation and growth on both rutile surfaces and native oxide on Ti substrates. Higher temperatures lead to easier formation of HA. It was even possible, at 65 degrees C, to grow HA on native titanium oxide from soaking in PBS. The coating quality was better for HA formed at 65 degrees C compared to 37 degrees C. All PVD-coatings showed HA growth after 1 week in PBS at 37 degrees C, thus even very thin coatings of crystalline titanium oxide coatings are bioactive.

Hydroxyapatite synthesis on solid surfaces using a biological approach

NASA Astrophysics Data System (ADS)

Wang, A.; Mei, J.; Tse, Y. Y.; Jones, I. P.; Sammons, R. L.

2012-12-01

Many naturally occurring mineralisation processes yield hydroxyapatite (HA) or related salts, but biological routes to calcification have not generally been exploited for production of hydroxyapatite for clinical and industrial applications. Serratia sp. NCIMB 40259 is a non-pathogenic Gram-negative bacterium which is capable of growing as a biofilm on many surfaces and can be used to form HA coatings on a variety of polymeric and metallic materials, including titanium. Here we review previous work and report the results of more recent studies on the influence of titanium compositional and surface properties on Serratia adherence and proliferation and biomineralisation on commercially pure titanium (cp Ti) discs and a Ti mesh. Bacterial adherence was equivalent on cpTi and Ti6Al4V, and biofilms formed on both rough and mirror-polished cpTi surfaces. Embedded alumina particles and alkali treatment did not noticeably alter the precipitation of Serratia HA, nor the structure of the coating in comparison with non-treated substrates. Coatings were retained after sintering at 800°C in argon, although the original curved plate-like crystals changed to nano-scale β-tricalcium phosphate particles. A phosphorous-rich diffusion zone formed at the coating-titanium interface. Bacterial mineralisation may have applications as a method for producing coatings on implants in non load-bearing sites, and non-clinical applications where a high surface area is the major concern.

Mechanical and Functional Properties of Nickel Titanium Adhesively Bonded Joints

NASA Astrophysics Data System (ADS)

Niccoli, F.; Alfano, M.; Bruno, L.; Furgiuele, F.; Maletta, C.

2014-07-01

In this study, adhesive joints made up of commercial NiTi sheets with shape memory capabilities are analyzed. Suitable surface pre-treatments, i.e., degreasing, sandblasting, and chemical etching, are preliminary compared in terms of surface roughness, surface energy, and substrate thinning. Results indicate that chemical etching induces marked substrate thinning without substantial gains in terms of surface roughness and free energy. Therefore, adhesive joints with degreased and sandblasted substrates are prepared and tested under both static and cyclic conditions, and damage development within the adhesive layer is monitored in situ using a CCD camera. Sandblasted specimens have a significantly higher mechanical static strength with respect to degreased ones, although they essentially fail in similar fashion, i.e., formation of microcracks followed by decohesion along the adhesive/substrate interface. In addition, the joints show a good functional response with almost complete shape memory recovery after thermo-mechanical cycling, i.e., a small accumulation of residual deformations occurs. The present results show that adhesive bonding is a viable joining technique for NiTi alloys.

Novel Phenylethynyl Imide Silanes as Coupling Agents for Titanium Alloy

NASA Technical Reports Server (NTRS)

Park, C.; Lowther, S. E.; Smith, J. G., Jr.; Conell, J. W.; Hergenrother, P. M.; SaintClair, T. L.

2004-01-01

The durability of titanium (Ti) alloys bonded with high temperature adhesives such as polyimides has failed to attain the level of performance required for many applications. The problem to a large part is attributed to the instability of the surface treatment on the Ti substrate. Although Ti alloy adhesive specimens with surface treatments such as chromic acid anodization, Pasa-Jell, Turco, etc. have provided high initial mechanical properties, these properties have decreased as a function of aging at ambient temperature and faster, when aged at elevated temperatures or in a hot-wet environment. As part of the High Speed Civil Transport program where Ti honeycomb sandwich structure must perform for 60,000 hours at 177 C, work was directed to the development of environmentally safe, durable Ti alloy surface treatments.

Hydrothermal growth and characterization of titanium dioxide nanostructures for use in dye sensitized solar cells

NASA Astrophysics Data System (ADS)

Sorge, Judith D.

As the world's energy needs continue to grow, next generation photovoltaic cells are in high demand because they offer the possibility of an inexpensive alternative to current energy production techniques. Dye sensitized solar cells (DSSC's), utilize common materials and low cost commercialization techniques, which make them a compelling choice for research in this area. This research focuses on the titanium dioxide coating, which transfers electrons from the photoactive dye to the electrode. 3-4% efficient DSSC's using doctor bladed titanium dioxide coatings with a specific surface area of 55-60m2/g have been demonstrated in our laboratory. To enhance the efficiency of these cells, both the surface area and the electron conduction of the titania layer must be optimized. This has been done by utilizing high aspect ratio nanoparticles of titania instead of mesoporous layers formed with spherical particles. Anodization of titanium metal or anodic alumina membrane templating are common ways to produce nanorods, but involve complex processes leading toward expensive commercialization. This research instead focuses on the hydrothermal growth of nanofibrous titania on a titanium metal substrate, removing the need for dispersion and deposition procedures as well as using a low temperature processing method. Depending upon the formulation utilized, a variety of structures can be produced, from thick carpets of nanofiber strands to large platelets. The composition and morphology of the products have been characterized with respect to the growth conditions using electron microscopy, energy dispersive spectroscopy and x-ray diffraction. The compositional analysis is used to investigate the complicated reaction mechanisms in the system. Coatings of titania nanotubes were then tested in the DSSC's, as were those with the titanium metal substrate acting as the photo anode. Modeling the geometric parameters of the different pore structures of the coatings helps us to understand the advantages afforded by these new cells.

Wetting of single crystal mullite by borosilicate and yttrium-aluminosilicate glasses and wetting phenomena of steels containing aluminum and titanium

NASA Astrophysics Data System (ADS)

Eldred, Benjamin Todd

This dissertation consists of two major sections. The first section concerns the wetting of single crystal mullite by borosilicate and yttrium-aluminosilicate glasses. The borosilicate glass showed poor wetting and interacted only moderately with the substrate. The yttrium-aluminosilicate glass interacted strongly with mullite and showed very good wetting. Balanced chemical equations between each glass and mullite were derived from EDS data. Wetting was found to be dependent on the crystallographic orientation of the substrate, in agreement with previous studies of the surface energy of mullite. The second section concerns the wetting phenomena of steels containing aluminum and titanium. A modified sessile drop technique was used to investigate the wetting of steels containing aluminum and/or titanium as a function of furnace atmosphere. It was found that the steel chemistry and furnace atmosphere had little effect on wetting except in the case of a particular ultra-low carbon steel containing both aluminum and titanium. This steel was found to show significantly lower contact angles than any other steel tested when it was in an atmosphere of pure hydrogen. As nitrogen was added to the atmosphere, the contact angle increased monotonically and irreversibly. The interaction between aluminum, titanium, and nitrogen is explained in terms of first-order interaction coefficients available in thermodynamic literature.

Oxygen diffusion barrier coating

NASA Technical Reports Server (NTRS)

Unnam, Jalaiah (Inventor); Clark, Ronald K. (Inventor)

1987-01-01

A method for coating a titanium panel or foil with aluminum and amorphous silicon to provide an oxygen barrier abrogating oxidation of the substrate metal is developed. The process is accomplished with known inexpensive procedures common in materials research laboratories, i.e., electron beam deposition and sputtering. The procedures are conductive to treating foil gage titanium and result in submicron layers which virtually add no weight to the titanium. There are no costly heating steps. The coatings blend with the substrate titanium until separate mechanical properties are subsumed by those of the substrate without cracking or spallation. This method appreciably increases the ability of titanium to mechanically perform in high thermal environments such as those witnessed on structures of space vehicles during re-entry

Preparation of Copper and Chromium Alloyed Layers on Pure Titanium by Plasma Surface Alloying Technology

NASA Astrophysics Data System (ADS)

He, Xiaojing; Li, Meng; Wang, Huizhen; Zhang, Xiangyu; Tang, Bin

2015-05-01

Cu-Cr alloyed layers with different Cu and Cr contents on pure titanium were obtained by means of plasma surface alloying technology. The microstructure, chemical composition and phase composition of Cu-Cr alloyed layers were analyzed by scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and X-ray diffraction (XRD), respectively. The experimental results demonstrate that the alloyed layers are bonded strongly to pure titanium substrate and consist of unbound Ti, CuTi, Cu3Ti, CuTi3 and Cr2Ti. The thickness of Cu5Cr5 and Cu7Cr3 alloyed layer are about 18 μm and 28 μm, respectively. The antibacterial properties against gram-negative Escherichia coli (E.coli, ATCC10536) and gram-positive Staphylococcus aureus (S. aureus, ATCC6538) of untreated pure titanium and Cu-Cr alloyed specimen were investigated by live/dead fluorescence staining method. The study shows that Cu-Cr alloyed layers exhibit excellent antibacterial activities against both E.coli and S.aureus within 24 h, which may be attributed to the formation of Cu-containing phases.

Novel Approach in the Use of Plasma Spray: Preparation of Bulk Titanium for Bone Augmentations

PubMed Central

Fousova, Michaela; Vojtech, Dalibor; Jablonska, Eva; Fojt, Jaroslav; Lipov, Jan

2017-01-01

Thermal plasma spray is a common, well-established technology used in various application fields. Nevertheless, in our work, this technology was employed in a completely new way; for the preparation of bulk titanium. The aim was to produce titanium with properties similar to human bone to be used for bone augmentations. Titanium rods sprayed on a thin substrate wire exerted a porosity of about 15%, which yielded a significant decrease of Young′s modulus to the bone range and provided rugged topography for enhanced biological fixation. For the first verification of the suitability of the selected approach, tests of the mechanical properties in terms of compression, bending, and impact were carried out, the surface was characterized, and its compatibility with bone cells was studied. While preserving a high enough compressive strength of 628 MPa, the elastic modulus reached 11.6 GPa, thus preventing a stress-shielding effect, a generally known problem of implantable metals. U-2 OS and Saos-2 cells derived from bone osteosarcoma grown on the plasma-sprayed surface showed good viability. PMID:28837101

Understanding the effects of process parameters on the properties of cold gas dynamic sprayed pure titanium coatings

NASA Astrophysics Data System (ADS)

Wong, Wilson

The cold gas dynamic spraying of commercially pure titanium coatings was investigated. Specifically, the relationship between several key cold spray parameters on the quality of the resulting coatings was studied in order to gain a more thorough understanding of the cold spray process. To achieve this goal, three distinct investigations were performed. The first part of the investigation focussed on the effect of propelling gas, particularly helium and nitrogen, during the cold spraying of titanium coatings. Coatings were characterised by SEM and were evaluated for their deposition efficiency (DE), microhardness, and porosity. In selected conditions, three particle velocities were investigated such that for each condition, the propelling gasses temperature and pressure were attuned to attain similar particle velocities for each gas. In addition, a thick and fully dense cold sprayed titanium coating was achieved with optimised spray parameters and nozzle using helium. The corresponding average particle velocity was 1173 m/s. The second part of the investigation studied the effect of particle morphology (spherical, sponge, and irregular) and size distributions (mean particle sizes of 20, 29, and 36 mum) of commercially pure titanium on the mechanical properties of the resulting cold sprayed coatings. Numerous powder and coating characterisations were performed. From these data, semi-empirical flow (stress-strain) curves were generated based on the Johnson-Cook plasticity model which could be used as a measure of cold sprayability. Cold sprayability can be defined as the ease with which a powder can be cold sprayed. It was found that the sponge and irregular commercially pure titanium powders had higher oxygen content, poorer powder flowability, higher compression ratio, lower powder packing factor, and higher average particle impact velocities compared to the spherical powders. XRD results showed no new phases present when comparing the various feedstock powders to their corresponding coatings. For all feedstock powder morphologies, it was observed that the larger the particle size, the higher the temperature generated on impact. For the spherical powders, the higher the temperature generated on impact, the lower the stress needed to deform the particle. In addition, as the kinetic energy of the impacting particle increased, the flow peak stress decreased while the final strain increased. Furthermore, higher final flow strains were associated with higher coating DeltaHV 10 (between the coatings and the feedstock powders). Similar relationships are expected to exist for the sponge and irregular feedstock powders. Based on porosity, the spherical medium powder was found to have the best cold sprayability. The final part of the investigation focussed on the effect of substrate surface roughness and coating thickness on the adhesion strength of commercially pure titanium cold sprayed coatings onto Steel 1020, Al 6061, and Ti substrates. Adhesion strength was measured by tensile/pull tests according to ASTM C-633-01 standard. Through-thickness residual stresses of selected coatings were measured using the modified layer removal method (MLRM). In addition, mean coating residual stresses were calculated from MLRM results. It was found that adhesion strength increases with increasing substrate surface roughness and decreases with increasing coating thickness. Furthermore, mean coating residual stresses were correlated with adhesion strength and it was suggested that higher adhesion strengths are associated with higher mean compressive stresses and a higher probability for adiabatic shear instability to occur due to the higher particle impact velocities. In general, it was found that under similar cold spray conditions and substrate surface preparation method, adhesion strength was strongest for commercially pure titanium coatings deposited onto Al 6061, followed by Ti, then Steel 1020.

Inorganic-organic hybrid coatings on stainless steel by layer-by-layer deposition and surface-initiated atom-transfer-radical polymerization for combating biocorrosion.

PubMed

Yuan, S J; Pehkonen, S O; Ting, Y P; Neoh, K G; Kang, E T

2009-03-01

To improve the biocorrosion resistance of stainless steel (SS) and to confer the bactericidal function on its surface for inhibiting bacterial adhesion and biofilm formation, well-defined inorganic-organic hybrid coatings, consisting of the inner compact titanium oxide multilayers and outer dense poly(vinyl-N-hexylpyridinium) brushes, were successfully developed. Nanostructured titanium oxide multilayer coatings were first built up on the SS substrates via the layer-by-layer sol-gel deposition process. The trichlorosilane coupling agent, containing the alkyl halide atom-transfer-radical polymerization (ATRP) initiator, was subsequently immobilized on the titanium oxide coatings for surface-initiated ATRP of 4-vinylpyridine (4VP). The pyridium nitrogen moieties of the covalently immobilized 4VP polymer, or P(4VP), brushes were quaternized with hexyl bromide to produce a high concentration of quaternary ammonium salt on the SS surfaces. The excellent antibacterial efficiency of the grafted polycations, poly(vinyl-N-pyridinium bromide), was revealed by viable cell counts and atomic force microscopy images of the surface. The effectiveness of the hybrid coatings in corrosion protection was verified by the Tafel plot and electrochemical impedance spectroscopy measurements.

Selective growth of titanium dioxide by low-temperature chemical vapor deposition.

PubMed

Reinke, Michael; Kuzminykh, Yury; Hoffmann, Patrik

2015-05-13

A key factor in engineering integrated optical devices such as electro-optic switches or waveguides is the patterning of thin films into specific geometries. In particular for functional oxides, etching processes are usually developed to a much lower extent than for silicon or silicon dioxide; therefore, selective area deposition techniques are of high interest for these materials. We report the selective area deposition of titanium dioxide using titanium isopropoxide and water in a high-vacuum chemical vapor deposition (HV-CVD) process at a substrate temperature of 225 °C. Here—contrary to conventional thermal CVD processes—only hydrolysis of the precursor on the surface drives the film growth as the thermal energy is not sufficient to thermally decompose the precursor. Local modification of the substrate surface energy by perfluoroalkylsilanization leads to a reduced surface residence time of the precursors and, consequently, to lower reaction rate and a prolonged incubation period before nucleation occurs, hence, enabling selective area growth. We discuss the dependence of the incubation time and the selectivity of the deposition process on the presence of the perfluoroalkylsilanization layer and on the precursor impinging rates—with selectivity, we refer to the difference of desired material deposition, before nucleation occurs in the undesired regions. The highest measured selectivity reached (99 ± 5) nm, a factor of 3 superior than previously reported in an atomic layer deposition process using the same chemistry. Furthermore, resolution of the obtained patterns will be discussed and illustrated.

TiO2 -enriched polymeric powder coatings support human mesenchymal cell spreading and osteogenic differentiation.

PubMed

Mozumder, Mohammad Sayem; Zhu, Jesse; Perinpanayagam, Hiran

2011-06-01

Novel polymeric powder coatings (PPC) were prepared by ultrafine powder coating technology and shown to support human mesenchymal cell attachment and growth. PPC surfaces enriched with nano-TiO(2) (nTiO(2)) showed enhanced cellular responses, and were compared to commercially pure titanium (cpTi). After cell attachment and growth, osteogenic differentiation and bone matrix formation ensures osseointegration for implantable biomaterials. Therefore, the objective of this study was to determine if mesenchymal cells grown on PPC could undergo osteogenic differentiation by inducing Runx2 and bone matrix proteins, and then initiate mineralization. Atomic force microscopy revealed intricate three-dimensional micro-topographies, and the measures of nano-roughness and porosity were similar for all PPC surfaces. Scanning electron microscopy showed that the cells attached and spread out over all of the surfaces. After 1 week in osteogenic media, RT-PCR analysis showed the induction of Runx2, the up-regulation of type I collagen, and the initial detection of alkaline phosphatase and bone sialoprotein. After 4 weeks, Alizarin Red staining showed mineral deposition. However, cell spreading and osteogenic differentiation were significantly (P < 0.05) higher on the cpTi controls than on the PPC surfaces. Furthermore, spreading and differentiation were consistently higher on the titanium-enriched PPC-2, -3 and -4 than on the titanium-free PPC-1. Therefore, despite the presence of complex micro-topographies and nano-features, titanium-enrichment enhanced the cellular response, and pure titanium still provided the best substrate. These findings confirm the cytocompatibility of these novel polymeric coatings and suggest that titanium-enrichment and nTiO(2) additives may enhance their performance.

The process development of laser surface modification of commercially pure titanium (Grade 2) with rhenium

NASA Astrophysics Data System (ADS)

Kobiela, K.; Smolina, I.; Dziedzic, R.; Szymczyk, P.; Kurzynowski, T.; Chlebus, E.

2016-12-01

The paper presents the results of the process development of laser surface modification of commercially pure titanium with rhenium. The criterion of the successful/optimal process is the repetitive geometry of the surface, characterized by predictable and repetitive chemical composition over its entire surface as well as special mechanical properties (hardness and wear resistance). The analysis of surface geometry concluded measurements of laser penetration depth and heat affected zone (HAZ), the width of a single track as well as width of a clad. The diode laser installed on the industrial robot carried out the laser treatment. This solution made possible the continuous supply of powder to the substrate during the process. The aim of an investigation is find out the possibility of improving the tribological characteristics of the surface due to the rhenium alloying. The verification of the surface properties (tribological) concluded geometry measurements, microstructure observation, hardness tests and evaluation of wear resistance.

LARC-13 adhesive development

NASA Technical Reports Server (NTRS)

Hill, S. G.; Sheppard, C. H.; Johnson, J. C.

1980-01-01

A LARC-13 type adhesive system was developed and property data obtained that demonstrated improved thermomechanical properties superior to base LARC-13 adhesive. An improved adhesive for 589 K (600 F) use was developed by physical or chemical modification of LARC-13. The adhesive was optimized for titanium and composite bonding, and a compatible surface preparation for titanium and composite substrates was identified. The data obtained with the improved adhesive system indicated it would meet the 589 K (600 F) properties desired for application on space shuttle components. Average titanium lap shear data were: (1) 21.1 MPa (3355 psi) at RT, (2) 13.0 MPa (1881 psi) at 600 F, and (3) 16.4 MPa (2335) after aging 125 hours at 600 F and tested at 600 F.

Microstructure and high temperature oxidation resistance of Ti-Ni gradient coating on TA2 titanium alloy fabricated by laser cladding

NASA Astrophysics Data System (ADS)

Liu, Fencheng; Mao, Yuqing; Lin, Xin; Zhou, Baosheng; Qian, Tao

2016-09-01

To improve the high temperature oxidation resistance of TA2 titanium alloy, a gradient Ni-Ti coating was laser cladded on the surface of the TA2 titanium alloy substrate, and the microstructure and oxidation behavior of the laser cladded coating were investigated experimentally. The gradient coating with a thickness of about 420-490 μm contains two different layers, e.g. a bright layer with coarse equiaxed grain and a dark layer with fine and columnar dendrites, and a transition layer with a thickness of about 10 μm exists between the substrate and the cladded coating. NiTi, NiTi2 and Ni3Ti intermetallic compounds are the main constructive phases of the laser cladded coating. The appearance of these phases enhances the microhardness, and the dense structure of the coating improves its oxidation resistance. The solidification procedure of the gradient coating is analyzed and different kinds of solidification processes occur due to the heat dissipation during the laser cladding process.

Reduced bacteria adhesion on octenidine loaded mesoporous silica nanoparticles coating on titanium substrates.

PubMed

Xu, Gaoqiang; Shen, Xinkun; Dai, Liangliang; Ran, Qichun; Ma, Pingping; Cai, Kaiyong

2017-01-01

Bacterial infection is one of the most severe postoperative complications leading to implantation failure. The early bacterial stage (4-6h) was proved to be the "decisive period" for long-term bacteria-related infection. Thus, to endow potential early antibacterial capacity for a titanium (Ti) based implant, an effective antiseptic agent of octenidine dihydrochloride (OCT) was effectively loaded on the mesoporous silica nanoparticles (MSNs)-incorporated titania coating which was fabricated by an electrophoretic-enhanced micro-arc oxidation technique. The surface characteristic of the coatings were characterized by various methods (SEM, AFM, XPS, XRD, etc.), and its corrosion resistance was also examined by the potentiodynamic polarization curves. The composite coating without OCT loading not only displayed good cytocompatibility but also exhibited certain anti-bacterial property. After loading with OCT, its antibacterial efficiency of the titanium substrates with composite coating was greatly enhanced without compromising their cytocompatibility. The study provides an approach for the fabrication of anti-bacterial Ti implant for potential orthopedic application. Copyright © 2016 Elsevier B.V. All rights reserved.

Epitaxial titanium diboride films grown by pulsed-laser deposition

NASA Astrophysics Data System (ADS)

Zhai, H. Y.; Christen, H. M.; Cantoni, C.; Goyal, A.; Lowndes, D. H.

2002-03-01

Epitaxial, smooth, and low-resistivity titanium diboride (TiB2) films have been grown on SiC substrates using pulsed-laser deposition. Combined studies from ex situ x-ray diffraction and in situ reflection high-energy electron diffraction indicate the crystallographic alignment between TiB2 and SiC both parallel and normal to the substrate. Atomic force microscopy and scanning electron microscopy studies show that these epitaxial films have a smooth surface, and the resistivity of these films is comparable to that of single-crystal TiB2. Growth of these films is motivated by this material's structural and chemical similarity and lattice match to the newly discovered superconductor MgB2, both to gain further insight into the physical mechanisms of diborides in general and, more specifically, as a component of MgB2-based thin-film heterostructures.

X-ray photoelectron spectroscopy characterization of composite TiO 2-poly(vinylidenefluoride) films synthesised for applications in pesticide photocatalytic degradation

NASA Astrophysics Data System (ADS)

Losito, I.; Amorisco, A.; Palmisano, F.; Zambonin, P. G.

2005-02-01

X-ray photoelectron spectroscopy (XPS) was adopted for the analytical characterization of composite titanium dioxide-poly(vinylidenefluoride) (TiO 2-PVDF) films developed for applications in the photocatalytic degradation of pollutants. The composites were deposited on glass substrates by casting or spin coating from TiO 2-PVDF suspensions in dimethylformamide (DMF). XPS data on the TiO 2-PVDF surface composition were used to optimize preparation conditions (composition of the TiO 2/PVDF suspension, deposition technique) in terms of titanium dioxide surface amount and film stability. The use of spin-coating deposition and the increase of TiO 2 amount in the DMF suspensions were found to improve the titanium surface content, although high TiO 2/PVDF ratios led to film instability. PVDF-TiO 2 films were also used in preliminary photocatalytic degradation tests on isoproturon, a phenylurea herbicide, under solar UV irradiation; the results were compared to direct photolysis to evaluate the catalytic efficiency of immobilized TiO 2 and the role played by the PVDF film during the degradation process.

Nano- and Micro-Scale Oxidative Patterning of Titanium Implant Surfaces for Improved Surface Wettability.

PubMed

Kim, In-hye; Son, Jun Sik; Choi, Seok Hwa; Kim, Kyo-han; Kwon, Tae-yub

2016-02-01

A simple and scalable surface modification treatment is demonstrated, in which nano- and microscale features are introduced into the surface of titanium (Ti) substrates by means of a novel and eco-friendly oxidative aqueous solution composed of hydrogen peroxide (H202) and sodium bicarbonate (NaHCO3). By immersing mirror-polished Ti discs in an aqueous mixture of 30 wt% H2O2/5 wt% NaHCO3 at 23 +/- 3 degrees C for 4 h, it was confirmed that this mixture is capable of generating microscale topographies on Ti surfaces. It also simultaneously formed nanochannels that were regularly arranged in a comb-like pattern on the Ti surface, thus forming a hierarchical surface structure. Further, these nano/micro-textured Ti surfaces showed great surface roughness and excellent wettability when compared with control Ti surfaces. This study demonstrates that a H2O2/NaHCO3 mixture can be effectively utilized to create reproducible nano/microscale topographies on Ti implant surfaces, thus providing an economical new oxidative solution that may be used effectively and safely as a Ti surface modification treatment.

Surface Participation Effects in Titanium Nitride and Niobium Resonators

NASA Astrophysics Data System (ADS)

Dove, Allison; Kreikebaum, John Mark; Livingston, William; Delva, Remy; Qiu, Yanjie; Lolowang, Reinhard; Ramasesh, Vinay; O'Brien, Kevin; Siddiqi, Irfan

Improving the coherence time of superconducting qubits requires a precise understanding of the location and density of surface defects. Superconducting microwave resonators are commonly used for quantum state readout and are a versatile testbed to systematically characterize materials properties as a function of device geometry and fabrication method. We report on sputter deposited titanium nitride and niobium on silicon coplanar waveguide resonators patterned using reactive ion etches to define the device geometry. We discuss the impact of different growth conditions (temperature and electrical bias) and processing techniques on the internal quality factor (Q) of these devices. In particular, to investigate the effect of surface participation, we use a Bosch process to etch many-micron-deep trenches in the silicon substrate and quantify the impact of etch depth and profile on the internal Q. This research was supported by the ARO.

Structural and surface property characterization of titanium dioxide nanotubes for orthopedic implants

NASA Astrophysics Data System (ADS)

Shokuhfar, Tolou

This research focused on the to modification of the surface structure of titanium implants with nanostructured morphology of TiO2 nanotubes and studied the interaction of nanotubes with osteoblast cells to understand the parameters that affect the cell growth. The electrical, mechanical, and structural properties of TiO2 nanotubes were characterized to establish a better understanding on the properties of such nanoscale morphological structures. To achieve the objectives of this research work I transformed the titanium and its alloys, either in bulk sheet form, bulk machined form, or thin film deposited on another substrate into a surface of titania nanotubes using a low cost and environmentally friendly process. The process requires only a simple electrolyte, low cost electrode, and a DC power supply. With this simple approach of scalable nanofabrication, a typical result is nanotubes that are each approximately 100nm in diameter and have a wall thickness of about 20nm. By changing the fabrication parameters, independent nanotubes can be fabricated with open volume between them. Titanium in this form is termed onedimensional since electron transport is narrowly confined along the length of the nanotube. My Ph.D. accomplishments have successfully shown that osteoblast cells, the cells that are the precursors to bone, have a strong tendency to attach to the inside and outside of the titanium nanotubes onto which they are grown using their filopodia -- cell's foot used for locomotion -- anchored to titanium nanotubes. In fact it was shown that the cell prefers to find many anchoring sites. These sites are critical for cell locomotion during the first several weeks of maturity and upon calcification as a strongly anchored bone cell. In addition I have shown that such a surface has a greater cell density than a smooth titanium surface. My work also developed a process that uses a focused and controllably rastered ion beam as a nano-scalpel to cut away sections of the osteoblast cells to probe the attachment beneath the main cell body. Ultimately the more rapid growth of osteoblasts, coupled with a stronger cell-surface interface, could provide cost reduction, shorter rehabilitation, and fewer follow-on surgeries due to implant loosening.

Modified surface of titanium dioxide nanoparticles-based biosensor for DNA detection

NASA Astrophysics Data System (ADS)

Nadzirah, Sh.; Hashim, U.; Rusop, M.

2018-05-01

A new technique was used to develop a simple and selective picoammeter DNA biosensor for identification of E. coli O157:H7. This biosensor was fabricated from titanium dioxide nanoparticles that was synthesized by sol-gel method and spin-coated on silicon dioxide substrate via spinner. 3-Aminopropyl triethoxy silane (APTES) was used to modify the surface of TiO2. Simple surface modification approach has been applied; which is single dropping of APTES onto the TiO2 nanoparticles surface. Carboxyl modified probe DNA has been bind onto the surface of APTES/TiO2 without any amplifier element. Electrical signal has been used as the indicator to differentiate each step (surface modification of TiO2 and probe DNA immobilization). The I-V measurements indicate extremely low current (pico-ampere) flow through the device which is 2.8138E-10 A for pure TiO2 nanoparticles, 2.8124E-10 A after APTES modification and 3.5949E-10 A after probe DNA immobilization.

Formation mechanism and adhesive strength of a hydroxyapatite/TiO2 composite coating on a titanium surface prepared by micro-arc oxidation

NASA Astrophysics Data System (ADS)

Liu, Shimin; Li, Baoe; Liang, Chunyong; Wang, Hongshui; Qiao, Zhixia

2016-01-01

A hydroxyapatite (HA)/TiO2 composite coating was prepared on a titanium surface by one-step micro-arc oxidation (MAO). The formation mechanism of the composite coating was investigated and the adhesion of the coating to the substrate was also measured. The results showed that flocculent structures could be obtained during the early stages of treatment. As the treatment period extended, increasing amounts of Ca-P precipitate appeared on the surface, and the flocculent morphology transformed into a plate-like morphology. Then the plate-like calcium and phosphate salt self-assembled to form flower-like apatite. The Ca/P atomic ratio gradually decreased, indicating that the amounts of Ca2+ ions which diffused into the coating decreased more rapidly than that of PO43- or HPO42-. The adhesive strength between the apatite and TiO2 coating was improved. This improvement is attributed to the interlocking effect between the apatite and TiO2 layer which formed simultaneously during the early stages of the one-step MAO. This study shows that it is a promising method to prepare bioactive coating on a titanium surface.

Effect of Atmospheric Plasma Treatment to Titanium Surface on Initial Osteoblast-Like Cell Spreading. .

PubMed

Kim, In-Hye; Son, Jun-Sik; Kwon, Tae-Yub; Kim, Kyo-Han

2015-01-01

Plasma treatments are becoming a popular method for modifying the characteristics of a range of substrate surfaces. Atmospheric pressure plasma is cost-efficient, safe and simple compared to high-pressure plasma. This study examined the effects of atmospheric pressure plasma to a titanium (Ti) surface on osteoblast-like cell (osteoblast) spreading and cellular networks. The characteristics of the Ti surface before and after the atmospheric plasma treatment were analyzed by X-ray photoemission spectroscopy (XPS), scanning electron microscopy (SEM), contact angle measurements, and an optical 3D profiling system. The morphology of osteoblasts attached to the Ti surfaces was observed by SEM and confocal laser scanning microscopy. The atmospheric pressure plasma made the Ti surfaces more hydrophilic. The osteoblasts that adhered to the untreated surface were round and spherical, whereas the cells covered a larger surface area on the plasma-treated surface. The plasma-treated Ti surface showed enhanced cell spreading and migration with more developed cellular networks. In conclusion, an atmospheric plasma treatment is a potential surface modifying method that can enhance the initial the cell affinity at the early stages in vitro.

The Growth Behavior of Titanium Boride Layers in α and β Phase Fields of Titanium

NASA Astrophysics Data System (ADS)

Lv, Xiaojun; Hu, Lingyun; Shuang, Yajing; Liu, Jianhua; Lai, Yanqing; Jiang, Liangxing; Li, Jie

2016-07-01

In this study, the commercially pure titanium was successfully electrochemical borided in a borax-based electrolyte. The process was carried out at a constant cathodic current density of 300 mA cm-2 and at temperatures of 1123 K and 1223 K (850 °C and 950 °C) for 0.5, 1, 2, 3, and 5 hours. The growth behavior of titanium boride layers in the α phase field of titanium was compared with that in the β phase field. After boriding, the presence of both the TiB2 top layer and TiB whisker sub-layer was confirmed by the X-ray diffraction (XRD) and scanning electron microscope. The relationship between the thickness of boride layers and boriding time was found to have a parabolic character in both α and β phase fields of titanium. The TiB whiskers showed ultra-fast growth rate in the β phase field. Its growth rate constant was found to be as high as 3.2002 × 10-13 m2 s-1. Besides, the chemical resistance of the TiB2 layer on the surface of titanium substrate was characterized by immersion tests in molten aluminum.

Microstructure and properties of TiB2-TiB reinforced titanium matrix composite coating by laser cladding

NASA Astrophysics Data System (ADS)

Lin, Yinghua; Yao, Jianhua; Lei, Yongping; Fu, Hanguang; Wang, Liang

2016-11-01

TiB2 particle and TiB short fiber reinforced titanium matrix composite coatings were prepared utilizing in situ synthesized technique by laser cladding on the surface of Ti6Al4V alloy. Through the experiment, it was found that the surface of the single-track coatings appeared in the depression, but it can be improved by laser track overlapping. With the increase of laser power density, the amount of TiB short fiber was increased, and the distribution of TiB2 and TiB became more uniform from the top to bottom. The micro-hardness of TiB2/TiB coating showed a gradient decreasing trend, and the average micro-hardness of the coatings was two-fold higher than that of the substrate. Due to the strengthening effect of TiB2 particle and TiB short fiber, the wear volume loss of the center of the coating was approximately 30% less than that of the Ti-6Al-4V substrate, and the wear mechanism of the coating was mild fatigue particle detachment.

Superconducting composite with multilayer patterns and multiple buffer layers

DOEpatents

Wu, X.D.; Muenchausen, R.E.

1993-10-12

An article of manufacture is described including a substrate, a patterned interlayer of a material selected from the group consisting of magnesium oxide, barium-titanium oxide or barium-zirconium oxide, the patterned interlayer material overcoated with a secondary interlayer material of yttria-stabilized zirconia or magnesium-aluminum oxide, upon the surface of the substrate whereby an intermediate article with an exposed surface of both the overcoated patterned interlayer and the substrate is formed, a coating of a buffer layer selected from the group consisting of cerium oxide, yttrium oxide, curium oxide, dysprosium oxide, erbium oxide, europium oxide, iron oxide, gadolinium oxide, holmium oxide, indium oxide, lanthanum oxide, manganese oxide, lutetium oxide, neodymium oxide, praseodymium oxide, plutonium oxide, samarium oxide, terbium oxide, thallium oxide, thulium oxide, yttrium oxide and ytterbium oxide over the entire exposed surface of the intermediate article, and, a ceramic superconductor. 5 figures.

Back-surface gold mirrors for vibrationally resonant sum-frequency (VR-SFG) spectroscopy using 3-mercaptopropyltrimethoxysilane as an adhesion promoter.

PubMed

Quast, Arthur D; Zhang, Feng; Linford, Matthew R; Patterson, James E

2011-06-01

Back-surface mirrors are needed as reference materials for vibrationally resonant sum-frequency generation (VR-SFG) probing of liquid-solid interfaces. Conventional noble metal mirrors are not suitable for back-surface applications due to the presence of a metal adhesion layer (chromium or titanium) between the window substrate and the reflective metal surface. Using vapor deposited 3-mercaptopropyltrimethoxysilane (MPTMS) as a bi-functional adhesion promoter, gold mirrors were fabricated on fused silica substrates. These mirrors exhibit excellent gold adhesion as determined by the Scotch(®) tape test. They also produce minimal spectroscopic interference in the C-H stretching region (2800-3000 cm(-1)), as characterized by VR-SFG. These mirrors are thus robust and can be used as back-surface mirrors for a variety of applications, including reference mirrors for VR-SFG.

Effects of bias voltage on diamond like carbon coatings deposited using titanium isopropoxide (TIPOT) and acetylene/argon mixtures onto various substrate materials.

PubMed

Said, R; Ghumman, C A A; Teodoro, M N D; Ahmed, W; Abuazza, A; Gracio, J

2010-04-01

RF-PECVD was used to prepare amorphous of carbon (DLC) onto stainless steel 316 and glass substrates. The substrates were negatively biased at between 100 V to 400 V. Thin films of DLC have been deposited using C2H2 and titanium isopropoxide (TIPOT). Argon was used to generate the plasma in the PECVD system chamber. DEKTAK 8 surface stylus profilometer was used to measure the film thickness and the deposition rate was calculated. Micro Raman spectroscopy was employed to determine the chemical structure and bonding present in the films. Composition analysis of the samples was carried out using VGTOF SIMS (IX23LS) instrument. In addition, X-ray photoelectron spectroscopy (XPS) was used to analyze the composition and chemical state of the films. The wettability of the films was examined using the optical contact angle meter (CAM200) system. Two types of liquids with different polarities were used to study changes in the surface energy. The as-grown films were in the thickness range of 200-400 nm. Raman spectroscopy results showed that the I(D)/I(G) ratio decreased when the bias voltage on the stainless steel substrates was increased. This indicates an increase in the graphitic nature of the film deposited. In contrast, on the glass substrates the I(D)/I(G) ratio increased when the bias voltage was increased indicates a greater degree of diamond like character. Chemical composition determined using XPS showed the presence of carbon and oxygen in both samples on glass and stainless steel substrates. Both coatings the contact angle of the films decreased except for 400 V which showed a slight increase. The oxygen is thought to play an important role on the polar component of a-C.

Surface analysis and biocorrosion properties of nanostructured surface sol-gel coatings on Ti6Al4V titanium alloy implants.

PubMed

Advincula, Maria C; Petersen, Don; Rahemtulla, Firoz; Advincula, Rigoberto; Lemons, Jack E

2007-01-01

Surfaces of biocompatible alloys used as implants play a significant role in their osseointegration. Surface sol-gel processing (SSP), a variant of the bulk sol-gel technique, is a relatively new process to prepare bioreactive nanostructured titanium oxide for thin film coatings. The surface topography, roughness, and composition of sol-gel processed Ti6Al4V titanium alloy coatings was investigated by atomic force microscopy (AFM) and X-ray electron spectroscopy (XPS). This was correlated with corrosion properties, adhesive strength, and bioreactivity in simulated body fluids (SBF). Electroimpedance spectroscopy (EIS) and polarization studies indicated similar advantageous corrosion properties between sol-gel coated and uncoated Ti6Al4V, which was attributed to the stable TiO2 composition, topography, and adhesive strength of the sol-gel coating. In addition, inductive coupled plasma (ICP) and scanning electron microscopy with energy dispersive spectrometry (SEM-EDS) analysis of substrates immersed in SBF revealed higher deposition of calcium and phosphate and low release rates of alloying elements from the sol-gel modified alloys. The equivalent corrosion behavior and the definite increase in nucleation of calcium apatite indicate the potential of the sol-gel coating for enhanced bioimplant applications. 2006 Wiley Periodicals, Inc.

Osteoblast responses to different oxide coatings produced by the sol-gel process on titanium substrates.

PubMed

Ochsenbein, Anne; Chai, Feng; Winter, Stefan; Traisnel, Michel; Breme, Jürgen; Hildebrand, Hartmut F

2008-09-01

In order to improve the osseointegration of endosseous implants made from titanium, the structure and composition of the surface were modified. Mirror-polished commercially pure (cp) titanium substrates were coated by the sol-gel process with different oxides: TiO(2), SiO(2), Nb(2)O(5) and SiO(2)-TiO(2). The coatings were physically and biologically characterized. Infrared spectroscopy confirmed the absence of organic residues. Ellipsometry determined the thickness of layers to be approximately 100nm. High resolution scanning electron microscopy (SEM) and atomice force microscopy revealed a nanoporous structure in the TiO(2) and Nb(2)O(5) layers, whereas the SiO(2) and SiO(2)-TiO(2) layers appeared almost smooth. The R(a) values, as determined by white-light interferometry, ranged from 20 to 50nm. The surface energy determined by the sessile-drop contact angle method revealed the highest polar component for SiO(2) (30.7mJm(-2)) and the lowest for cp-Ti and 316L stainless steel (6.7mJm(-2)). Cytocompatibility of the oxide layers was investigated with MC3T3-E1 osteoblasts in vitro (proliferation, vitality, morphology and cytochemical/immunolabelling of actin and vinculin). Higher cell proliferation rates were found in SiO(2)-TiO(2) and TiO(2), and lower in Nb(2)O(5) and SiO(2); whereas the vitality rates increased for cp-Ti and Nb(2)O(5). Cytochemical assays showed that all substrates induced a normal cytoskeleton and well-developed focal adhesion contacts. SEM revealed good cell attachment for all coating layers. In conclusion, the sol-gel-derived oxide layers were thin, pure and nanostructured; consequent different osteoblast responses to those coatings are explained by the mutual action and coadjustment of different interrelated surface parameters.

Sol-gel synthesis and optical properties of titanium dioxide thin film

NASA Astrophysics Data System (ADS)

Ullah, Irfan; Khattak, Shaukat Ali; Ahmad, Tanveer; Saman; Ludhi, Nayab Ali

2018-03-01

The titanium dioxide (TiO2) is synthesized by sol-gel method using titanium-tetra-iso-propoxide (TTIP) as a starting material, and deposited on the pre-cleaned glass substrate using spin coating technique at optimized parameters. Energy dispersive X-ray (EDX) spectroscopy confirms successful TiO2 growth. The optical properties concerning the transmission and absorption spectra show 85% transparency and 3.28 eV wide optical band gap for indirect transition, calculated from absorbance. The exponential behavior of absorption edge is observed and attributed to the localized states electronic transitions, curtailed in the indirect band gap of the thin film. The film reveals decreasing refractive index with increasing wavelength. The photoluminescence (PL) study ascertains that luminescent properties are due to the surface defects.

Effect of pulsed laser parameters on in-situ TiC synthesis in laser surface treatment

NASA Astrophysics Data System (ADS)

Hamedi, M. J.; Torkamany, M. J.; Sabbaghzadeh, J.

2011-04-01

Commercial titanium sheets pre-coated with 300-μm thick graphite layer were treated by employing a pulsed Nd:YAG laser in order to enhance surface properties such as wear and erosion resistance. Laser in-situ alloying method produced a composite layer by melting the titanium substrate and dissolution of graphite in the melt pool. Correlations between pulsed laser parameters, microstructure and microhardness of the synthesized composite coatings were investigated. Effects of pulse duration and overlapping factor on the microstructure and hardness of the alloyed layer were deduced from Vickers micro-indentation tests, XRD, SEM and metallographic analyses of cross sections of the generated layer. Results show that the composite cladding layer was constituted with TiC intermetallic phase between the titanium matrix in particle and dendrite forms. The dendritic morphology of composite layer was changed to cellular grain structure by increasing laser pulse duration and irradiated energy. High values of the measured hardness indicate that deposited titanium carbide increases in the conditions with more pulse duration and low process speed. This occurs due to more dissolution of carbon into liquid Ti by heat input increasing and positive influence of the Marangoni flow in the melted zone.

Influence of sulfurization temperature on Cu2ZnSnS4 absorber layer on flexible titanium substrates for thin film solar cells

NASA Astrophysics Data System (ADS)

Gokcen Buldu, Dilara; Cantas, Ayten; Turkoglu, Fulya; Gulsah Akca, Fatime; Meric, Ece; Ozdemir, Mehtap; Tarhan, Enver; Ozyuzer, Lutfi; Aygun, Gulnur

2018-02-01

In this study, the effect of sulfurization temperature on the morphology, composition and structure of Cu2ZnSnS4 (CZTS) thin films grown on titanium (Ti) substrates has been investigated. Since Ti foils are flexible, they were preferred as a substrate. As a result of their flexibility, they allow large area manufacturing and roll-to-roll processes. To understand the effects of sulfurization temperature on the CZTS formation on Ti foils, CZTS films fabricated with various sulfurization temperatures were investigated with several analyses including x-ray diffraction (XRD), scanning electron microscopy (SEM), x-ray photoelectron spectroscopy and Raman scattering. XRD measurements showed a sharp and intense peak coming from the (112) planes of the kesterite type lattice structure (KS), which is strong evidence for good crystallinity. The surface morphologies of our thin films were investigated using SEM. Electron dispersive spectroscopy was also used for the compositional analysis of the thin films. According to these analysis, it is observed that Ti foils were suitable as substrates for the growth of CZTS thin films with desired properties and the sulfurization temperature plays a crucial role for producing good quality CZTS thin films on Ti foil substrates.

Laser cladding of bioactive glass coatings.

PubMed

Comesaña, R; Quintero, F; Lusquiños, F; Pascual, M J; Boutinguiza, M; Durán, A; Pou, J

2010-03-01

Laser cladding by powder injection has been used to produce bioactive glass coatings on titanium alloy (Ti6Al4V) substrates. Bioactive glass compositions alternative to 45S5 Bioglass were demonstrated to exhibit a gradual wetting angle-temperature evolution and therefore a more homogeneous deposition of the coating over the substrate was achieved. Among the different compositions studied, the S520 bioactive glass showed smoother wetting angle-temperature behavior and was successfully used as precursor material to produce bioactive coatings. Coatings processed using a Nd:YAG laser presented calcium silicate crystallization at the surface, with a uniform composition along the coating cross-section, and no significant dilution of the titanium alloy was observed. These coatings maintain similar bioactivity to that of the precursor material as demonstrated by immersion in simulated body fluid. Copyright 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Tritium target manufacturing for use in accelerators

NASA Astrophysics Data System (ADS)

Bach, P.; Monnin, C.; Van Rompay, M.; Ballanger, A.

2001-07-01

As a neutron tube manufacturer, SODERN is now in charge of manufacturing tritium targets for accelerators, in cooperation with CEA/DAM/DTMN in Valduc. Specific deuterium and tritium targets are manufactured on request, according to the requirements of the users, starting from titanium target on copper substrate, and going to more sophisticated devices. A wide range of possible uses is covered, including thin targets for neutron calibration, thick targets with controlled loading of deuterium and tritium, rotating targets for higher lifetimes, or large size rotating targets for accelerators used in boron neutron therapy. Activity of targets lies in the 1 to 1000 Curie, diameter of targets being up to 30 cm. Special targets are also considered, including surface layer targets for lowering tritium desorption under irradiation, or those made from different kinds of occluders such as titanium, zirconium, erbium, scandium, with different substrates. It is then possible to optimize either neutron output, or lifetime and stability, or thermal behavior.

Methods of repairing a substrate

NASA Technical Reports Server (NTRS)

Riedell, James A. (Inventor); Easler, Timothy E. (Inventor)

2011-01-01

A precursor of a ceramic adhesive suitable for use in a vacuum, thermal, and microgravity environment. The precursor of the ceramic adhesive includes a silicon-based, preceramic polymer and at least one ceramic powder selected from the group consisting of aluminum oxide, aluminum nitride, boron carbide, boron oxide, boron nitride, hafnium boride, hafnium carbide, hafnium oxide, lithium aluminate, molybdenum silicide, niobium carbide, niobium nitride, silicon boride, silicon carbide, silicon oxide, silicon nitride, tin oxide, tantalum boride, tantalum carbide, tantalum oxide, tantalum nitride, titanium boride, titanium carbide, titanium oxide, titanium nitride, yttrium oxide, zirconium boride, zirconium carbide, zirconium oxide, and zirconium silicate. Methods of forming the ceramic adhesive and of repairing a substrate in a vacuum and microgravity environment are also disclosed, as is a substrate repaired with the ceramic adhesive.

Effect of nanostructured titanium on anodization growth of self-organized TiO2 nanotubes

NASA Astrophysics Data System (ADS)

Zhang, Lan; Han, Yong

2010-02-01

To understand the effect of substrate microstructure on the formation of TiO2 nanotubes, anodic oxidizations of commercially pure titanium subjected to surface mechanical attrition treatment (SMATed-Ti) and unSMATed-Ti in a glycol solution containing NH4F and small amounts of water were investigated. The SMATed-Ti exhibit a nanocrystallized surface layer containing a high density of grain boundaries compared with unSMATed-Ti. The anodization results show that the formed TiO2 nanotube layer on the SMATed-Ti is much thicker than that on the unSMATed-Ti. It is indicated that nanocrystallized Ti is propitious to the growth of TiO2 nanotubes; grain boundaries and dislocations play the leading role in accelerating the reaction rate and ion diffusion coefficient during anodization. In addition, nanocrystallization of Ti does not change surface morphologies and phase components of the TiO2 nanotubes.

The fabrication and in vitro properties of antibacterial polydopamine-LL-37-POPC coatings on micro-arc oxidized titanium.

PubMed

He, Ye; Zhang, Yangyang; Shen, Xinkun; Tao, Bailong; Liu, Ju; Yuan, Zhang; Cai, Kaiyong

2018-05-31

Bacterial infection commonly occurs in clinical settings when the procedure involves a medical implant. Thus, the fabrication of antimicrobial medical materials has attracted much attention in recent years. To improve the antibacterial properties of titanium (Ti)-based biomedical materials, surface microporous structures, with antimicrobial peptide coatings, were employed in this study. Native Ti substrates were endowed with a certain level of antibacterial activity after treatment with the micro-arc oxidation (MAO). A multilayer consisting of polydopamine, cationic antimicrobial peptides LL-37, and phospholipid (POPC) was coated onto MAO substrates, leading to antibacterial activity against both Gram-positive (S. aureus) and Gram-negative (E. coli) bacteria. The combination of polydopamine-LL-37-POPC was found to alleviate the burst release of LL-37 in the initial phase. This multilayer coated onto microporous Ti substrates also showed favorable cytocompatibility to both mesenchymal stem cells (MSCs) and osteoblasts. These findings illustrate a novel strategy for the development of antibacterial Ti-based implants. Copyright © 2018 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Henry, Michael David; Lewis, Rupert M.

The present invention relates to the use of gallium beam lithography to form superconductive structures. Generally, the method includes exposing a surface to gallium to form an implanted region and then removing material adjacent to and/or below that implanted region. In particular embodiments, the methods herein provide microstructures and nanostructures in any useful substrate, such as those including niobium, tantalum, tungsten, or titanium.

Effects of hydrogenated TiO2 nanotube arrays on protein adsorption and compatibility with osteoblast-like cells.

PubMed

Lu, Ran; Wang, Caiyun; Wang, Xin; Wang, Yuji; Wang, Na; Chou, Joshua; Li, Tao; Zhang, Zhenting; Ling, Yunhan; Chen, Su

2018-01-01

Modified titanium (Ti) substrates with titanium dioxide (TiO 2 ) nanotubes have broad usage as implant surface treatments and as drug delivery systems. To improve drug-loading capacity and accelerate bone integration with titanium, in this study, we hydrogenated anodized titanium dioxide nanotubes (TNTs) by a thermal treatment. Three groups were examined, namely: hydrogenated TNTs (H 2 -TNTs, test), unmodified TNTs (air-TNTs, control), and Ti substrates (Ti, control). Our results showed that oxygen vacancies were present in all the nanotubes. The quantity of -OH groups greatly increased after hydrogenation. Furthermore, the protein adsorption and loading capacity of the H 2 -TNTs were considerably enhanced as compared with the properties of the air-TNTs ( P <0.05). Additionally, time-of-flight secondary ion mass spectrometry (TOF-SIMS) was used to investigate the interactions of TNTs with proteins. During the protein-loading process, the H 2 -TNTs not only enabled rapid protein adsorption, but also decreased the rate of protein elution compared with that of the air-TNTs. We found that the H 2 -TNTs exhibited better biocompatibility than the air-TNT and Ti groups. Both cell adhesion activity and alkaline phosphatase activity were significantly improved toward MG-63 human osteoblast-like cells as compared with the control groups ( P <0.05). We conclude that hydrogenated TNTs could greatly improve the loading capacity of bioactive molecules and MG-63 cell proliferation.

Porous titanium obtained by a new powder metallurgy technique: Preliminary results of human osteoblast adhesion on surface polished substrates.

PubMed

Biasotto, M; Ricceri, R; Scuor, N; Schmid, C; Sandrucci, M A; Di Lenarda, R; Matteazzi, P

2003-01-01

This study concerns a novel powder metallurgy method for producing porous titanium (pTi) exhibiting high mechanical properties. The preparation procedure consisted of the following stages: first, the preparation of Ti and titanium hydride (TiH2) powder mixtures and their consolidation with a cold isostatic press, followed by a sintering of the green bodies performed with hot isostatic press (HIP) equipment. Thermal decomposition in controlled environment of the TiH2 phase results in the foam structure. The resulting porosity percolates with a volume fraction of approximately 20%. The final material exhibits interesting mechanical properties, comparable to those of full density titanium (between grade 2 and grade 3), with the advantage of a minor density. The samples produced were tested to verify their biological response by studying the effectiveness of osteoblast adhesion and growth. In this preliminary study, osteoblastic cell morphology was investigated and compared to that observed on fully dense commercially pure titanium (Ti-cp) (ASTM, grade 3). The preliminary results were promising regarding cellular adhesion and spreading. (Journal of Applied Biomaterials & Biomechanics 2003; 1: 172-7).

The role of the domain size and titanium dopant in nanocrystalline hematite thin films for water photolysis

DOE PAGES

Yan, Danhua; Tao, Jing; Kisslinger, Kim; ...

2015-10-13

Here we develop a novel technique for preparing high quality Ti-doped hematite thin films for photoelectrochemical (PEC) water splitting, through sputtering deposition of metallic iron films from an iron target embedded with titanium (dopants) pellets, followed by a thermal oxidation step that turns the metal films into doped hematite. It is found that the hematite domain size can be tuned from ~10 nm to over 100 nm by adjusting the sputtering atmosphere from more oxidative to mostly inert. The better crystallinity at a larger domain size ensures excellent PEC water splitting performance, leading to record high photocurrent from pure planarmore » hematite thin films on FTO substrates. Titanium doping further enhances the PEC performance of hematite photoanodes. The photocurrent is improved by 50%, with a titanium dopant concentration as low as 0.5 atom%. As a result, it is also found that the role of the titanium dopant in improving the PEC performance is not apparently related to the films’ electrical conductivity which had been widely believed, but is more likely due to the passivation of surface defects by the titanium dopants.« less

A study of the physical, chemical and biological properties of TiO2 coatings produced by micro-arc oxidation in a Ca-P-based electrolyte.

PubMed

dos Santos, Amanda; Araujo, Joyce R; Landi, Sandra M; Kuznetsov, Alexei; Granjeiro, José M; de Sena, Lidia Ágata; Achete, Carlos Alberto

2014-07-01

In this work, a porous and homogeneous titanium dioxide layer was grown on commercially pure titanium substrate using a micro-arc oxidation (MAO) process and Ca-P-based electrolyte. The structure and morphology of the TiO2 coatings were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy, and profilometry. The chemical properties were studied using electron dispersive X-ray spectroscopy (SEM-EDS) and X-ray photoelectron spectroscopy. The wettability of the coating was evaluated using contact angle measurements. During the MAO process, Ca and P ions were incorporated into the oxide layer. The TiO2 coating was composed of a mixture of crystalline and amorphous structures. The crystalline part of the sample consisted of a major anatase phase and a minor rutile phase. A cross-sectional image of the coating-substrate interface reveals the presence of voids elongated along the interface. An osteoblast culture was performed to verify the cytocompatibility of the anodized surface. The results of the cytotoxicity tests show satisfactory cell viability of the titanium dioxide films produced in this study.

Fabrication of free standing anodic titanium oxide membranes with clean surface using recycling process.

PubMed

Meng, Xianhui; Lee, Tae-Young; Chen, Huiyu; Shin, Dong-Wook; Kwon, Kee-Won; Kwon, Sang Jik; Yoo, Ji-Beom

2010-07-01

Large area of self-organized, free standing anodic titanium oxide (ATO) nanotube membranes with clean surfaces were facilely prepared to desired lengths via electrochemical anodization of highly pure Ti sheets in an ethylene glycol electrolyte, with a small amount of NH4F and H2O at 50 V, followed by self-detachment of the ATO membrane from the Ti substrate using recycling processes. In the first anodization step, the nanowire oxide layer existed over the well-arranged ATO nanotube. After sufficiently rinsing with water, the whole ATO layer was removed from the Ti sheet by high pressure N2 gas, and a well-patterned dimple layer with a thickness of about 30 nm existed on the Ti substrate. By using these naturally formed nano-scale pits as templates, in the second and third anodization process, highly ordered, vertically aligned, and free standing ATO membranes with the anodic aluminum oxide (AAO)-like clean surface were obtained. The inter-pore distance and diameter was 154 +/- 2 nm and 91+/- 2 nm, the tube arrays lengths for 25 and 46 hours were 44 and 70 microm, respectively. The present study demonstrates a simple approach to producing high quality, length controllable, large area TiO2 membrane.

Electrophoretic deposition of hydroxyapatite-hexagonal boron nitride composite coatings on Ti substrate.

PubMed

Göncü, Yapıncak; Geçgin, Merve; Bakan, Feray; Ay, Nuran

2017-10-01

In this study, commercial pure titanium samples were coated with nano hydroxyapatite-nano hexagonal boron nitride (nano HA-nano hBN) composite by electrophoretic deposition (EPD). The effect of process parameters (applied voltage, deposition time and solid concentration) on the coating morphology, thickness and the adhesion behavior were studied systematically and crack free nano hBN-nano HA composite coating production was achieved for developing bioactive coatings on titanium substrates for orthopedic applications. For the examination of structural and morphological characteristics of the coating surfaces, various complementary analysis methods were performed. For the structural characterization, XRD and Raman Spectroscopy were used while, Scanning Electron Microscopy (SEM) equipped with an energy dispersive spectrometer (EDS) and Transmission Electron Microscopy (TEM) techniques were carried out for revealing the morphological characterization. The results showed that nano HA-nano hBN were successfully deposited on Ti surface with uniform, crack-free coating by EPD. The amounts of hBN in suspension are considered to have no effect on coating thickness. By adding hBN into HA, the morphology of HA did not change and hBN has no significant effect on porous structure. These nanostructured surfaces are expected to be suitable for proliferation of cells and have high potential for bioactive materials. Copyright © 2017 Elsevier B.V. All rights reserved.

In vitro fatigue behaviour of vacuum plasma and detonation gun sprayed hydroxyapatite coatings.

PubMed

Gledhill, H C; Turner, I G; Doyle, C

2001-06-01

The fatigue behaviour of vacuum plasma sprayed (VPS) and detonation gun sprayed (DGUN) hydroxyapatite coatings on titanium substrates has been compared in air and in buffered Ringer's solution. There was an increase in the surface microcracking and bulk porosity of both types of coating tested in air. After 1 million cycles in Ringer's solution the VPS coatings had completely delaminated from their substrates. In contrast the DGUN coatings retained their integrity when tested up to 10 million cycles but were beginning to show signs of delamination at the interface.

Influence of substrate material and surface finishing on the morphology of the calcium-phosphate coating.

PubMed

Leitão, E; Barbosa, M A; de Groot, K

1997-07-01

The formation of an apatite-like layer was achieved by immersing Ti-6A1-4V, Ti-Al-2.5Fe, and 316 L stainless-steel substrata in Hank's balanced salt solution (HBSS). The layer was characterized by surface analysis techniques, namely X-ray microanalysis and X-ray diffraction, and the morphology was observed by scanning electron microscopy and atomic force microscopy. The concentrations of Ca and P were monitored as a function of time. The morphology of the precipitate layer seems to be dependent both on the type of metal substrate and its surface finish. Polished Ti-6A1-4V and Ti-Al-2.5Fe surfaces exhibit a plate precipitate morphology, whereas rougher surfaces show scattered crystal-like precipitation. The results suggest that the layer produced by immersion of polished titanium alloys in HBSS is constituted by an amorphous apatite.

Surface-enhanced Raman scattering of amorphous TiO2 thin films by gold nanostructures: Revealing first layer effect with thickness variation

NASA Astrophysics Data System (ADS)

Degioanni, S.; Jurdyc, A.-M.; Bessueille, F.; Coulm, J.; Champagnon, B.; Vouagner, D.

2013-12-01

In this paper, amorphous titanium dioxide (TiO2) thin films have been deposited on a commercially available Klarite substrate using the sol-gel process to produce surface-enhanced Raman scattering (SERS). The substrate consists of square arrays of micrometer-sized pyramidal pits in silicon with a gold coating. Several thin TiO2 layers have been deposited on the surface to study the influence of film thickness. Ultimately, we obtained information on SERS of an amorphous TiO2 layer by gold nanostructures, whose range is less than a few nanometers. Mechanisms responsible for the enhancement are the product of concomitant chemical and electromagnetic effects with an important contribution from plasmon-induced charge transfer.

Understanding Organic Film Behavior on Alloy and Metal Oxides

PubMed Central

Raman, Aparna; Quiñones, Rosalynn; Barriger, Lisa; Eastman, Rachel; Parsi, Arash

2010-01-01

Native oxide surfaces of stainless steel 316L and Nitinol alloys and their constituent metal oxides namely, nickel, chromium, molybdenum, manganese, iron and titanium were modified with long chain organic acids to better understand organic film formation. The adhesion and stability of films of octadecylphosphonic acid, octadecylhydroxamic acid, octadecylcarboxylic acid and octadecylsulfonic acid on these substrates was examined in this study. The films formed on these surfaces were analyzed by diffuse reflectance infrared Fourier transform spectroscopy, contact angle goniometry, atomic force microscopy and matrix assisted laser desorption ionization mass spectrometry. The effect of the acidity of the organic moiety and substrate composition on the film characteristics and stability is discussed. Interestingly, on the alloy surfaces, the presence of less reactive metal sites does not inhibit film formation. PMID:20039608

Design of a nitrogen-implanted titanium-based superelastic alloy with optimized properties for biomedical applications.

PubMed

Gordin, D M; Busardo, D; Cimpean, A; Vasilescu, C; Höche, D; Drob, S I; Mitran, V; Cornen, M; Gloriant, T

2013-10-01

In this study, a superelastic Ni-free Ti-based biomedical alloy was treated in surface by the implantation of nitrogen ions for the first time. The N-implanted surface was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and secondary ion mass spectroscopy, and the superficial mechanical properties were evaluated by nano-indentation and by ball-on-disk tribological tests. To investigate the biocompatibility, the corrosion resistance of the N-implanted Ti alloy was evaluated in simulated body fluids (SBF) complemented by in-vitro cytocompatibility tests on human fetal osteoblasts. After implantation, surface analysis methods revealed the formation of a titanium-based nitride on the substrate surface. Consequently, an increase in superficial hardness and a significant reduction of friction coefficient were observed compared to the non-implanted sample. Also, a better corrosion resistance and a significant decrease in ion release rates have been obtained. Cell culture experiments indicated that the cytocompatibility of the N-implanted Ti alloy was superior to that of the corresponding non-treated sample. Thus, this new functional N-implanted titanium-based superelastic alloy presents the optimized properties that are required for various medical devices: superelasticity, high superficial mechanical properties, high corrosion resistance and excellent cytocompatibility. Copyright © 2013 Elsevier B.V. All rights reserved.

A new method for production of titanium vapor and synthesis of titanium nitride coatings

NASA Astrophysics Data System (ADS)

Grigoriev, Sergey N.; Melnik, Yury A.; Metel, Alexander S.; Volosova, Marina A.

2018-03-01

It is proposed to synthesize on machine parts and cutting tools wear-resistant titanium nitride coatings with the help of the hollow-cathode glow discharge, a molybdenum crucible for titanium evaporation being used as the anode of the discharge and a process vacuum chamber being used as the hollow cathode. The research revealed that at the anode surface area less than a critical value S* = (2m/M)1/2S, where S is the area of the chamber walls, m is the mass of electrons and M is the mass of ions, the anode fall of potential is positive and grows from ˜50 V at argon pressure p = 0.2 Pa to ˜2 kV at p = 0.02 Pa. At the discharge current I = 0.6 A electrons accelerated by the anode fall of 0.9 kV transport into the crucible with the inner diameter of 12 mm the power of ˜0.54 kW, which allows the titanium evaporation and the coating deposition rate of 5 µm·h-1 on a substrate distanced from the crucible at 100 mm. After the argon is replaced with the nitrogen, titanium nitride coating without titanium droplets is synthesized the deposition rate amounting to about the same value.

A novel anti-frictional multiphase layer produced by plasma nitriding of PVD titanium coated ZL205A aluminum alloy

NASA Astrophysics Data System (ADS)

Lu, C.; Yao, J. W.; Wang, Y. X.; Zhu, Y. D.; Guo, J. H.; Wang, Y.; Fu, H. Y.; Chen, Z. B.; Yan, M. F.

2018-02-01

The heat treatment (consisting of solid solution and aging), is integrated with the nitriding process of titanium coated ZL205A aluminum alloy to improve the surface and matrix mechanical properties simultaneously. Two-step duplex treatment is adopted to prepare the gradient multiphase layer on a magnesium-free ZL205A aluminum-copper based alloy. Firstly, pure titanium film is deposited on the aluminum alloy substrate using magnetron sputtering. Secondly, the Ti-coated specimen is nitrided at the solid solution temperature of the substrate alloying elements in a gas mixture of N2 and H2 and aged at 175 °C. The microstructure evolution, microhardness as well as the wear resistance of obtained multiphase layers are investigated by means of scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometer (EDS), microhardness tester and pin-on-disc tribometer. The multiphase layer, dominated by TiN0.3 or Al3Ti, is prepared with significantly increased layer depth after duplex treatment. The surface hardness of multiphase layer is remarkably improved from 23.7HV to 457HV. The core matrix hardness is also increased to 65HV after aging. The wear rate of the multiphase layer decreases about 55.22% and 49.28% in comparison with the aged and Ti coated specimens, respectively. The predominant wear mechanism for the multiphase layer is abrasive and oxidation, but severe adhesive wear for the aged and Ti coated specimens.

Photoluminescence in the characterization and early detection of biomimetic bone-like apatite formation on the surface of alkaline-treated titanium implant: state of the art.

PubMed

Sepahvandi, Azadeh; Moztarzadeh, Fathollah; Mozafari, Masoud; Ghaffari, Maryam; Raee, Nahid

2011-09-01

Photoluminescence (PL) property is particularly important in the characterization of materials that contain significant proportions of noncrystalline components, multiple phases, or low concentrations of mineral phases. In this research, the ability of biomimetic bone-like apatite deposition on the surface of titanium alloy (Ti6Al4V) substrates in simulated body fluid (SBF) right after alkaline-treatment and subsequent heat-treatment was studied by the inherent luminescence properties of apatite. For this purpose, the metallic substrates were treated in 5 M NaOH solution at 60 °C. Subsequently, the substrates were heat-treated at 600 °C for 1 h for consolidation of the sodium titanate hydrogel layer. Then, they were soaked in SBF for different periods of time. Finally, the possibility to use of PL monitoring as an effective method and early detection tool is discussed. According to the obtained results, it was concluded that the PL emission peak did not have any significant shift to the shorter or higher wavelengths, and the PL intensity increased as the exposure time increased. This research proved that the observed inherent PL of the newly formed apatite coatings might be of specific interest for histological probing and bone remodelling monitoring. Copyright © 2011 Elsevier B.V. All rights reserved.

Interaction of carbon nanotubes coatings with titanium substrate

NASA Astrophysics Data System (ADS)

Fraczek-Szczypta, Aneta; Wedel-Grzenda, Alicja; Benko, Aleksandra; Grzonka, Justyna; Mizera, Jaroslaw

2017-02-01

The aim of this study was to evaluate the impact of multi-walled carbon nanotubes (MWCNTs) after chemical surface functionalization on the interaction with a titanium surface. Two kinds of MWCNTs differing in terms of concentration of functional groups were deposited on the Ti surface using the electrophoretic deposition method (EPD). The study has shown the detailed analysis of the physicochemical properties of this form of carbon nanomaterial and received on their base coatings using various techniques, such as scanning electron microscopy (SEM), confocal microscopy, X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The adhesion of the MWCNTs coatings to the Ti surface was determined using the shear test method, according to standard ASTM F-1044-05. These results indicated that one type of MWCNTs characterized by a higher concentration of functional groups has better adhesion to the metal surface than the second type. Analysis of the MWCNT-metal interface using Raman spectroscopy and SEM and STEM indicates the presence of phase built of MWCNT and TiO2. This phase could be a type of nanocomposite that affects the improvement of the adhesion of MWCNT to the Ti surface.

Laser engineered multilayer coating of biphasic calcium phosphate/titanium nanocomposite on metal substrates.

PubMed

Zhang, Martin Yi; Ye, Chang; Erasquin, Uriel Joseph; Huynh, Toan; Cai, Chengzhi; Cheng, Gary J

2011-02-01

In this work, laser coating of biphasic calcium phosphate/titanium (BCP/Ti) nanocomposite on Ti-6Al-4 V substrates was developed. A continuous wave neodymium-doped yttrium aluminium garnet (Nd:YAG) laser was used to form a robust multilayer of BCP/Ti nanocomposite starting from hydroxyapatite and titanium nanoparticles. In this process, low power coating is realized because of the strong laser-nanoparticle interaction and good sinterability of nanosized titanium. To guide the optimization of laser processing conditions for the coating process, a multiphysics model coupling electromagnetic module with heat transfer module was developed. This model was validated by laser coating experiments. Important features of the coated samples, including microstructures, chemical compositions, and interfacial bonding strength, were characterized. We found that a multilayer of BCP, consisting of 72% hydroxyapatite (HA) and 28% beta-tricalcium phosphate (β-TCP), and titanium nanocomposite was formed on Ti-6Al-4 V substrates. Significantly, the coating/substrate interfacial bonding strength was found to be two times higher than that of the commercial plasma sprayed coatings. Preliminary cell culture studies showed that the resultant BCP/Ti nanocomposite coating supported the adhesion and proliferation of osteoblast-like UMR-106 cells.

Influence of spacer length on heparin coupling efficiency and fibrinogen adsorption of modified titanium surfaces

PubMed Central

Tebbe, David; Thull, Roger; Gbureck, Uwe

2007-01-01

Background Chemical bonding of the drug onto surfaces by means of spacer molecules is accompanied with a reduction of the biological activity of the drug due to a constricted mobility since normally only short spacer molecule like aminopropyltrimethoxysilane (APMS) are used for drug coupling. This work aimed to study covalent attachment of heparin to titanium(oxide) surfaces by varying the length of the silane coupling agent, which should affect the biological potency of the drug due to a higher mobility with longer spacer chains. Methods Covalent attachment of heparin to titanium metal and TiO2 powder was carried out using the coupling agents 3-(Trimethoxysilyl)-propylamine (APMS), N- [3-(Trimethoxysilyl)propyl]ethylenediamine (Diamino-APMS) and N1- [3-(Trimethoxy-silyl)-propyl]diethylenetriamine (Triamino-APMS). The amount of bound coupling agent and heparin was quantified photometrically by the ninhydrin reaction and the tolidine-blue test. The biological potency of heparin was determined photometrically by the chromogenic substrate Chromozym TH and fibrinogen adsorption to the modified surfaces was researched using the QCM-D (Quartz Crystal Microbalance with Dissipation Monitoring) technique. Results Zeta-potential measurements confirmed the successful coupling reaction; the potential of the unmodified anatase surface (approx. -26 mV) shifted into the positive range (> + 40 mV) after silanisation. Binding of heparin results in a strongly negatively charged surface with zeta-potentials of approx. -39 mV. The retaining biological activity of heparin was highest for the spacer molecule Triamino-APMS. QCM-D measurements showed a lower viscosity for adsorbed fibrinogen films on heparinised surfaces by means of Triamino-APMS. Conclusion The remaining activity of heparin was found to be highest for the covalent attachment with Triamino-APMS as coupling agent due to the long chain of this spacer molecule and therefore the highest mobility of the drug. Furthermore, the adsorption of fibrinogen on the differently heparinised surfaces in real time demonstrated that with longer spacer chains the ΔD/Δf ratios became higher, which is also associated with better biocompatible properties of the substrates in contact with a biosystem. PMID:17640335

The influence of surface chemistry and topography on the contact guidance of MG63 osteoblast cells.

PubMed

Ismail, F S Magdon; Rohanizadeh, R; Atwa, S; Mason, R S; Ruys, A J; Martin, P J; Bendavid, A

2007-05-01

The purpose of the present study was to determine in vitro the effects of different surface topographies and chemistries of commercially pure titanium (cpTi) and diamond-like carbon (DLC) surfaces on osteoblast growth and attachment. Microgrooves (widths of 2, 4, 8 and 10 microm and a depth of 1.5-2 microm) were patterned onto silicon (Si) substrates using microlithography and reactive ion etching. The Si substrates were subsequently vapor coated with either cpTi or DLC coatings. All surfaces were characterized using atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and contact angle measurements. Using the MG63 Osteoblast-Like cell line, we determined cell viability, adhesion, and morphology on different substrates over a 3 day culture period. The results showed cpTi surfaces to be significantly more hydrophilic than DLC for groove sizes larger than 2 microm. Cell contact guidance was observed for all grooved samples in comparison to the unpatterned controls. The cell viability tests indicated a significantly greater cell number for 8 and 10 microm grooves on cpTi surfaces compared to other groove sizes. The cell adhesion study showed that the smaller groove sizes, as well as the unpatterned control groups, displayed better cell adhesion to the substrate.

Modulation of human dermal microvascular endothelial cell and human gingival fibroblast behavior by micropatterned silica coating surfaces for zirconia dental implant applications

PubMed Central

Laranjeira, Marta S; Carvalho, Ângela; Pelaez-Vargas, Alejandro; Hansford, Derek; Ferraz, Maria Pia; Coimbra, Susana; Costa, Elísio; Santos-Silva, Alice; Fernandes, Maria Helena; Monteiro, Fernando Jorge

2014-01-01

Dental ceramic implants have shown superior esthetic behavior and the absence of induced allergic disorders when compared to titanium implants. Zirconia may become a potential candidate to be used as an alternative to titanium dental implants if surface modifications are introduced. In this work, bioactive micropatterned silica coatings were produced on zirconia substrates, using a combined methodology of sol–gel processing and soft lithography. The aim of the work was to compare the in vitro behavior of human gingival fibroblasts (HGFs) and human dermal microvascular endothelial cells (HDMECs) on three types of silica-coated zirconia surfaces: flat and micropatterned (with pillars and with parallel grooves). Our results showed that cells had a higher metabolic activity (HGF, HDMEC) and increased gene expression levels of fibroblast-specific protein-1 (FSP-1) and collagen type I (COL I) on surfaces with pillars. Nevertheless, parallel grooved surfaces were able to guide cell growth. Even capillary tube-like networks of HDMEC were oriented according to the surface geometry. Zirconia and silica with different topographies have shown to be blood compatible and silica coating reduced bacteria adhesion. All together, the results indicated that microstructured bioactive coating seems to be an efficient strategy to improve soft tissue integration on zirconia implants, protecting implants from peri-implant inflammation and improving long-term implant stabilization. This new approach of micropatterned silica coating on zirconia substrates can generate promising novel dental implants, with surfaces that provide physical cues to guide cells and enhance their behavior. PMID:27877662

Modulation of human dermal microvascular endothelial cell and human gingival fibroblast behavior by micropatterned silica coating surfaces for zirconia dental implant applications

NASA Astrophysics Data System (ADS)

Laranjeira, Marta S.; Carvalho, Ângela; Pelaez-Vargas, Alejandro; Hansford, Derek; Ferraz, Maria Pia; Coimbra, Susana; Costa, Elísio; Santos-Silva, Alice; Fernandes, Maria Helena; Monteiro, Fernando Jorge

2014-04-01

Dental ceramic implants have shown superior esthetic behavior and the absence of induced allergic disorders when compared to titanium implants. Zirconia may become a potential candidate to be used as an alternative to titanium dental implants if surface modifications are introduced. In this work, bioactive micropatterned silica coatings were produced on zirconia substrates, using a combined methodology of sol-gel processing and soft lithography. The aim of the work was to compare the in vitro behavior of human gingival fibroblasts (HGFs) and human dermal microvascular endothelial cells (HDMECs) on three types of silica-coated zirconia surfaces: flat and micropatterned (with pillars and with parallel grooves). Our results showed that cells had a higher metabolic activity (HGF, HDMEC) and increased gene expression levels of fibroblast-specific protein-1 (FSP-1) and collagen type I (COL I) on surfaces with pillars. Nevertheless, parallel grooved surfaces were able to guide cell growth. Even capillary tube-like networks of HDMEC were oriented according to the surface geometry. Zirconia and silica with different topographies have shown to be blood compatible and silica coating reduced bacteria adhesion. All together, the results indicated that microstructured bioactive coating seems to be an efficient strategy to improve soft tissue integration on zirconia implants, protecting implants from peri-implant inflammation and improving long-term implant stabilization. This new approach of micropatterned silica coating on zirconia substrates can generate promising novel dental implants, with surfaces that provide physical cues to guide cells and enhance their behavior.

Preparation, characterization, and biological properties of organic-inorganic nanocomposite coatings on titanium substrates prepared by sol-gel.

PubMed

Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando

2014-02-01

When surface-reactive (bioactive) coatings are applied to medical implants by means of the sol-gel dip-coating technique, the biological proprieties of the surface of the implant can be locally modified to match the properties of the surrounding tissues to provide a firm fixation of the implant. The aim of this study has been to synthesize, via sol-gel, organoinorganic nanoporous materials and to dip-coat a substrate to use in dental applications. Different systems have been prepared consisting of an inorganic zirconium-based matrix, in which a biodegradable polymer, the poly-ε-caprolactone was incorporated in different percentages. The materials synthesized by the sol-gel process, before gelation, when they were still in sol phase, have been used to coat a titanium grade 4 (Ti-4) substrate to change its surface biological properties. Thin films have been obtained by means of the dip-coating technique. A microstructural analysis of the obtained coatings was performed using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy. The biological proprieties have been investigated by means of tests in vitro. The bone-bonding capability of the nanocomposite films has been evaluated by examining the appearance of apatite on their surface when plunged in a simulated body fluid (SBF) with ion concentrations nearly equal to those of human blood plasma. The examination of apatite formation on the nanocomposites, after immersion in SBF, has been carried out by SEM equipped with energy-dispersive X-ray spectroscopy. To evaluate cells-materials interaction, human osteosarcoma cell line (Saos-2) has been seeded on specimens and cell vitality evaluated by WST-8 assay. © 2013 Wiley Periodicals, Inc.

The effect of different surface treatments on the bond strength of a gingiva-colored indirect composite veneering material to three implant framework materials.

PubMed

Koizuka, Mai; Komine, Futoshi; Blatz, Markus B; Fushiki, Ryosuke; Taguchi, Kohei; Matsumura, Hideo

2013-09-01

To evaluate and compare the shear-bond strength of a gingiva-colored indirect composite material to three different implant framework materials (zirconia ceramics, gold alloy, and titanium), and to investigate the effect of surface pretreatment by air-particle abrasion and four priming agents. A gingiva-colored indirect composite (Ceramage) was bonded to three framework materials (n = 80): commercially pure titanium (CP- Ti ), ADA (American Dental Association)-type 4 casting gold alloy (Type IV), and zirconia ceramics (Zirconia) with or without airborne-particle abrasion. Before bonding, the surface of the specimens was treated using no (control) or one of four priming agents: Alloy Primer (ALP), Estenia Opaque Primer (EOP), Metal Link Primer (MLP), and V-Primer (VPR). Shear-bond strength was determined after 24-h wet storage. Data were analyzed using Steel-Dwass for multiple comparisons, and Mann-Whitney U-test (P = 0.05). For both CP- Ti and Zirconia substrates, three groups, ALP, EOP, and MLP, showed significantly higher bond strengths (P < 0.05) than the other groups with or without airborne-particle abrasion. For Type IV substrates, significantly higher bond strengths were obtained in ALP and MLP groups (P < 0.01) compared with the other groups with airborne-particle abrasion. Application of priming agents containing specific phosphoric ester groups significantly enhances the bond strength of a gingiva-colored composite material to commercially pure titanium and zirconia frameworks. Combined use of a thione monomer with a phosphoric monomer enhances the bond strengths to airborne-particle abraded type IV gold alloy. © 2012 John Wiley & Sons A/S.

Processing of hydroxylapatite coatings on titanium alloy bone prostheses

DOEpatents

Nastasi, M.A.; Levine, T.E.; Mayer, J.W.; Pizziconi, V.B.

1998-10-06

Processing of hydroxylapatite sol-gel films on titanium alloy bone prostheses. A method utilizing non-line-of-sight ion beam implantation and/or rapid thermal processing to provide improved bonding of layers of hydroxylapatite to titanium alloy substrates while encouraging bone ingrowth into the hydroxylapatite layers located away from the substrate, is described for the fabrication of prostheses. The first layer of hydroxylapatite is mixed into the substrate by the ions or rapidly thermally annealed, while subsequent layers are heat treated or densified using ion implantation to form layers of decreasing density and larger crystallization, with the outermost layers being suitable for bone ingrowth.

Processing of hydroxylapatite coatings on titanium alloy bone prostheses

DOEpatents

Nastasi, Michael A.; Levine, Timothy E.; Mayer, James W.; Pizziconi, Vincent B.

1998-01-01

Processing of hydroxylapatite sol-gel films on titanium alloy bone prostheses. A method utilizing non-line-of-sight ion beam implantation and/or rapid thermal processing to provide improved bonding of layers of hydroxylapatite to titanium alloy substrates while encouraging bone ingrowth into the hydroxylapatite layers located away from the substrate, is described for the fabrication of prostheses. The first layer of hydroxylapatite is mixed into the substrate by the ions or rapidly thermally annealed, while subsequent layers are heat treated or densified using ion implantation to form layers of decreasing density and larger crystallization, with the outermost layers being suitable for bone ingrowth.

Sol-gel modification of wood substrates to retard weathering

Treesearch

Mandla A Tshabalala; Sam Williams

2008-01-01

Wood specimens were treated with sol-gel systems based on metalorganic precursors of silicon (Si), iron (Fe), zirconium (Zr), and titanium (Ti). The effect of these sol-gel systems on weathering properties of wood was investigated. These sol-gel systems were found to have a positive effect on surface color stability and water vapor resistance of the specimens. Under...

An Investigation into the Effects of Process Conditions on the Tribological Performance of Pack Carburized Titanium with Limited Oxygen Diffusion

NASA Astrophysics Data System (ADS)

Bailey, R.; Sun, Y.

2018-04-01

In the present study, a new pack carburization technique for titanium has been investigated. The aim of this treatment is to produce a titanium carbide/oxycarbide layer atop of an extended oxygen diffusion zone [α-Ti(O)]. The effects of treatment temperature and pack composition have been investigated in order to determine the optimal conditions required to grant the best tribological response. The resulting structural features were investigated with particular interest in the carbon and oxygen concentrations across the samples cross section. The optimization showed that a temperature of 925 °C with a pack composition of 1 part carbon to 1 part energizer produced surface capable of withstanding a contact pressure of ≈ 1.5 GPa for 1 h. The process resulted in TiC surface structure which offers enhanced hardness (2100 HV) and generates a low friction coefficient (μ ≈ 0.2) when in dry sliding contact with an alumina (Al2O3) ball. The process also produced an extended oxygen diffusion zone that helps to improve the load bearing capacity of the substrate.

Studies of the micromorphology of sputtered TiN thin films by autocorrelation techniques

NASA Astrophysics Data System (ADS)

Smagoń, Kamil; Stach, Sebastian; Ţălu, Ştefan; Arman, Ali; Achour, Amine; Luna, Carlos; Ghobadi, Nader; Mardani, Mohsen; Hafezi, Fatemeh; Ahmadpourian, Azin; Ganji, Mohsen; Grayeli Korpi, Alireza

2017-12-01

Autocorrelation techniques are crucial tools for the study of the micromorphology of surfaces: They provide the description of anisotropic properties and the identification of repeated patterns on the surface, facilitating the comparison of samples. In the present investigation, some fundamental concepts of these techniques including the autocorrelation function and autocorrelation length have been reviewed and applied in the study of titanium nitride thin films by atomic force microscopy (AFM). The studied samples were grown on glass substrates by reactive magnetron sputtering at different substrate temperatures (from 25 {}°C to 400 {}°C , and their micromorphology was studied by AFM. The obtained AFM data were analyzed using MountainsMap Premium software obtaining the correlation function, the structure of isotropy and the spatial parameters according to ISO 25178 and EUR 15178N. These studies indicated that the substrate temperature during the deposition process is an important parameter to modify the micromorphology of sputtered TiN thin films and to find optimized surface properties. For instance, the autocorrelation length exhibited a maximum value for the sample prepared at a substrate temperature of 300 {}°C , and the sample obtained at 400 {}°C presented a maximum angle of the direction of the surface structure.

Relevant insight of surface characterization techniques to study covalent grafting of a biopolymer to titanium implant and its acidic resistance

NASA Astrophysics Data System (ADS)

D'Almeida, Mélanie; Amalric, Julien; Brunon, Céline; Grosgogeat, Brigitte; Toury, Bérangère

2015-02-01

Peri-implant bacterial infections are the main cause of complications in dentistry. Our group has previously proposed the attachment of chitosan on titanium implants via a covalent bond to improve its antibacterial properties while maintaining its biocompatibility. A better knowledge of the coating preparation process allows a better understanding of the bioactive coating in biological conditions. In this work, several relevant characterization techniques were used to assess an implant device during its production phase and its resistance in natural media at different pH. The titanium surface was functionalized with 3-aminopropyltriethoxysilane (APTES) followed by grafting of an organic coupling agent; succinic anhydride, able to form two covalent links, with the substrate through a Ti-O-Si bond and the biopolymer through a peptide bond. Each step of the coating synthesis as well as the presence confirmation of the biopolymer on titanium after saliva immersion was followed by FTIR-ATR, SEM, EDS, 3D profilometry, XPS and ToF-SIMS analyses. Results allowed to highlight the efficiency of each step of the process, and to propose a mechanism occurring during the chitosan coating degradation in saliva media at pH 5 and at pH 3.

Modeling of the interaction between osteoblasts and biocompatible substrates as a function of adhesion strength.

PubMed

Portan, D V; Deligianni, D D; Deligianni, K; Kroustalli, A A; Tyllianakis, M; Papanicolaou, G C

2018-03-01

A goal of current implantology research is to design devices that induce controlled, guided, and rapid healing. Nanoscale structured substrates [e.g., titania nanotubes (TNTs) or carbon nanotubes (CNTs)] dramatically improve the functions of conventional biomaterials. The present investigation evaluated the behavior of osteoblasts cells cultured on smooth and nanostructured substrates, by measuring osteoblasts specific biomarkers [alkaline phosphatase (AP) and total protein] and cells adhesion strength to substrates, followed by semi-empirical modeling to predict the experimental results. Findings were in total agreement with the current state of the art. The proliferation, as well as the AP and total protein levels were higher on the nanostructure phases (TNTs, CNTs) comparing to the smooth ones (plastic and pure titanium). Cells adhesion strength measured was found higher on the nanostructured materials. This coincided with a higher value of proteins which are directly implicated in the process of adherence. Results were accurately predicted through the Viscoelastic Hybrid Interphase Model. A gradual adherence of bone cells to implants using multilayered biomaterials that involve biodegradable polymeric films and a nanoscale modification of titanium surface is suggested to improve performance through an interphase-mediated osteointegration of orthopedic implants. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 106A: 621-628, 2018. © 2017 Wiley Periodicals, Inc.

The Cross-Sectional Investigation of Oxide Scale FeCr Alloys and Commercial Ferritic Steel Implanted with Lanthanum and Titanium Dopants after Oxidation Test at 900°C

NASA Astrophysics Data System (ADS)

Saryanto, Hendi; Sebayang, Darwin; Untoro, Pudji; Sujitno, Tjipto

2018-03-01

The cross-sectional examinations of oxide scales formed by oxidation on the surface of FeCr alloys and Ferritic Steel that implanted with lanthanum and titanium dopants were observed and investigated. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS) has been used to study the cross-sectional oxides produced by specimens after oxidation process. X-ray diffraction (XRD) analysis was used to strengthen the analysis of the oxide scale morphology, oxide phases and oxidation products. Cross-sectional observations show the effectiveness of La implantation for improving thinner and stronger scale/substrate interface during oxidation process. The result shows that the thickness of oxide scales formed on the surface of La implanted FeCr alloy and ferritic steel was found less than 3 μm and 300 μm, respectively. The oxide scale formed on the surface of La implanted specimens consisted roughly of Cr2O3 with a small amount of FeO mixture, which indicates that lanthanum implantation can improve the adherence, reduce the growth of the oxide scale as well as reduce the Cr evaporation. On the other side, the oxide scale formed on the surface of FeCr alloys and ferritic steel that implanted with titanium dopant was thicker, indicating that significant increase in oxidation mass gain. It can be noticed that titanium implantation ineffectively promotes Cr rich oxide. At the same time, the amount of Fe increased and diffused outwards, which caused the formation and rapid growth of FeO.

IN SITU Deposition of Fe-TiC Nanocomposite on Steel by Laser Cladding

NASA Astrophysics Data System (ADS)

Razavi, Mansour; Rahimipour, Mohammad Reza; Ganji, Mojdeh; Ganjali, Mansoreh; Gangali, Monireh

The possibility of deposition of Fe-TiC nanocomposite on the surface of carbon steel substrate with the laser coating method had been investigated. Mechanical milling was used for the preparation of raw materials. The mixture of milled powders was used as a coating material on the substrate steel surface and a CO2 laser was used in continuous mode for coating. Microstructural studies were performed by scanning electron microscopy. Determinations of produced phases, crystallite size and mean strain have been done by X-ray diffraction. The hardness and wear resistance of coated samples were measured. The results showed that the in situ formation of Fe-TiC nanocomposite coating using laser method is possible. This coating has been successfully used to improve the hardness and wear resistance of the substrate so that the hardness increased by about six times. Coated iron and titanium carbide crystallite sizes were in the nanometer scale.

Diffusion Bonding of Silicon Carbide for MEMS-LDI Applications

NASA Technical Reports Server (NTRS)

Halbig, Michael C.; Singh, Mrityunjay; Shpargel, Tarah P.; Kiser, J. Douglas

2007-01-01

A robust joining approach is critically needed for a Micro-Electro-Mechanical Systems-Lean Direct Injector (MEMS-LDI) application which requires leak free joints with high temperature mechanical capability. Diffusion bonding is well suited for the MEMS-LDI application. Diffusion bonds were fabricated using titanium interlayers between silicon carbide substrates during hot pressing. The interlayers consisted of either alloyed titanium foil or physically vapor deposited (PVD) titanium coatings. Microscopy shows that well adhered, crack free diffusion bonds are formed under optimal conditions. Under less than optimal conditions, microcracks are present in the bond layer due to the formation of intermetallic phases. Electron microprobe analysis was used to identify the reaction formed phases in the diffusion bond. Various compatibility issues among the phases in the interlayer and substrate are discussed. Also, the effects of temperature, pressure, time, silicon carbide substrate type, and type of titanium interlayer and thickness on the microstructure and composition of joints are discussed.

Chitosan-58S bioactive glass nanocomposite coatings on TiO2 nanotube: Structural and biological properties

NASA Astrophysics Data System (ADS)

Mokhtari, H.; Ghasemi, Z.; Kharaziha, M.; Karimzadeh, F.; Alihosseini, F.

2018-05-01

Bacterial infection and insignificant osseointegration have been recognized as the main reasons of the failures of titanium based implants. The aim of this study was to apply titanium oxide nanotube (TNT) array on titanium using electrochemical anodization process as a more appropriate substrate for chitosan and chitosan-58S bioactive glass (BG) (58S-BG-Chitosan) nanocomposite coatings covered TNTs (TNT/Chiosan, TNT/58S-BG-Chitosan, respectively) through a conventional dip-coating process. Results showed that a TNT layer with average inner diameter of 82 ± 19 nm and wall's thickness of 23 ± 9 nm was developed on titanium surface using electrochemical anodization process. Roughness and contact angle measurement showed that TNT with Ra = 449 nm had highest roughness and hydrophilicity which then reduced to 86 nm and 143 nm for TNT/Chitosan and TNT/58S-BG-Chitosan, respectively. In vitro bioactivity evaluation in simulated buffer fluid (SBF) solution and antibacterial activity assay predicted that TNT/58S-BG-Chitosan was superior in bone like apatite formation and antibacterial activity against both gram-positive and gram-negative bacteria compared to Ti, TNT and TNT/Chitosan samples, respectively. Results revealed the noticeable MG63 cell attachment and proliferation on TNT/58S-BG-Chitosan coating compared to those of uncoated TNTs. These results confirmed the positive effect of using TNT substrate for natural polymer coating on improved bioactivity of implant.

Parameter optimization for Ag-coated TiO2 nanotube arrays as recyclable SERS substrates

NASA Astrophysics Data System (ADS)

Sun, Yuyang; Yang, Lulu; Liao, Fan; Dang, Qian; Shao, Mingwang

2018-06-01

The Ag-coated titanium dioxide nanotube arrays (Ag-coated TNTs) are obtained via the deposition of Ag nanoparticles on the two-step anodized TNTs. The wall thickness of TNTs is modulated via finite difference time domain simulation to get the favorable electromagnetic field for surface enhanced Raman scattering (SERS). Ag-coated TNTs with optimal wall thickness of 20 nm were employed as the SERS substrates to detect 2-mercaptobenzoxazole, which show superior detection sensitivity and uniformity. In addition, due to the photocatalysis of TNTs, the SERS substrates could clean themselves and be repeatedly used by photo-degradation of target molecules under the ultra-violet irradiation. The Ag-coated TNTs are a kind of bifunctional SERS substrates which can produce high-quality SERS signals and reuse to reduce the cost.

Improvement of the titanium implant biological properties by coating with poly (ε-caprolactone)-based hybrid nanocomposites synthesized via sol-gel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Catauro, Michelina; Bollino, Flavia; Papale, Ferdinando

When bioactive coatings are applied to medical implants by means of sol-gel dip coating technique, the biological proprieties of the implant surface can be modified to match the properties of the surrounding tissues. In this study organo-inorganic nanocomposites materials were synthesized via sol-gel. They consisted of an inorganic zirconium-based and silica-based matrix, in which a biodegradable polymer (the poly-ε-caprolactone, PCL) was incorporated in different weight percentages. The synthesized materials, in sol phase, were used to dip-coat a substrate of commercially pure titanium grade 4 (CP Ti gr. 4) in order to improve its biological properties. A microstructural analysis of themore » obtained films was carried out by scanning electron microscopy (SEM) and attenuated total reflectance (ATR) Fourier transform infrared spectroscopy (FT-IR). Biological proprieties of the coated substrates were investigated by means of in vitro tests.« less

Surface laser marking optimization using an experimental design approach

NASA Astrophysics Data System (ADS)

Brihmat-Hamadi, F.; Amara, E. H.; Lavisse, L.; Jouvard, J. M.; Cicala, E.; Kellou, H.

2017-04-01

Laser surface marking is performed on a titanium substrate using a pulsed frequency doubled Nd:YAG laser ( λ= 532 nm, τ pulse=5 ns) to process the substrate surface under normal atmospheric conditions. The aim of the work is to investigate, following experimental and statistical approaches, the correlation between the process parameters and the response variables (output), using a Design of Experiment method (DOE): Taguchi methodology and a response surface methodology (RSM). A design is first created using MINTAB program, and then the laser marking process is performed according to the planned design. The response variables; surface roughness and surface reflectance were measured for each sample, and incorporated into the design matrix. The results are then analyzed and the RSM model is developed and verified for predicting the process output for the given set of process parameters values. The analysis shows that the laser beam scanning speed is the most influential operating factor followed by the laser pumping intensity during marking, while the other factors show complex influences on the objective functions.

Characterisation of DLC films deposited using titanium isopropoxide (TIPOT) at different flow rates.

PubMed

Said, R; Ali, N; Ghumman, C A A; Teodoro, O M N D; Ahmed, W

2009-07-01

In recent years, there has been growing interest in the search for advanced biomaterials for biomedical applications, such as human implants and surgical cutting tools. It is known that both carbon and titanium exhibit good biocompatibility and have been used as implants in the human body. It is highly desirable to deposit biocompatible thin films onto a range of components in order to impart biocompatibility and to minimise wear in implants. Diamond like carbon (DLC) is a good candidate material for achieving biocompatibility and low wear rates. In this study, thin films of diamond-like-carbon DLC were deposited onto stainless steel (316) substrates using C2H2, argon and titanium isopropoxide (TIPOT) precursors. Argon was used to generate the plasma in the plasma enhanced vapour deposition (PECVD) system. A critical coating feature governing the performance of the component during service is film thickness. The as-grown films were in the thickness range 90-100 nm and were found to be dependent on TIPOT flow rate. Atomic force microscopy (AFM) was used to characterise the surface roughness of the samples. As the flow rate of TIPOT increased the average roughness was found to increase in conjunction with the film thickness. Raman spectroscopy was used to investigate the chemical structure of amorphous carbon matrix. Surface tension values were calculated using contact angle measurements. In general, the trend of the surface tension results exhibited an opposite trend to that of the contact angle. The elemental composition of the samples was characterised using a VG ToF SIMS (IX23LS) instrument and X-ray photoelectron spectroscopy (XPS). Surprisingly, SIMS and XPS results showed that the DLC samples did not show evidence of titanium since no peaks representing to titanium appeared on the SIMS/XPS spectra.

Inorganic antimicrobial coating for titanium alloy and its effect on bacteria.

PubMed

Tamai, Katsuya; Kawate, Kenji; Kawahara, Ikuo; Takakura, Yoshinori; Sakaki, Kazuhiko

2009-03-01

For orthopedic implants, infection is a serious problem. Therefore, we considered an implant with antimicrobial ability can prevent infection. We tried to coat a titanium alloy surface with Novaron, a commercially available inorganic antimicrobial. The purpose of this study was to analyze the differences among the surfaces of materials coated using different processing pressures of the working gas and analysis of the antimicrobial activity. One of the inorganic antimicrobials Novaron (grade VZ 600) was applied to titanium alloy (Ti6Al4V) plates. This antimicrobial has limited heat resistance, so we used cold spray technology to coat the titanium alloy with it. The principle of cold spray technology is spraying a powder in a high-velocity gas jet, accelerated by adiabatic expansion, against a substrate. Scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS) were used to analyze the differences among the surfaces of materials coated using different processing pressures of the working gas. The Japanese Industrial Standard (JIS) method (JIS Z2801: 2000) was used to analyze the antimicrobial activity against Staphylococcus aureus, Pseudomonas aeruginosa, and Klebsiella pneumoniae. Antimicrobial activity was analyzed only for the sample coated at 3.0 MPa. The SEM and EDS results indicated that when the pressure of the working gas was increased, the antimicrobial coated the titanium adequately. This material showed good effects against S. aureus and P. aeruginosa and some effect for K. pneumoniae. Antimicrobial implants represent a preventive method against infection. There is a possibility of using them not only for clean operations but also for operations with suspected bacterial contamination, such as fixation of slight compound fractures.

Structure and optical properties of TiO2 thin films deposited by ALD method

NASA Astrophysics Data System (ADS)

Szindler, Marek; Szindler, Magdalena M.; Boryło, Paulina; Jung, Tymoteusz

2017-12-01

This paper presents the results of study on titanium dioxide thin films prepared by atomic layer deposition method on a silicon substrate. The changes of surface morphology have been observed in topographic images performed with the atomic force microscope (AFM) and scanning electron microscope (SEM). Obtained roughness parameters have been calculated with XEI Park Systems software. Qualitative studies of chemical composition were also performed using the energy dispersive spectrometer (EDS). The structure of titanium dioxide was investigated by X-ray crystallography. A variety of crystalline TiO2 was also confirmed by using the Raman spectrometer. The optical reflection spectra have been measured with UV-Vis spectrophotometry.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samoylenko, Vitaliy V., E-mail: samoylenko.vitaliy@mail.ru; Lenivtseva, Olga G., E-mail: lenivtseva-olga@mail.ru; Polyakov, Igor A., E-mail: status9@mail.ru

In this paper structural investigations and mechanical tests of Ti-Ta-Zr coatings obtained on surfaces of cp-titanium workpieces were carried out. It was found that the coatings had a dendrite structure; investigations at high-power magnifications revealed a platelet structure. An increase of tantalum concentration led to refinement of structural components. The microhardness level of all coatings, excepting a specimen with the maximum tantalum content, was 370 HV. The microhardness of this coating reached 400 HV. The ultimate tensile strength of cladded layers varied from 697 to 947 MPa. Adhesion tests showed that bimetallic composites were characterized by high bond strength of claddedmore » layers to the substrate, which exceeded cp-titanium strength characteristics.« less

Development of Titanium-Sputtered Anodized Aluminum Substrates for Dye-Sensitized Solar Cells

NASA Astrophysics Data System (ADS)

Côté, Marie-Pier; Parsi Benehkohal, Nima; Alpay, Neslihan; Demopoulos, George P.; Brochu, Mathieu

2014-12-01

In this study, anodized aluminum coupons are sputtered with titanium and successfully demonstrated as dye-sensitized solar cell (DSC) electrode substrates in both anode [back-illumination (BI)] and cathode [front-illumination (FI)] configurations. The FI DSCs were found to be significantly more efficient than the BI devices registering an average efficiency of 5.7 vs 2.6 pct. By comparison, the efficiency of benchmark cells built with fluorine-tin oxide-glass was 6.7 and 4.6 pct, respectively. The thickness of the titanium-sputtered film was varied from 0.85 to 1.1 μm with the latter providing a better average efficiency when used as a counter electrode. According to preliminary stability testing, the Ti-sputtered anodized aluminum-based DSC devices exhibited a significant reduction of their efficiency over a period of 10 days that was partly attributed to triiodide redox electrolyte reaction with the aluminum substrate. This points to the need for optimization of the sputtered-titanium coating microstructure in order to completely isolate the aluminum substrate from the liquid electrolyte.

Biofilm formation on nanostructured titanium oxide surfaces and a micro/nanofabrication-based preventive strategy using colloidal lithography.

PubMed

Singh, Ajay Vikram; Vyas, Varun; Salve, Tushar S; Cortelli, Daniele; Dellasega, David; Podestà, Alessandro; Milani, Paolo; Gade, W N

2012-06-01

The contamination of implant devices as a result of biofilm formation through bacterial infection has instigated major research in this area, particularly to understand the mechanism of bacterial cell/implant surface interactions and their preventions. In this paper, we demonstrate a controlled method of nanostructured titanium oxide surface synthesis using supersonic cluster beam depositions. The nanoscale surface characterization using atomic force microscopy and a profilometer display a regulated evolution in nanomorphology and physical properties. X-ray photoelectron spectroscopy analyses display a stoichiometric nanostructured TiO(2) film. Measurement of the water contact angle shows a nominal increase in the hydrophilic nature of ns-TiO(2) films, whereas the surface energy increases with decreasing contact angle. Bacterial species Staphylococcus aureus and Escherichia coli interaction with nanostructured surfaces shows an increase in adhesion and biofilm formation with increasing nanoscale morphological properties. Conversely, limiting ns-TiO(2) film distribution to micro/nanopatterned designed substrates integrated with bovine serum albumin functionalization leads to a reduction in biofilm formations due to a globally decreased bacterial cell-surface interaction area. The results have potential implications in inhibiting bacterial colonization and promoting mammalian cell-implant interactions.

Tea Polyphenol-Reduced Graphene Oxide Deposition on Titanium Surface Enhances Osteoblast Bioactivity.

PubMed

Liu, Mengting; Hao, Liying; Huang, Qian; Zhao, Dan; Li, Qianshun; Cai, Xiaoxiao

2018-05-01

Graphene, a novel carbon-based material, has been widely used as osteogenic agent for the potential effect on the promotion of osteoblast proliferation. Tea polyphenol-reduced graphene oxide (TPG) is a simple and environmental-friendly raw material to obtain graphene. In this study, TPG was deposited on the Ti substrate to promote the bone regeneration. We prepared a honeycomb-like structure by acid and alkali pretreatment and immobilized the TPG layer (Ti-TPG) on the surface via electrochemical deposition. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD) were used to identify the immobilization of TPG on the titanium (Ti) successfully. Furthermore, the biological response of the Ti-TPG surface to rat osteoblast was evaluated. We also studied the cell adhesion, proliferation and expression of ossification genes on the sample. The results revealed that Ti-TPG had an advantage over Ti alloys in modulating cellular activity and Ti-TPG may be a promising coating for biological materials.

Effect of sandblasting intensity on microstructures and properties of pure titanium micro-arc oxidation coatings in an optimized composite technique

NASA Astrophysics Data System (ADS)

Wang, Hong-Yuan; Zhu, Rui-Fu; Lu, Yu-Peng; Xiao, Gui-Yong; He, Kun; Yuan, Y. F.; Ma, Xiao-Ni; Li, Ying

2014-02-01

Sandblasting is one of the most effective methods to modify a metal surface and improve its properties for application. Micro-arc oxidation (MAO) could produce a ceramic coating on a dental implant, facilitating cellular differentiation and osseocomposite on it. This study aims to deposit bioceramic Ca- and P-containing coatings on sandblasted commercially pure titanium by an optimum composite technique to improve the bioactive performance. The effect of sandblasting intensity on microstructures and properties of the implant coatings is examined, and the modified surfaces are characterized in terms of their topography, phase, chemical composition, mechanical properties and hydroxyapatite (HA)-inducing ability. The results show that a moderate sandblasting micromachines the substrate in favorable combination of rough and residual stresses; its MAO coating deposits nano-hydroxyapatite after immersion in simulated body fluid (SBF) for 5 days exhibiting better bioactivity. The further improvement of the implant surface performance is attributed to an optimized composite technique.

Manufacturing of composite titanium-titanium nitride coatings by reactive very low pressure plasma spraying (R-VLPPS)

NASA Astrophysics Data System (ADS)

Vautherin, B.; Planche, M.-P.; Quet, A.; Bianchi, L.; Montavon, G.

2014-11-01

Very Low Pressure Plasma Spraying (VLPPS) is an emerging spray process nowadays intensively studied by many research centers in the World. To date, studies are mostly focused on the manufacturing of ceramic or metallic coatings. None refers to composite coatings manufacturing by reactive plasma spraying under very low pressure (i.e., ~150 Pa). This paper aims at presenting the carried-out developments and some results concerning the manufacturing of composite coatings by reactive spraying. Titanium was selected as metallic material in order to deposit titanium-nitride titanium coatings (Ti-TiN). Nitrogen was used as plasma gas and was injected along an Ar-H2-N2 plasma jet via a secondary injector in order to reach the nitrogen content on the substrate surface. Thus, different kind of reactive mechanisms were highlighted. Resulting coatings were characterized by Scanning Electron Microscopy (SEM) observations. Porous microstructures are clearly identified and the deposits exhibit condensed vapours and molten particles. Glow Discharge Optical Emission Spectroscopy (GDOES) analysis evidenced nitrogen inside the deposits and X-Ray Diffraction (XRD) analysis confirmed the formation of titanium nitride phases, such as TiN and Ti2N, depending upon the location of the nitrogen injection. Microhardness values as high as 800 VHN were measured on manufactured samples (to be compared to 220 VHN for pure titanium VLPPS-manufactured coatings).

Sputtering characteristics, crystal structures, and transparent conductive properties of TiOxNy films deposited on α-Al2O3(0 0 0 1) and glass substrates

NASA Astrophysics Data System (ADS)

Akazawa, Housei

2012-12-01

Adding N2 gas during reactive sputtering of a Ti target prevented the target surface from being severely poisoned by oxygen atoms and sustained a high deposition rate for titanium oxynitride films under metal-mode-like sputtering conditions. With progress in the degree of oxidization, films deposited onto a glass substrate varied from TiO1-xNx having a face-centered cubic (fcc) structure to TiO2-xNx having an anatase structure. Titanium oxynitride films deposited on an Al2O3(0 0 0 1) substrate were epitaxial with major orientations toward the (1 1 1) and (2 0 0) directions for fcc-TiO1-xNx and (1 1 2) for anatase-TiO2-xNx. Intermediately oxidized films between TiO1-xNx and TiO2-xNx were amorphous on the glass substrate but crystallized into a Magneli phase, TinO(N)2n-1, on the Al2O3(0 0 0 1) substrate. Partially substituting oxygen in TiO2 with nitrogen as well as continuously irradiating the growing film surface with a Xe plasma stream preferentially formed anatase rather than rutile. However, the occupation of anion sites with enough oxygen rather than nitrogen was the required condition for anatase crystals to form. The transparent conductive properties of epitaxial TiO2-xNx films on Al2O3(0 0 0 1) were superior to those of microcrystalline films on the glass substrate. Since resistivity and optical transmittance of TiOxNy films vary continuously with changing N2 flow rate, their transparent conductive properties can be controlled more easily than TiOx. Nb5+ ions could be doped as donors in TiO2-xNx anatase crystals.

Fast plasma sintering delivers functional graded materials components with macroporous structures and osseointegration properties.

PubMed

Godoy, R F; Coathup, M J; Blunn, G W; Alves, A L; Robotti, P; Goodship, A E

2016-04-13

We explored the osseointegration potential of two macroporous titanium surfaces obtained using fast plasma sintering (FPS): Ti macroporous structures with 400-600 µmØ pores (TiMac400) and 850-1000 µmØ pores (TiMac850). They were compared against two surfaces currently in clinical use: Ti-Growth® and air plasma spray (Ti-Y367). Each surface was tested, once placed over a Ti-alloy and once onto a CoCr bulk substrate. Implants were placed in medial femoral condyles in 24 sheep. Samples were explanted at four and eight weeks after surgery. Push-out loads were measured using a material-testing system. Bone contact and ingrowth were assessed by histomorphometry and SEM and EDX analyses. Histology showed early osseointegration for all the surfaces tested. At 8 weeks, TiMac400, TiMac850 and Ti-Growth® showed deep bone ingrowth and extended colonisation with newly formed bone. The mechanical push-out force was equal in all tested surfaces. Plasma spray surfaces showed greater bone-implant contact and higher level of pores colonisation with new bone than FPS produced surfaces. However, the void pore area in FPS specimens was significantly higher, yet the FPS porous surfaces allowed a deeper osseointegration of bone to implant. FPS manufactured specimens showed similar osseointegration potential to the plasma spray surfaces for orthopaedic implants. FPS is a useful technology for manufacturing macroporous titanium surfaces. Furthermore, its capability to combine two implantable materials, using bulk CoCr with macroporous titanium surfaces, could be of interest as it enables designers to conceive and manufacture innovative components. FPS delivers functional graded materials components with macroporous structures optimised for osseointegration.

Effect of the voltage pulse frequency on the structure of TiO2 coatings grown by plasma electrolytic oxidation

NASA Astrophysics Data System (ADS)

Torres-Cerón, D. A.; Gordillo-Delgado, F.; Moya-Betancourt, S. N.

2017-12-01

Plasma Electrolytic Oxidation (PEO) is used to synthetize titanium dioxide (TiO2) ceramic coatings with the appropriate selection of an electrolyte. The dimension of the micro-cavities and the particle size at the surface can be controlled through the pulse frequency of the voltage that is applied between the electrodes. The change of surface morphology can increase the surface area-to-volume ratio. In this work, PEO of an ASME SB-265 titanium substrate (20×20×1mm) was made in a water solution containing 8g/L Na3PO4 and 0.4g/L NaOH. Hence, the coatings were fabricated using voltage pulses of 340V for 10 minutes with a 10% duty cycle and frequencies of 1000, 1500 and 2000Hz. According to the X-ray diffractograms of the obtained samples, the sintering process at 500°C during 1 hour generated Anatase titanium dioxide porous coatings. The grain size decreased approximately from 29nm for 1000 and 1500Hz pulse frequencies until 21nm for 2000Hz. On the other hand, from the micrographs of scanning electron microscopy was possible to see the uniform formation of the micro-cavities with the largest diameter, 900nm, for the lowest frequency value used in PEO.

In vitro assessments on bacterial adhesion and corrosion performance of TiN coating on Ti6Al4V titanium alloy synthesized by multi-arc ion plating

NASA Astrophysics Data System (ADS)

Lin, Naiming; Huang, Xiaobo; Zhang, Xiangyu; Fan, Ailan; Qin, Lin; Tang, Bin

2012-07-01

TiN coating was synthesized on Ti6Al4V titanium alloy surface by multi-arc ion plating (MIP) technique. Surface morphology, cross sectional microstructure, elemental distributions and phase compositions of the obtained coating were analyzed by means of scanning electron microscope (SEM), optical microscope (OM), glow discharge optical emission spectroscope (GDOES) and X-ray diffraction (XRD). Bacterial adhesion and corrosion performance of Ti6Al4V and the TiN coating were assessed via in vitro bacterial adhesion tests and corrosion experiments, respectively. The results indicated that continuous and compact coating which was built up by pure TiN with a typical columnar crystal structure has reached a thickness of 1.5 μm. This TiN coating could significantly reduce the bacterial adhesion and enhance the corrosion resistance of Ti6Al4V substrate.

The effects of a SiO2 coating on the corrosion parameters cpTi and Ti-6Al-7Nb alloy

PubMed Central

Basiaga, Marcin; Walke, Witold; Paszenda, Zbigniew; Karasiński, Paweł; Szewczenko, Janusz

2014-01-01

The aim of this paper was to evaluate the usefulness of the sol-gel method application, to modificate the surface of the Ti6Al7Nb alloy and the cpTi titanium (Grade 4) with SiO2 oxide, applied on the vascular implants to improve their hemocompatibility. Mechanical treatment was followed by film deposition on surface of the titanium samples. An appropriate selection of the process parameters was verified in the studies of corrosion, using potentiodynamic and impedance method. A test was conducted in the solution simulating blood vessels environment, in simulated body fluid at t = 37.0 ± 1 °C and pH = 7.0 ± 0.2. Results showed varied electrochemical properties of the SiO2 film, depending on its deposition parameters. Correlations between corrosion resistance and layer adhesion to the substrate were observed, depending on annealing temperature. PMID:25482412

Palladium-directed self-assembly of multi-titanium(IV)-porphyrin arrays on the substrate surface as sensitive ultrathin films for hydrogen peroxide sensing, photocurrent generation, and photochromism of viologen

NASA Astrophysics Data System (ADS)

He, Wen-Li; Fang, Fang; Ma, Dong-Mei; Chen, Meng; Qian, Dong-Jin; Liu, Minghua

2018-01-01

Multiporphyrin arrays are large, π-conjugated chromophores with high absorption efficiency and strong chemical stability that play an important role in supramolecular and advanced material sciences. Palladium-directed self-assembly of multiporphyrin array ultrathin films was achieved on substrate surfaces using oxo[5,10,15,20-tetra(4-pyridyl)porphyrinato]titanium (IV) complex [TiO(TPyP)] as a linker and sodium tetrachloropalladate (Na2PdCl4) as a connector. The Pd-TiOTPyP films as prepared were characterized by using UV-vis absorption and X-ray photoelectron spectroscopy, as well as by atomic force and scanning electron microscopy. The Soret absorption band of TiOTPyP was observed to red shift by 6 nm when the Pd-TiOTPyP multilayer-modified quartz substrate was immersed in an aqueous solution containing hydrogen peroxide. This was attributed to the formation of a TiO2TPyP monoperoxo complex. This oxidation reaction could be accelerated in an acidic solution. Furthermore, the immobilized Pd-TiOTPyP multilayers could act as light-harvesting units for photocurrent generation and photochromism of viologens, with strong stability, reproducibility, and recyclability. The photocurrent density could be enhanced in electrolyte solutions containing electron donors such as triethanolamine, or electron acceptors such as viologens. Finally, photoinduced reduction (photochromism) of viologens was investigated using the Pd-TiOTPyP multilayers as light sensitizers and EDTA as the electron donors.

Kinetic and microstructural study of titanium nitride deposited by laser chemical vapor deposition

NASA Astrophysics Data System (ADS)

Egland, Keith Maynard

Titanium nitride (TiN) films were deposited onto Ti-6Al-4V substrates by laser chemical vapor deposition using a cw COsb2 laser and TiClsb4,\\ Nsb2, and Hsb2 reactant gases. In-situ laser induced fluorescence (LIF) and multi-wavelength pyrometry determined relative titanium gas phase atomic number density and deposition temperature, respectively. Deposited films were yellow to gold in color. Transmission electron microscopy on one sample revealed a face-centered cubic structure with a lattice parameter (0.4237 nm) expected for TiN. Auger electron spectroscopy found substoichiometric compositions with a N/Ti ratio between 0.7 and 0.9. Variables decreasing grain size (lower temperature, higher TiClsb4 input) decreased the N/Ti ratio. Higher Nsb2 input increased stoichiometry, while larger Hsb2 input decreased stoichiometry. The deposit substoichiometry is believed to be caused by diffusion of nitrogen through TiN grain boundaries to the titanium alloy substrate. The morphology starts as a dense polycrystalline structure evolving into a columnar structure having facets or nodules at the surface with crystallite sizes ranging from 10-1000 nm. TiClsb4 input had a inverse correlation with crystallite size, while Nsb2:Hsb2 ratio had minimal effect; the crystallite size (G) varied exponentially with temperature (T) for a given irradiation time, i.e., G = C exp (-28000/T), with constant C reflecting substrate roughness and gas composition. Microhardness tests revealed substrate contributions; nevertheless, films appeared to have a minimum hardness of 2000 Hsbv. The deposition apparent activation energy was calculated as 122 ± 9 kJ/mole using growth rates measured by film height and 117 ± 23 kJ/mole using growth rates measured by LIF signals. This puts the process in the surface kinetic growth regime over the temperature range 1370-1610 K. Above Nsb2 and Hsb2 levels of 1.25% and below TiClsb4 input of 4.5%, the growth rate has a half-order dependence on nitrogen and a linear dependence on hydrogen and is approximated by$r = {{kPsb{TiClsb4}Psb{Hsb2}Psbsp{Nsb2}{1/2}exp≤ft({{-}Esb{a}/ {RT}right)}/{1 + Psb{Ar}}}}.Since nitrogen positively affects growth rate (when added to a TiClsb4+Hsb2 mixture), stepwise reduction of TiClsb4 to Ti by hydrogen does not occur. NHsb{x} complexes are clearly involved in the growth mechanism; a likely combination of rate determining steps is the formation of NH and the initial reduction of TiClsb4$ by hydrogen.

Titanium dioxide nanotubes functionalized with Cratylia mollis seed lectin, Cramoll, enhanced osteoblast-like cells adhesion and proliferation.

PubMed

Oliveira, Weslley F; Silva, Germana M M; Cabral Filho, Paulo E; Fontes, Adriana; Oliveira, Maria D L; Andrade, César A S; Silva, Márcia V; Coelho, Luana C B B; Machado, Giovanna; Correia, Maria T S

2018-09-01

An alternative to accelerate the osseointegration on titanium dioxide nanotubes (TNTs) used in osseointegrated implants is through the functionalization of these nanostructured surfaces with biomolecules. In this work, we immobilized a lectin with recognized mitogenic activity, the Cramoll lectin, extracted from Cratylia mollis seeds, on surfaces modified by TNTs. For the immobilization of Cramoll on TNTs surfaces, we used the Layer-by-Layer technique (LbL) by growing five alternate layers of poly(allylamine) hydrochloride (PAH) and poly(acrylic) acid (PAA); lastly we incubated the lectin, at different concentrations, with the TNTs-LbL. Before and after the immobilization procedures, the substrate surfaces were characterized by scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), and, electrochemical impedance spectroscopy (EIS). We also evaluated the Cramoll activity after immobilization on TNTs by using the lectin interaction with ovalbumin. The lectin did not lose its biological activity, even after immobilization onto nanotubular arrays. In addition, we observed an increase osteoblast-like cell adhesion on the TNTs-LbL-Cramoll system when compared to the bare TNTs surfaces. Moreover, a significative cell proliferation was identified on the substrates when Cramoll was immobilized at concentrations of 80, 160 and 320 μg/mL after 48 h of incubation by using the resazurin assay. Our results suggest that Cramoll was efficiently immobilized on a nanotubular array and this new platform presents a great potential to be tested in implantology. Copyright © 2018 Elsevier B.V. All rights reserved.

Osseointegration improvement by plasma electrolytic oxidation of modified titanium alloys surfaces.

PubMed

Echeverry-Rendón, Mónica; Galvis, Oscar; Quintero Giraldo, David; Pavón, Juan; López-Lacomba, José Luis; Jiménez-Piqué, Emilio; Anglada, Marc; Robledo, Sara M; Castaño, Juan G; Echeverría, Félix

2015-02-01

Titanium (Ti) is a material frequently used in orthopedic applications, due to its good mechanical properties and high corrosion resistance. However, formation of a non-adherent fibrous tissue between material and bone drastically could affect the osseointegration process and, therefore, the mechanical stability of the implant. Modifications of topography and configuration of the tissue/material interface is one of the mechanisms to improve that process by manipulating parameters such as morphology and roughness. There are different techniques that can be used to modify the titanium surface; plasma electrolytic oxidation (PEO) is one of those alternatives, which consists of obtaining porous anodic coatings by controlling parameters such as voltage, current, anodizing solution and time of the reaction. From all of the above factors, and based on previous studies that demonstrated that bone cells sense substrates features to grow new tissue, in this work commercially pure Ti (c.p Ti) and Ti6Al4V alloy samples were modified at their surface by PEO in different anodizing solutions composed of H2SO4 and H3PO4 mixtures. Treated surfaces were characterized and used as platforms to grow osteoblasts; subsequently, cell behavior parameters like adhesion, proliferation and differentiation were also studied. Although the results showed no significant differences in proliferation, differentiation and cell biological activity, overall results showed an important influence of topography of the modified surfaces compared with polished untreated surfaces. Finally, this study offers an alternative protocol to modify surfaces of Ti and their alloys in a controlled and reproducible way in which biocompatibility of the material is not compromised and osseointegration would be improved.

The shear strength of three-dimensional capillary-porous titanium coatings for intraosseous implants.

PubMed

Kalita, V I; Komlev, D I; Komlev, V S; Radyuk, A A

2016-03-01

A plasma spraying process for the deposition of three-dimensional capillary-porous titanium coatings using a wire has been developed. In this process, two additional dc arcs are discharged between plasmatron and both the wire and the substrate, resulting in additional activation of the substrate and the particles, particularly by increasing their temperature. The shear strength of the titanium coating with 46% porosity is 120.6 MPa. A new procedure for estimating the shear strength of porous coatings has been developed. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of Extreme Wettability on Platelet Adhesion on Metallic Implants: From Superhydrophilicity to Superhydrophobicity.

PubMed

Moradi, Sona; Hadjesfandiari, Narges; Toosi, Salma Fallah; Kizhakkedathu, Jayachandran N; Hatzikiriakos, Savvas G

2016-07-13

In order to design antithrombotic implants, the effect of extreme wettability (superhydrophilicity to superhydrophobicity) on the biocompatibility of the metallic substrates (stainless steel and titanium) was investigated. The wettability of the surface was altered by chemical treatments and laser ablation methods. The chemical treatments generated different functionality groups and chemical composition as evident from XPS analysis. The micro/nanopatterning by laser ablation resulted in three different pattern geometry and different surface roughness and consequently wettability. The patterned surface were further modified with chemical treatments to generate a wide range of surface wettability. The influence of chemical functional groups, pattern geometry, and surface wettability on protein adsorption and platelet adhesion was studied. On chemically treated flat surfaces, the type of hydrophilic treatment was shown to be a contributing factor that determines the platelet adhesion, since the hydrophilic oxidized substrates exhibit less platelet adhesion in comparison to the control untreated or acid treated surfaces. Also, the surface morphology, surface roughness, and superhydrophobic character of the surfaces are contributing factors to platelet adhesion on the surface. Our results show that superhydrophobic cauliflower-like patterns are highly resistant to platelet adhesion possibly due to the stability of Cassie-Baxter state for this pattern compared to others. Our results also show that simple surface treatments on metals offer a novel way to improve the hemocompatibility of metallic substrates.

Functionalization of Ti99.2 substrates surface by hybrid treatment investigated with spectroscopic methods

NASA Astrophysics Data System (ADS)

Jasinski, Jaroslaw Jan; Lubas, Malgorzata; Kurpaska, Lukasz; Napadlek, Wojciech; Sitarz, Maciej

2018-07-01

The article presents spectroscopic investigation of Ti 99.2 based functional substrates formed by hybrid oxidation process. Surface treatments were performed by combining methods of fluidized bed atmospheric diffusion treatment (FADT) with physical vapor deposition (PVD) - magnetron sputtering and laser surface texturing (LST) treatments. The processes were implemented to form a titanium diffusive layer saturated with oxygen in the substrate and a tight homogeneous oxide coating on Ti surface deposited with magnetron sputtering or laser texturing technique. The hybrid treatment was realized in Al2O3 fluidized bed reactor with air atmosphere, at 640 °C for 8 h and 12 h. At the same time, magnetron sputtering with the use of TiO2 target at a pressure of 3 × 102 mbar and laser surface texturing treatment with Nd:YAG λ = 1064 nm was performed. In order to investigate the effects of hybrid oxidation, microscopic (AFM, CLSM, SEM/SEM-EDX), spectroscopic (RS) and X-ray investigations (GID-XRD) were performed. Applied hybrid technique made possible to combine the effects of the generated layers and to reduce the stresses in the area of the PVD coating/oxidized Ti substrate interface. Furthermore, Raman spectroscopy results obtained at oxide layers manufactured with different variants of oxidation allowed detailed analysis of the created oxides. The coatings have shown structure with a Tiα(O) diffusion zone, a TiO2 rutile and anatase oxide zone deposited and textured on the substrate. Phase composition and morphology of these oxides is essential for the osseointegration process i.e. intensity of hydroxyapatite growing on the implant surface. Performed processes influenced the surface roughness parameter and cause the increase of substrate functional properties, which are important for biomedical applications.

Application of diffusion barriers to the refractory fibers of tungsten, columbium, carbon and aluminum oxide

NASA Technical Reports Server (NTRS)

Douglas, F. C.; Paradis, E. L.; Veltri, R. D.

1973-01-01

A radio frequency powered ion-plating system was used to plate protective layers of refractory oxides and carbide onto high strength fiber substrates. Subsequent overplating of these combinations with nickel and titanium was made to determine the effectiveness of such barrier layers in preventing diffusion of the overcoat metal into the fibers with consequent loss of fiber strength. Four substrates, five coatings, and two metal matrix materials were employed for a total of forty material combinations. The substrates were tungsten, niobium, NASA-Hough carbon, and Tyco sapphire. The diffusion-barrier coatings were aluminum oxide, yttrium oxide, titanium carbide, tungsten carbide with 14% cobalt addition, and zirconium carbide. The metal matrix materials were IN 600 nickel and Ti 6/4 titanium. Adhesion of the coatings to all substrates was good except for the NASA-Hough carbon, where flaking off of the oxide coatings in particular was observed.

Laser Surface Microstructuring of Biocompatible Materials Using a Microlens Array and the Talbot Effect: Evaluation of the Cell Adhesion.

PubMed

Aymerich, María; Nieto, Daniel; Álvarez, Ezequiel; Flores-Arias, María T

2017-02-22

A laser based technique for microstructuring titanium and tantalum substrates using the Talbot effect and an array of microlenses is presented. By using this hybrid technique; we are able to generate different patterns and geometries on the top surfaces of the biomaterials. The Talbot effect allows us to rapidly make microstructuring, solving the common problems of using microlenses for multipatterning; where the material expelled during the ablation of biomaterials damages the microlens. The Talbot effect permits us to increase the working distance and reduce the period of the patterns. We also demonstrate that the geometries and patterns act as anchor points for cells; affecting the cell adhesion to the metallic substrates and guiding how they spread over the material.

Laser Surface Microstructuring of Biocompatible Materials Using a Microlens Array and the Talbot Effect: Evaluation of the Cell Adhesion

PubMed Central

Aymerich, María; Nieto, Daniel; Álvarez, Ezequiel; Flores-Arias, María T.

2017-01-01

A laser based technique for microstructuring titanium and tantalum substrates using the Talbot effect and an array of microlenses is presented. By using this hybrid technique; we are able to generate different patterns and geometries on the top surfaces of the biomaterials. The Talbot effect allows us to rapidly make microstructuring, solving the common problems of using microlenses for multipatterning; where the material expelled during the ablation of biomaterials damages the microlens. The Talbot effect permits us to increase the working distance and reduce the period of the patterns. We also demonstrate that the geometries and patterns act as anchor points for cells; affecting the cell adhesion to the metallic substrates and guiding how they spread over the material. PMID:28772574

The effect of Al intermediate layer on thermal resistance of EB-PVD yttria-stabilized zirconia coatings on titanium substrate

NASA Astrophysics Data System (ADS)

Panin, Alexey; Panin, Victor; Kazachenok, Marina; Shugurov, Artur; Sinyakova, Elena; Martynov, Sergey; Rusyaev, Andrey; Kasterov, Artur

2017-12-01

The yttria-stabilized zirconia coatings sprayed on titanium substrates by the electron beam physical vapor deposition were subjected to thermal annealing in air at 1000°C for 1, 30 and 60 min. The delamination and fracture of the coatings are studied by the scanning electron microscopy and X-ray diffraction. It is shown that a magnetron sputtered Al interlayer between the coating and the substrate considerably improves the thermal resistance of ceramic coatings.

Ceramic substrate including thin film multilayer surface conductor

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wolf, Joseph Ambrose; Peterson, Kenneth A.

2017-05-09

A ceramic substrate comprises a plurality of ceramic sheets, a plurality of inner conductive layers, a plurality of vias, and an upper conductive layer. The ceramic sheets are stacked one on top of another and include a top ceramic sheet. The inner conductive layers include electrically conductive material that forms electrically conductive features on an upper surface of each ceramic sheet excluding the top ceramic sheet. The vias are formed in each of the ceramic sheets with each via being filled with electrically conductive material. The upper conductive layer includes electrically conductive material that forms electrically conductive features on anmore » upper surface of the top ceramic sheet. The upper conductive layer is constructed from a stack of four sublayers. A first sublayer is formed from titanium. A second sublayer is formed from copper. A third sublayer is formed from platinum. A fourth sublayer is formed from gold.« less

Electrochemical depositing rGO-Ti-rGO heterogeneous substrates with higher thermal conductivity and heat transfer performance compared to pure Ti.

PubMed

Wang, Jing; Wang, Huatao; Zhang, Wenying; Yang, Xinyi; Wen, Guangwu; Wang, Yijie; Zhou, Weiwei

2017-02-17

Titanium (Ti) and its alloys are widely applied in many high strength, light weight applications, but their thermal conductivity is lower compared to that of other metals, which limits their further applications. In this paper, we demonstrated experimentally that rGO-Ti-rGO heterogeneous substrates with higher thermal conductivity, up to ∼38.8% higher than Ti, could be fabricated by electrochemical depositing rGO on their surface. The rGO layers are grown on the surface of Ti substrates, with appearance of bedclothes on the beds. The thickness of rGO layers is around 300-500 nm and around 600-1000 nm when deposited for 5 cycles and 10 cycles, respectively. According to the cooling experiment results, as-prepared Ti + rGO substrates can present excellent thermal conduction performance, and reduce the chip temperature close to 3.2 °C-13.1 °C lower than Ti alloy substrates with the heat flow density of 0.4-3.6 W cm -2 . Finally, the approach to electro-chemically deposit hundreds of nanometer rGO layers on the surface of Ti substrates can improve their thermal conductivity and heat transfer performance, which may have further application in the increasing thermal conduction of other metal-alloys, ceramics and polymers.

Cell Attachment Following Instrumentation with Titanium and Plastic Instruments, Diode Laser, and Titanium Brush on Titanium, Titanium-Zirconium, and Zirconia Surfaces.

PubMed

Lang, Melissa S; Cerutis, D Roselyn; Miyamoto, Takanari; Nunn, Martha E

2016-01-01

The aim of this study was to evaluate the surface characteristics and gingival fibroblast adhesion of disks composed of implant and abutment materials following brief and repeated instrumentation with instruments commonly used in procedures for implant maintenance, stage-two implant surgery, and periimplantitis treatment. One hundred twenty disks (40 titanium, 40 titaniumzirconium, 40 zirconia) were grouped into treatment categories of instrumentation by plastic curette, titanium curette, diode microlaser, rotary titanium brush, and no treatment. Twenty strokes were applied to half of the disks in the plastic and titanium curette treatment categories, while half of the disks received 100 strokes each to simulate implant maintenance occurring on a repetitive basis. Following analysis of the disks by optical laser profilometry, disks were cultured with human gingival fibroblasts. Cell counts were conducted from scanning electron microscopy (SEM) images. Differences in surface roughness across all instruments tested for zirconia disks were negligible, while both titanium disks and titaniumzirconium disks showed large differences in surface roughness across the spectrum of instruments tested. The rotary titanium brush and the titanium curette yielded the greatest overall mean surface roughness, while the plastic curette yielded the lowest mean surface roughness. The greatest mean cell counts for each disk type were as follows: titanium disks with plastic curettes, titanium-zirconium disks with titanium curettes, and zirconia disks with the diode microlaser. Repeated instrumentation did not result in cumulative changes in surface roughness of implant materials made of titanium, titanium-zirconium, or zirconia. Instrumentation with plastic implant curettes on titanium and zirconia surfaces appeared to be more favorable than titanium implant curettes in terms of gingival fibroblast attachment on these surfaces.

Toward optimizing dental implant performance: Surface characterization of Ti and TiZr implant materials.

PubMed

Murphy, M; Walczak, M S; Thomas, A G; Silikas, N; Berner, S; Lindsay, R

2017-01-01

Targeting understanding enhanced osseointegration kinetics, the goal of this study was to characterize the surface morphology and composition of Ti and TiZr dental implant substrates subjected to one of two surface treatments developed by Straumann. These two treatments are typically known as SLA and SLActive, with the latter resulting in more rapid osseointegration. A range of techniques was applied to characterize four different substrate/surface treatment combinations (Ti SLA , Ti SLActive , TiZr SLA , and TiZr SLActive ). Contact angle measurements established their hydrophilic/hydrophobic nature. Surface morphology was probed with scanning electron microscopy. X-ray diffraction, Raman μ-spectroscopy, and X-ray photoelectron spectroscopy were used to elucidate the composition of the near-surface region. Consistent with previous work, surface morphology was found to differ only at the nanoscale, with both SLActive substrates displaying nano-protrusions. Spectroscopic data indicate that all substrates exhibit surface films of titanium oxide displaying near TiO 2 stoichiometry. Raman μ-spectroscopy reveals that amorphous TiO 2 is most likely the only phase present on Ti SL A , whilst rutile-TiO 2 is also evidenced on Ti SLActive , TiZr SLA , and TiZr SLActive . For TiZr alloy substrates, there is no evidence of discrete phases of oxidized Zr. X-ray photoelectron spectra demonstrate that all samples are terminated by adventitious carbon, with it being somewhat thicker (∼1nm) on Ti SL A and TiZr SLA . Given previous in vivo studies, acquired data suggest that both nanoscale protrusions, and a thinner layer of adventitious carbon contribute to the more rapid osseointegration of SLActive dental implants. Composition of the surface oxide layer is apparently less important in determining osseointegration kinetics. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The influence of titanium adhesion layer oxygen stoichiometry on thermal boundary conductance at gold contacts

NASA Astrophysics Data System (ADS)

Olson, David H.; Freedy, Keren M.; McDonnell, Stephen J.; Hopkins, Patrick E.

2018-04-01

We experimentally demonstrate the role of oxygen stoichiometry on the thermal boundary conductance across Au/TiOx/substrate interfaces. By evaporating two different sets of Au/TiOx/substrate samples under both high vacuum and ultrahigh vacuum conditions, we vary the oxygen composition in the TiOx layer from 0 ≤ x ≤ 2.85. We measure the thermal boundary conductance across the Au/TiOx/substrate interfaces with time-domain thermoreflectance and characterize the interfacial chemistry with x-ray photoemission spectroscopy. Under high vacuum conditions, we speculate that the environment provides a sufficient flux of oxidizing species to the sample surface such that one essentially co-deposits Ti and these oxidizing species. We show that slower deposition rates correspond to a higher oxygen content in the TiOx layer, which results in a lower thermal boundary conductance across the Au/TiOx/substrate interfacial region. Under the ultrahigh vacuum evaporation conditions, pure metallic Ti is deposited on the substrate surface. In the case of quartz substrates, the metallic Ti reacts with the substrate and getters oxygen, leading to a TiOx layer. Our results suggest that Ti layers with relatively low oxygen compositions are best suited to maximize the thermal boundary conductance.

Scale-Up of a Titanium Carbonitride Coating System for Titanium Alloys.

DTIC Science & Technology

1980-07-01

Ti-Cote C on JT12 Compressor 7th-Stage Airfoil -Optical Photomicrograph Porosity in Ti-Cote C Titanium 6AI- 4V Substrate - -- Mag: 1000OX FD 171506...30 21 TiCN Coating on Titanium 6A1- 4V ...indication of any corrosive damage to the titanium 6A1- 4V . This had been a matter of concern due to the corrosive nature of the reactive gases and

Design and Manufacture of a Highly Reliable, Miniaturized and Low Mass Shutter Mechanism

NASA Technical Reports Server (NTRS)

Manhart, M.; Zeh, T.; Preibler, G.; Hurni, A.; Walter, I.; Helbert, J.; Hiesinger, H.

2010-01-01

This paper describes the development, manufacturing and testing of a lightweight shutter mechanism made of titanium for the MERTIS Instrument. MERTIS is a thermal infrared imaging spectrometer onboard ESA's future BepiColombo mission to Mercury. The mechanism is built as a parallelogram arrangement of flexible hinges, actuated by a voice coil. In a first test run, it was shown that the selected EDM processing led to the generation of titanium oxides and an oxygen-enriched surface layer on the substrate (so called alpha-case layer). In the revised version of the shutter, it was possible to manufacture the complex geometry by micro-milling and an adjacent pickling procedure. The adequacy of this approach was verified by lifetime and vibration testing.

Structure and mechanical properties of coatings fabricated by nonvacuum electron beam cladding of Ti-Ta-Zr powder mixtures

NASA Astrophysics Data System (ADS)

Samoylenko, Vitaliy V.; Lenivtseva, Olga G.; Polyakov, Igor A.; Laptev, Ilya S.

2015-10-01

In this paper structural investigations and mechanical tests of Ti-Ta-Zr coatings obtained on surfaces of cp-titanium workpieces were carried out. It was found that the coatings had a dendrite structure; investigations at high-power magnifications revealed a platelet structure. An increase of tantalum concentration led to refinement of structural components. The microhardness level of all coatings, excepting a specimen with the maximum tantalum content, was 370 HV. The microhardness of this coating reached 400 HV. The ultimate tensile strength of cladded layers varied from 697 to 947 MPa. Adhesion tests showed that bimetallic composites were characterized by high bond strength of cladded layers to the substrate, which exceeded cp-titanium strength characteristics.

Hydrogenated amorphous silicon coatings may modulate gingival cell response

NASA Astrophysics Data System (ADS)

Mussano, F.; Genova, T.; Laurenti, M.; Munaron, L.; Pirri, C. F.; Rivolo, P.; Carossa, S.; Mandracci, P.

2018-04-01

Silicon-based materials present a high potential for dental implant applications, since silicon has been proven necessary for the correct bone formation in animals and humans. Notably, the addition of silicon is effective to enhance the bioactivity of hydroxyapatite and other biomaterials. The present work aims to expand the knowledge of the role exerted by hydrogen in the biological interaction of silicon-based materials, comparing two hydrogenated amorphous silicon coatings, with different hydrogen content, as means to enhance soft tissue cell adhesion. To accomplish this task, the films were produced by plasma enhanced chemical vapor deposition (PECVD) on titanium substrates and their surface composition and hydrogen content were analyzed by means of X-ray photoelectron spectroscopy (XPS) and Fourier-transform infrared spectrophotometry (FTIR) respectively. The surface energy and roughness were measured through optical contact angle analysis (OCA) and high-resolution mechanical profilometry respectively. Coated surfaces showed a slightly lower roughness, compared to bare titanium samples, regardless of the hydrogen content. The early cell responses of human keratinocytes and fibroblasts were tested on the above mentioned surface modifications, in terms of cell adhesion, viability and morphometrical assessment. Films with lower hydrogen content were endowed with a surface energy comparable to the titanium surfaces. Films with higher hydrogen incorporation displayed a lower surface oxidation and a considerably lower surface energy, compared to the less hydrogenated samples. As regards mean cell area and focal adhesion density, both a-Si coatings influenced fibroblasts, but had no significant effects on keratinocytes. On the contrary, hydrogen-rich films increased manifolds the adhesion and viability of keratinocytes, but not of fibroblasts, suggesting a selective biological effect on these cells.

Structure-related antibacterial activity of a titanium nanostructured surface fabricated by glancing angle sputter deposition

NASA Astrophysics Data System (ADS)

Sengstock, Christina; Lopian, Michael; Motemani, Yahya; Borgmann, Anna; Khare, Chinmay; Buenconsejo, Pio John S.; Schildhauer, Thomas A.; Ludwig, Alfred; Köller, Manfred

2014-05-01

The aim of this study was to reproduce the physico-mechanical antibacterial effect of the nanocolumnar cicada wing surface for metallic biomaterials by fabrication of titanium (Ti) nanocolumnar surfaces using glancing angle sputter deposition (GLAD). Nanocolumnar Ti thin films were fabricated by GLAD on silicon substrates. S. aureus as well as E. coli were incubated with nanostructured or reference dense Ti thin film test samples for one or three hours at 37 °C. Bacterial adherence, morphology, and viability were analyzed by fluorescence staining and scanning electron microscopy and compared to human mesenchymal stem cells (hMSCs). Bacterial adherence was not significantly different after short (1 h) incubation on the dense or the nanostructured Ti surface. In contrast to S. aureus the viability of E. coli was significantly decreased after 3 h on the nanostructured film compared to the dense film and was accompanied by an irregular morphology and a cell wall deformation. Cell adherence, spreading and viability of hMSCs were not altered on the nanostructured surface. The results show that the selective antibacterial effect of the cicada wing could be transferred to a nanostructured metallic biomaterial by mimicking the natural nanocolumnar topography.

Optical and hydrophobic properties of co-sputtered chromium and titanium oxynitride films

NASA Astrophysics Data System (ADS)

Rawal, Sushant K.; Chawla, Amit Kumar; Jayaganthan, R.; Chandra, Ramesh

2011-08-01

The chromium and titanium oxynitride films on glass substrate were deposited by using reactive RF magnetron sputtering in the present work. The structural and optical properties of the chromium and titanium oxynitride films as a function of power variations are investigated. The chromium oxynitride films are crystalline even at low power of Cr target (≥60 W) but the titanium oxynitride films are amorphous at low target power of Ti target (≤90 W) as observed from glancing incidence X-ray diffraction (GIXRD) patterns. The residual stress and strain of the chromium oxynitride films are calculated by sin 2 ψ method, as the average crystallite size decreases with the increase in sputtering power of the Cr target, higher stress and strain values are observed. The chromium oxynitride films changes from hydrophilic to hydrophobic with the increase of contact angle value from 86.4° to 94.1°, but the deposited titanium oxynitride films are hydrophilic as observed from contact angle measurements. The changes in surface energy were calculated using contact angle measurements to substantiate the hydrophobic properties of the films. UV-vis and NIR spectrophotometer were used to obtain the transmission and absorption spectra, and the later was used for determining band gap values of the films, respectively. The refractive index of chromium and titanium oxynitride films increases with film packing density due to formation of crystalline chromium and titanium oxynitride films with the gradual rise in deposition rate as a result of increase in target powers.

Preparation of Superhydrophobic Film on Ti Substrate and Its Anticorrosion Property

PubMed Central

Zhu, Min; Tang, Wenchuan; Huang, Luyao; Zhang, Dawei; Du, Cuiwei; Yu, Gaohong; Chen, Ming; Chowwanonthapunya, Thee

2017-01-01

Superhydrophobic films were fabricated on a titanium substrate with or without anodizing by using a self-assembling method. Firstly, the pretreatments of mechanical polishing/anodizing or mechanical polishing only were conducted, respectively. Subsequently, the preparation of polydopamine film layer, deposition of nano-silver particles, and post modification of 1H,1H,2H,2H-perfluorodecanethiol were performed on the surface of the pretreated substrate. The surface morphologies, compositions, wettability, and corrosion resistance of the films were investigated with scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS), water contact angle measurements, and electrochemical tests, respectively. Meanwhile, the effect of the deposition time in the silver nitrate solution on the hydrophobicity of the specimen surface was investigated. The result showed that with the increase of deposition time, the hydrophobic property enhanced gradually. The surface deposited for 7 h exhibited an optimum hydrophobic effect, which was characterized with a large water contact angle (WCA) of 154°, and the surface was rather rough and covered by a relatively uniform layer of micro-nano silver particles. The excellent hydrophobicity was attributed to a rough stratified microstructure along with the low surface energy. The electrochemical measurements showed that the existence of the superhydrophobic film can effectively enhance the corrosion resistance of Ti samples. PMID:28772987

Preparation of Superhydrophobic Film on Ti Substrate and Its Anticorrosion Property.

PubMed

Zhu, Min; Tang, Wenchuan; Huang, Luyao; Zhang, Dawei; Du, Cuiwei; Yu, Gaohong; Chen, Ming; Chowwanonthapunya, Thee

2017-06-08

Superhydrophobic films were fabricated on a titanium substrate with or without anodizing by using a self-assembling method. Firstly, the pretreatments of mechanical polishing/anodizing or mechanical polishing only were conducted, respectively. Subsequently, the preparation of polydopamine film layer, deposition of nano-silver particles, and post modification of 1H,1H,2H,2H-perfluorodecanethiol were performed on the surface of the pretreated substrate. The surface morphologies, compositions, wettability, and corrosion resistance of the films were investigated with scanning electron microscopy (SEM), energy-dispersive spectrometry (EDS), water contact angle measurements, and electrochemical tests, respectively. Meanwhile, the effect of the deposition time in the silver nitrate solution on the hydrophobicity of the specimen surface was investigated. The result showed that with the increase of deposition time, the hydrophobic property enhanced gradually. The surface deposited for 7 h exhibited an optimum hydrophobic effect, which was characterized with a large water contact angle (WCA) of 154°, and the surface was rather rough and covered by a relatively uniform layer of micro-nano silver particles. The excellent hydrophobicity was attributed to a rough stratified microstructure along with the low surface energy. The electrochemical measurements showed that the existence of the superhydrophobic film can effectively enhance the corrosion resistance of Ti samples.

Hybrid Calcium Phosphate Coatings for Titanium Implants

NASA Astrophysics Data System (ADS)

Kharapudchenko, E.; Ignatov, V.; Ivanov, V.; Tverdokhlebov, S.

2017-01-01

Hybrid multilayer coatings were obtained on titanium substrates by the combination of two methods: the micro-arc oxidation in phosphoric acid solution with the addition of calcium compounds to high supersaturated state and RF magnetron sputtering of the target made of synthetic hydroxyapatite. 16 different groups of coatings were formed on titanium substrates and in vitro studies were conducted in accordance with ISO 23317 in the solution simulating body fluid. The studies using SEM, XRD of the coatings of the samples before and after exposure to SBF were performed. The features of morphology, chemical and phase composition of the studied coatings are shown.

Antimicrobial design of titanium surface that kill sessile bacteria but support stem cells adhesion

NASA Astrophysics Data System (ADS)

Zhu, Chen; Bao, Ni-Rong; Chen, Shuo; Zhao, Jian-Ning

2016-12-01

Implant-related bacterial infection is one of the most severe postoperative complications in orthopedic or dental surgery. In this context, from the perspective of surface modification, increasing efforts have been made to enhance the antibacterial capability of titanium surface. In this work, a hierarchical hybrid surface architecture was firstly constructed on titanium surface by two-step strategy of acid etching and H2O2 aging. Then silver nanoparticles were firmly immobilized on the hierarchical surface by ion implantation, showing no detectable release of silver ions from surface. The designed titanium surface showed good bioactivity. More importantly, this elaborately designed titanium surface can effectively inactivate the adherent S. aureus on surface by virtue of a contact-killing mode. Meanwhile, the designed titanium surface can significantly facilitate the initial adhesion and spreading behaviors of bone marrow mesenchymal stem cells (MSCs) on titanium. The results suggested that, the elaborately designed titanium surface might own a cell-favoring ability that can help mammalian cells win the initial adhesion race against bacteria. We hope the present study can provide a new insight for the better understanding and designing of antimicrobial titanium surface, and pave the way to satisfying clinical requirements.

Shear strength of a three-dimensional capillary-porous titanium coating for biomedical applications

NASA Astrophysics Data System (ADS)

Kalita, V. I.; Komlev, D. I.; Radyuk, A. A.; Ivannikov, A. Yu; Alpatov, A. V.; Komlev, V. S.; Mamonov, V. I.; Sevostyanov, M. A.; Baikin, A. S.

2018-04-01

The effect of pretreatment and plasma preheating of Ti-substrate on shear strength of three-dimensional capillary porous Ti-coating was studied. After sandblasting the shear strength of the plasma sprayed coating was 200 ± 2 MPa, and after additional matting it was 68 ± 4 MPa. The use of plasma preheating of the substrates for 9 seconds decreased difference between values of the shear strength to 249 ± 17 MPa and 229 ± 16 MPa, respectively. After plasma spraying the microhardness of the surface layer of the substrate was 4.34 ± 0.35 GPa, the microhardness of the boundary between the coating and the substrate was 8.08 ± 0.45 GPa, and the microhardness of the coating was 3.48 ± 0.25 GPa. High shear strength of the coating was attributed to the activation of the substrate by means of plasma preheating and hardening of the boundary between the coating and the substrate by oxides and nitrides.

Characterization of PEG-Like Macromolecular Coatings on Plasma Modified NiTi Alloy

NASA Astrophysics Data System (ADS)

Yang, Jun; Gao, Jiacheng; Chang, Peng; Wang, Jianhua

2008-04-01

A poly (ethylene glycol) (PEG-like) coating was developed to improve the biocompatibility of Nickel-Titanium (NiTi) alloy implants. The PEG-like macromolecular coatings were deposited on NiTi substrates at a room temperature of 298 K through a ECR (electron-cyclotron resonance) cold-plasma enhanced chemical vapor deposition method using tetraglyme (CH3-O-(CH2-CH2-O)4-CH3) as a precursor. A power supply with a frequency of 2.45 GHz was applied to ignite the plasma with Ar(argon) used as the carrier gas. Based on the atomic force microscopy (AFM) studies, a thin smooth coating on NiTi substrates with highly amorphous functional groups on the modified NiTi surfaces were mainly the same accumulated stoichiometric ratio of C and O with PEG. The vitro studies showed that platelet-rich plasma (PRP) adsorption on the modified NiTi alloy surface was significantly reduced. This study indicated that plasma surface modification changes the surface components of NiTi alloy and subsequently improves its biocompatibility.

Robust self-cleaning surfaces that function when exposed to either air or oil

NASA Astrophysics Data System (ADS)

Lu, Yao; Sathasivam, Sanjayan; Song, Jinlong; Crick, Colin R.; Carmalt, Claire J.; Parkin, Ivan P.

2015-03-01

Superhydrophobic self-cleaning surfaces are based on the surface micro/nanomorphologies; however, such surfaces are mechanically weak and stop functioning when exposed to oil. We have created an ethanolic suspension of perfluorosilane-coated titanium dioxide nanoparticles that forms a paint that can be sprayed, dipped, or extruded onto both hard and soft materials to create a self-cleaning surface that functions even upon emersion in oil. Commercial adhesives were used to bond the paint to various substrates and promote robustness. These surfaces maintained their water repellency after finger-wipe, knife-scratch, and even 40 abrasion cycles with sandpaper. The formulations developed can be used on clothes, paper, glass, and steel for a myriad of self-cleaning applications.

Tensile properties of titanium electrolytically charged with hydrogen

NASA Technical Reports Server (NTRS)

Smith, R. J.; Otterson, D. A.

1971-01-01

Yield strength, ultimate tensile strength, and elongation were studied for annealed titanium electrolytically charged with hydrogen. The hydrogen was present as a surface hydride layer. These tensile properties were generally lower for uncharged titanium than for titanium with a continuous surface hydride; they were greater for uncharged titanium than for titanium with an assumed discontinuous surface hydride. We suggest that the interface between titanium and titanium hydride is weak. And the hydride does not necessarily impair strength and ductility of annealed titanium. The possibility that oxygen and/or nitrogen can embrittle titanium hydride is discussed.

[The surface roughness analysis of the titanium casting founding by a new titanium casting investment material].

PubMed

Liang, Qin-ye; Wu, Xia-yi; Lin, Xue-feng

2012-04-01

To investigate the surface roughness property of the titanium castings cast in a new investment for titanium casting. Six wax patterns (20 mm × 20 mm × 0.5 mm) were invested using two investments: three in a new titanium investment material and three in the control material (Rematitan Plus). Six titanium specimens were obtained by conventional casting. After casting, surface roughness of the specimens were evaluated with a surface profilometer. The surface roughness of the specimens cast in new titanium investment material was (1.72 ± 0.08) µm, which was much smaller than that from Rematitan Plus [(1.91 ± 0.15) µm, P < 0.05]. The surfaces of titanium cast using these two investment materials are both smooth enough to fulfill the demand of the titanium precision-casting for prosthodontic clinical use.

Laser Cladding of γ-TiAl Intermetallic Alloy on Titanium Alloy Substrates

NASA Astrophysics Data System (ADS)

Maliutina, Iuliia Nikolaevna; Si-Mohand, Hocine; Piolet, Romain; Missemer, Florent; Popelyukh, Albert Igorevich; Belousova, Natalya Sergeevna; Bertrand, Philippe

2016-01-01

The enhancement of titanium and titanium alloy's tribological properties is of major interest in many applications such as the aerospace and automotive industry. Therefore, the current research paper investigates the laser cladding of Ti48Al2Cr2Nb powder onto Ti6242 titanium alloy substrates. The work was carried out in two steps. First, the optimal deposition parameters were defined using the so-called "combined parameters," i.e., the specific energy E specific and powder density G. Thus, the results show that those combined parameters have a significant influence on the geometry, microstructure, and microhardness of titanium aluminide-formed tracks. Then, the formation of dense, homogeneous, and defect-free coatings based on optimal parameters has been investigated. Optical and scanning electron microscopy techniques as well as energy-dispersive spectroscopy and X-ray diffraction analyses have shown that a duplex structure consisting of γ-TiAl and α 2-Ti3Al phases was obtained in the coatings during laser cladding. Moreover, it was shown that produced coatings exhibit higher values of microhardness (477 ± 9 Hv0.3) and wear resistance (average friction coefficient is 0.31 and volume of worn material is 5 mm3 after 400 m) compared to those obtained with bare titanium alloy substrates (353 Hv0.3, average friction coefficient is 0.57 and a volume of worn material after 400 m is 35 mm3).

Nanoporous array anodic titanium-supported co-polymeric ionic liquids as high performance solid-phase microextraction sorbents for hydrogen bonding compounds.

PubMed

Jia, Jing; Liang, Xiaojing; Wang, Licheng; Guo, Yong; Liu, Xia; Jiang, Shengxiang

2013-12-13

A nanoporous array anodic titanium-supported co-polymeric ionic liquids (NAAT/PILs) solid-phase microextraction (SPME) fiber was prepared in situ on the titanium wire. NAAT was selected as the substrate, in view of its high surface-to-volume ratio, easy preparation, mechanical stability, and rich titanol groups on its surface which can anchor silica coupling agent containing vinyl and then introduce ionic liquid copolymers as sorbents. In this work, 1-vinyl-3-nonanol imidazolium bromide ([C9OHVIm]Br) and 1,4-di(3-vinylimidazolium) butane dibromide ([(VIM)2C4]2[Br]) were synthesized and used as monomer and crosslinker, respectively. Extraction properties of the NAAT/PILs fiber for polar alcohols and volatile fatty acids (VFAs) in aqueous matrix were examined using gaseous sampling-SPME (GS-SPME) and headspace SPME (HS-SPME) mode, respectively. Combining the superior properties of NAAT substrate and the strong hydrogen bond interaction of PILs to polar compounds, the NAAT/PILs SPME fiber showed much higher adsorption affinity to aliphatic alcohols than bare NAAT and pure PILs fibers. The detection limits (LOD) of established GS-SPME-GC-FID method are in the range of 0.35-17.30ngL(-1) with a linear range from 0.01 to 500ngmL(-1). Also, it showed high extraction performance toward volatile fatty acids (VFAs) compounds from aqueous matrix. Under the optimized SPME conditions, wide linear ranges were obtained with correlation coefficients (R(2)) greater than 0.99 and limits of detection were in the range of 0.85-8.74ngL(-1). Moreover, real-world samples were analyzed and good results were obtained. Copyright © 2013. Published by Elsevier B.V.

Sprayable titanium composition

DOEpatents

Tracy, Chester E.; Kern, Werner; Vibronek, Robert D.

1980-01-01

The addition of 2-ethyl-1-hexanol to an organometallic titanium compound dissolved in a diluent and optionally containing a lower aliphatic alcohol spreading modifier, produces a solution that can be sprayed onto a substrate and cured to form an antireflection titanium oxide coating having a refractive index of from about 2.0 to 2.2.

Laser surface modification of Ti and TiC coatings on magnesium alloy

NASA Astrophysics Data System (ADS)

Kim, J. M.; Lee, S. G.; Park, J. S.; Kim, H. G.

2014-12-01

In order to enhance the surface properties of magnesium alloy, a highly intense laser surface melting process following plasma spraying of Ti or TiC on AZ31 alloy were employed. When laser surface melting was applied to Ti coated magnesium alloy, the formation of fine Ti particle dispersed surface layer on the substrate occurred. The corrosion potential of the AZ31 alloy with Ti dispersed surface was significantly increased in 3.5 wt % NaCl solution. Additionally, an improved hardness was observed for the laser treated specimens as compared to the untreated AZ31 alloy. Laser melting process following plasma thermal deposition was also applied for obtaining in situ TiC coating layer on AZ31 alloy. The TiC coating layer could be successfully formed via in situ reaction between pure titanium and carbon powders. Incomplete TiC formation was observed in the plasma sprayed specimen, while completely transformed TiC layer was found after post laser melting process. It was also confirmed that the laser post treatment induced enhanced adhesion strength between the coating and the substrate.

Preparation and bioactive properties of nanocrystalline hydroxyapatite thin films obtained by conversion of atomic layer deposited calcium carbonate.

PubMed

Holopainen, Jani; Kauppinen, Kyösti; Mizohata, Kenichiro; Santala, Eero; Mikkola, Esa; Heikkilä, Mikko; Kokkonen, Hanna; Leskelä, Markku; Lehenkari, Petri; Tuukkanen, Juha; Ritala, Mikko

2014-09-01

Nanocrystalline hydroxyapatite thin films were fabricated on silicon and titanium by atomic layer deposition (ALD) of CaCO3 and its subsequent conversion to hydroxyapatite by diammonium hydrogen phosphate (DAP) solution. The effects of conversion process parameters to crystallinity and morphology of the films were examined. DAP concentration was found to be critical in controlling the crystal size and homogeneity of the films. The hydroxyapatite phase was identified by XRD. ToF-elastic recoil detection analysis studies revealed that the films are calcium deficient in relation to hydroxyapatite with a Ca/P ratio of 1.39 for films converted with 0.2 M DAP at 95 °C. The coatings prepared on titanium conformally follow the rough surface topography of the substrate, verifying that the good step coverage of the ALD method was maintained in the conversion process. The dissolution tests revealed that the coating was nondissolvable in the cell culture medium. Annealing the coated sample at 700 °C for 1 h seemed to enhance its bonding properties to the substrate. Also, the biocompatibility of the coatings was confirmed by human bone marrow derived cells in vitro. The developed method provides a new possibility to produce thin film coatings on titanium implants with bone-type hydroxyapatite that is biocompatible with human osteoblasts and osteoclasts.

Optical and morphological properties of sol gel derived titanium dioxide films

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, A. B.; Sharma, S. K.; M, Vishwas

2015-08-28

Titanium oxide (Titania) thin films were synthesized on different substrates via the sol-gel dip-coating method using alkoxide solution. Some selected samples were also prepared with different percentage of Lead (Pb). The influence of Pb addition in precursor sol on the optical properties of titanium dioxide thin films was studied. The optical transmittance in the visible region has increased with increase in weight percentage of lead. The refractive index was slightly decreased with Pb addition. Crystallization of these coatings was achieved through thermal annealing at temperatures above 400 °C. The structural properties and surface morphology of the crystallized coatings were studiedmore » by Scanning Electron Microscopy. Increase in average grain size from 250 nm to 350 nm with increase in Pb concentration is observed. Films were appeared to more coarse with increase in Pb addition. An increase in Pb addition resulted increase in average roughness from 12 nm to 25 nm.« less

Regulation of osteogenesis by micro/nano hierarchical titanium surfaces through a Rock-Wnt5a feedback loop.

PubMed

Yu, Yonglin; Shen, Xinkun; Liu, Junjie; Hu, Yan; Ran, Qichun; Mu, Caiyun; Cai, Kaiyong

2018-05-28

Titanium substrates with micro/nano hierarchical features could positively mediate the osteogenesis of a titanium implant; nevertheless, the underlying molecular mechanism needs to be further revealed. In this work, we fabricated a micro/nano hierarchically structured Ti (MNT) sample and attempted to evaluate its topography-mediated biological effects and potential molecular mechanisms in vitro. The results proved that MNT could not only affect cell morphology and osteogenic differentiation, but also regulate ROCK activity cell biological functions of osteoblasts involved in ROCK activation, β-catenin accumulation, and high-Wnt5a expression in respect to topographical features. Moreover, blockade of ROCK activation resulted in significant inhibition of cell differentiation and Wnt5a expression. Furthermore, the anti-Wnt5a significantly down-regulated ROCK activity. In short, these results indicate the important role of ROCK-Wnt5a feedback loop in regulating cell differentiation by topographies. Copyright © 2018. Published by Elsevier B.V.

Surface modification of TiO2 nanotubes with osteogenic growth peptide to enhance osteoblast differentiation.

PubMed

Lai, Min; Jin, Ziyang; Su, Zhiguo

2017-04-01

To investigate the influence of surface-biofunctionalized substrates on osteoblast behavior, a layer of aligned TiO 2 nanotubes with a diameter of around 70nm was fabricated on titanium surface by anodization, and then osteogenic growth peptide (OGP) was conjugated onto TiO 2 nanotubes through the intermediate layer of polydopamine. The morphology, composition and wettability of different surfaces were characterized by field-emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and contact angle measurements, respectively. The effects of OGP-modified TiO 2 nanotube substrates on the morphology, proliferation and differentiation of osteoblasts were examined in vitro. Immunofluorescence staining revealed that the OGP-functionalized TiO 2 nanotubes were favorable for cell spreading. However, there was no significant difference in cell proliferation observed among the different groups. Cells grown onto OGP-functionalized TiO 2 nanotubes showed significantly higher (p<0.05 or p<0.01) levels of alkaline phosphatase (ALP) and mineralization after 4, 7 and 14days of culture, respectively. Cells grown on OGP-functionalized TiO 2 nanotubes had significantly higher (p<0.05 or p<0.01) expression of osteogenic-related genes including runt related transcription factor 2 (Runx2), ALP, collagen type I (Col I), osteopontin (OPN) and osteocalcin (OC) after 14days of culture. These data suggest that surface functionalization of TiO 2 nanotubes with OGP was beneficial for cell spreading and differentiation. This study provides a novel platform for the development and fabrication of titanium-based implants that enhance the propensity for osseointegration between the native tissue and implant interface. Copyright © 2016 Elsevier B.V. All rights reserved.

Method for Surface Texturing Titanium Products

NASA Technical Reports Server (NTRS)

Banks, Bruce A. (Inventor)

1998-01-01

The present invention teaches a method of producing a textured surface upon an arbitrarily configured titanium or titanium alloy object for the purpose of improving bonding between the object and other materials such as polymer matrix composites and/or human bone for the direct in-growth of orthopaedic implants. The titanium or titanium alloy object is placed in an electrolytic cell having an ultrasonically agitated solution of sodium chloride therein whereby a pattern of uniform "pock mark" like pores or cavities are produced upon the object's surface. The process is very cost effective compared to other methods of producing rough surfaces on titanium and titanium alloy components. The surface textures produced by the present invention are etched directly into the parent metal at discrete sites separated by areas unaffected by the etching process. Bonding materials to such surface textures on titanium or titanium alloy can thus support a shear load even if adhesion of the bonding material is poor.

Microstructured Titanium Regulates Interleukin Production by Osteoblasts, an Effect Modulated by Exogenous BMP-2

PubMed Central

Hyzy, Sharon; Olivares-Navarrete, Rene; Hutton, Daphne L.; Tan, Christian; Boyan, Barbara D.; Schwartz, Zvi

2013-01-01

Microtextured implant surfaces increase osteoblast differentiation in vitro and enhance bone-to-implant contact in vivo and clinically. These implants may be used in combination with recombinant human bone morphogenetic protein 2 (rhBMP-2) to enhance peri-implant bone formation. However, the effect of surface modifications alone or in combination with rhBMP-2 on osteoblast-produced inflammatory microenvironment is unknown. MG63 cells were cultured on tissue culture polystyrene or titanium substrates: smooth pretreated (PT, Ra=0.2μm), sandblasted/acid-etched (SLA, Ra=3.2μm), or hydrophilic-SLA (modSLA). Expression and protein production of pro-inflammatory interleukins (IL1b, IL6, IL8, IL17) and anti-inflammatory interleukins (IL10) were measured in cells with or without rhBMP-2. To determine which BMP signaling pathways were involved, cultures were incubated with BMP pathway inhibitors to blocking Smad (dorsomorphin), TAB/TAK1 ((5Z)-7-oxozeaenol), or PKA (H-8) signaling. Culture on rough SLA and modSLA surfaces decreased pro-inflammatory interleukins and increased anti-inflammatory IL10. This effect was negated in cells treated with rhBMP-2, which caused an increase in pro-inflammatory interleukins and a decrease in anti-inflammatory interleukins through TAB/TAK signaling. The results suggest that surface microtexture modulates the inflammatory process during osseointegration, an effect that may enhance healing. However, rhBMP-2 in combination with microtextured titanium implants can influence the effect of cells on these surfaces, and may adversely affect cells involved in osseointegration. PMID:23123301

Comparison of different substrates for laser-induced electron transfer desorption/ionization of metal complexes

NASA Astrophysics Data System (ADS)

Grechnikov, A. A.; Georgieva, V. B.; Donkov, N.; Borodkov, A. S.; Pento, A. V.; Raicheva, Z. G.; Yordanov, Tc A.

2016-03-01

Four different substrates, namely, graphite, tungsten, amorphous silicon (α-Si) and titanium dioxide (TiO2) films, were compared in view of the laser-induced electron transfer desorption/ionization (LETDI) of metal coordination complexes. A rhenium complex with 8-mercaptoquinoline, a copper complex with diphenylthiocarbazone and chlorophyll A were studied as the test analytes. The dependencies of the ion yield and the surface temperature on the incident radiation fluence were investigated experimentally and theoretically. The temperature was estimated using the numerical solution of a one-dimensional heat conduction problem with a heat source distributed in time and space. It was found that at the same temperature, the ion yield from the different substrates varies in the range of three orders of magnitude. The direct comparison of all studied substrates revealed that LETDI from the TiO2 and α-Si films offer a better choice for producing molecular ions of metal coordination complexes.

Thermally Oxidized C, N Co-Doped ANATASE-TiO2 Coatings on Stainless Steel for Tribological Properties

NASA Astrophysics Data System (ADS)

Wang, Hefeng; Shu, Xuefeng; Li, Xiuyan; Tang, Bin; Lin, Naiming

2013-07-01

Ti(C, N) coatings were prepared on stainless steel (SS) substrates by plasma surface alloying technique. Carbon-nitrogen co-doped titanium dioxide (C-N-TiO2) coatings were fabricated by oxidative of the Ti(C, N) coatings in air. The prepared C-N-TiO2 coatings were characterized by SEM, XPS and XRD. Results reveal that the SS substrates were entirely shielded by the C-N-TiO2 coatings. The C-N-TiO2 coatings are anatase in structure as characterized by X-ray diffraction. The tribological behavior of the coatings was tested with ball-on-disc sliding wear and compared with substrate. Such a C-N-TiO2 coatings showed good adhesion with the substrate and tribological properties of the SS in terms of much reduced friction coefficient and increased wear resistance.

[The bonding characteristic of titanium and RG experiment porcelain].

PubMed

Ren, Wei-hong; Guo, Tian-wen; Tian, Jie-mo; Zhang, Yun-long

2003-07-01

To study the bonding characteristic of Titanium and RG experiment porcelain. 5 specimens with a size of 10 mm x 5 mm x 1.4 mm were cast from pure titanium. Then 1 mm of RG experiment opaque and body porcelain were fused on the surface of the titanium specimens. The interface of titanium and porcelain was analyzed with a scanning electron microscope with energy-despersive spectrometry; 6 metal specimens with the size of 25 mm x 3 mm x 0.5 mm were cast from Ni-Cr alloy and a uniform thickness of 1 mm of VMK 99 porcelain was veneered on the central area of 8 mm x 3 mm 18 metal specimens as the same size were cast from pure titanium. The uniform thickness of 1 mm of VITA TITANKERAMIK porcelain, of Noritake super porcelain Ti-22 and of RG experiment porcelain were veneered on every 6 specimens respectively in the central area of 8 mm x 3 mm. The specimens were subjected to a three-point bending test on a load-test machine with a span of 20 mm, then the failure loads were recorded and statistically analysised. The RG porcelain/titanium crown was fabricated by fusing RG opaque porcelain and body porcelain to cast titanium substrate crown. The SEM results show no porosity and crackle were found in the interface. The energy-dispersive spectrometry show that there are Si, Ti and O in the 1 micro m layer between porcelain and titanium, which suggesting titanium and experiment porcelain bonding well. The three point test showed the fracture force for the combinations of titanium/VITA TITANKERAMIK porcelain, titanium/Noritake super porcelain Ti-22 and titanium/RG experiment porcelain were (7.233 +/- 2.539) N, (5.533 +/- 1.199) N and (6.316 +/- 1.433) N respectively. There were not statistically significant differences among them (t test, P < 0.01). The fracture force for the Ni-Cr alloy/VMK99 porcelain combination (12.733 +/- 3.297) N was significantly greater than those of the cast titanium/porcelain (t test, P > 0.05). The crown was translucent with no crack. RG porcelain is well compatible with titanium.

21 CFR 888.3358 - Hip joint metal/polymer/metal semi-constrained porous-coated uncemented prosthesis.

Code of Federal Regulations, 2012 CFR

2012-04-01

... substrates, beads of the same alloy, and in the case of Ti-6Al-4V substrates, fibers of commercially pure titanium or Ti-6Al-4V alloy. The porous coating has a volume porosity between 30 and 70 percent, an average... titanium-aluminum-vanadium (Ti-6Al-4V) alloy and an acetabular component composed of an ultra-high...

21 CFR 888.3358 - Hip joint metal/polymer/metal semi-constrained porous-coated uncemented prosthesis.

Code of Federal Regulations, 2011 CFR

2011-04-01

... substrates, beads of the same alloy, and in the case of Ti-6Al-4V substrates, fibers of commercially pure titanium or Ti-6Al-4V alloy. The porous coating has a volume porosity between 30 and 70 percent, an average... titanium-aluminum-vanadium (Ti-6Al-4V) alloy and an acetabular component composed of an ultra-high...

21 CFR 888.3358 - Hip joint metal/polymer/metal semi-constrained porous-coated uncemented prosthesis.

Code of Federal Regulations, 2014 CFR

2014-04-01

... substrates, beads of the same alloy, and in the case of Ti-6Al-4V substrates, fibers of commercially pure titanium or Ti-6Al-4V alloy. The porous coating has a volume porosity between 30 and 70 percent, an average... titanium-aluminum-vanadium (Ti-6Al-4V) alloy and an acetabular component composed of an ultra-high...

21 CFR 888.3358 - Hip joint metal/polymer/metal semi-constrained porous-coated uncemented prosthesis.

Code of Federal Regulations, 2013 CFR

2013-04-01

... substrates, beads of the same alloy, and in the case of Ti-6Al-4V substrates, fibers of commercially pure titanium or Ti-6Al-4V alloy. The porous coating has a volume porosity between 30 and 70 percent, an average... titanium-aluminum-vanadium (Ti-6Al-4V) alloy and an acetabular component composed of an ultra-high...

Thermo-mechanical modeling of laser treatment on titanium cold-spray coatings

NASA Astrophysics Data System (ADS)

Paradiso, V.; Rubino, F.; Tucci, F.; Astarita, A.; Carlone, P.

2018-05-01

Titanium coatings are very attractive to several industrial fields, especially aeronautics, due to the enhanced corrosion resistance and wear properties as well as improved compatibility with carbon fiber reinforced plastic (CFRP) materials. Cold sprayed titanium coatings, among the others deposition processes, are finding a widespread use in high performance applications, whereas post-deposition treatments are often used to modify the microstructure of the cold-sprayed layer. Laser treatments allow one to noticeably increase the superficial properties of titanium coatings when the process parameters are properly set. On the other hand, the high heat input required to melt titanium particles may result in excessive temperature increase even in the substrate. This paper introduces a thermo-mechanical model to simulate the laser treatment effects on a cold sprayed titanium coating as well as the aluminium substrate. The proposed thermo-mechanical finite element model considers the transient temperature field due to the laser source and applied boundary conditions using them as input loads for the subsequent stress-strain analysis. Numerical outcomes highlighted the relevance of thermal gradients and thermally induced stresses and strains in promoting the damage of the coating.

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, Raghu N.; Ginley, David S.

1995-01-01

A process for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications.

Preparation of lead-zirconium-titanium film and powder by electrodeposition

DOEpatents

Bhattacharya, R.N.; Ginley, D.S.

1995-10-31

A process is disclosed for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications. 4 figs.

Ceramic surfaces, interfaces and solid-state reactions

NASA Astrophysics Data System (ADS)

Heffelfinger, Jason Roy

Faceting, the decomposition of a surface into two or more surfaces of different orientation, is studied as a function of annealing time for ceramic surfaces. Single-crystals of Alsb2Osb3\\ (alpha-Alsb2Osb3 or corundum structure) are carefully prepared and characterized by atomic force microscopy, scanning electron microscopy and transmission electron microscopy. The mechanisms by which the originally smooth vicinal surface transforms into either a hill-and-valley or a terrace-and-step structure have been characterized. The progression of faceting is found to have a series of stages: surface smoothing, nucleation and growth of individual facets, formation of facet domains, coalescence of individual and facet domains and facet coarsening. These stages provide a model for the mechanisms of how other ceramic surfaces may facet into hill-and-valley and terrace-and-step surface microstructures. The well characterized Alsb2Osb3 surfaces provide excellent substrates by which to study the effect of surface structure on thin-film growth. Pulsed-laser deposition was used to grow thin films of yttria stabilized zirconia (YSZ) and Ysb2Osb3 onto annealed Alsb2Osb3 substrates. The substrate surface structure, such as surface steps and terraces, was found to have several effects on thin-film growth. Thin-films grown onto single-crystal substrates serve as a model geometry for studying thin-film solid-state reactions. Here, the reaction sequence and orientation relationship between thin films of Ysb2Osb3 and an Alsb2Osb3 substrate were characterized for different reaction temperatures. In a system were multiple reaction phases can form, the yttria aluminum monoclinic phase (YAM) was found to form prior to formation of other phases in this system. In a second system, a titanium alloy was reacted with single crystal Alsb2Osb3 in order to study phase formation in an intermetallic system. Both Tisb3Al and TiAl were found to form as reaction products and their orientation relationships with the Alsb2Osb3 are discussed.

Electrically conductive, black thermal control coatings for space craft application. II - Silicone matrix formulation

NASA Technical Reports Server (NTRS)

Hribar, V. F.; Bauer, J. L.; O'Donnell, T. P.

1986-01-01

Five black electrically conductive thermal-control coatings have been formulated and tested for application on the Galileo spacecraft. The coatings consisted of organic and inorganic systems applied on titanium and aluminum surfaces. The coatings were tested under simulated space environment conditions. Coated specimens were subjected to thermal radiation and convective and conductive heating from -196 to 538 C. Mechanical, physical, thermal, electrical, and optical characteristics, formulation, mixing, application, surface preparation of substrates, and a method of determining electrical resistance are presented for the silicone matrix formulation designated as GF-580.

Combinatorial growth of oxide nanoscaffolds and its influence in osteoblast cell adhesion

NASA Astrophysics Data System (ADS)

Acevedo-Morantes, Claudia Y.; Irizarry-Ortiz, Roberto A.; Caceres-Valencia, Pablo G.; Singh, Surinder P.; Ramirez-Vick, Jaime E.

2012-05-01

We report a novel method for high-throughput investigations on cell-material interactions based on metal oxide nanoscaffolds. These scaffolds possess a continuous gradient of various titanium alloys allowing the compositional and morphological variation that could substantially improve the formation of an osseointegrative interface with bone. The model nanoscaffold has been fabricated on commercially pure titanium (cp-Ti) substrate with a compositional gradients of tin (Sn), chromium (Cr), and niobium (Nb) deposited using a combinatorial approach followed by annealing to create native oxide surface. As an invitro test system, the human fetal osteoblastic cell line (hFOB 1.19) has been used. Cell-adhesion of hFOB 1.19 cells and the suitability of these alloys have been evaluated for cell-morphology, cell-number, and protein adsorption. Although, cell-morphology was not affected by surface composition, cell-proliferation rates varied significantly with surface metal oxide composition; with the Sn- and Nb-rich regions showing the highest proliferation rate and the Cr-rich regions presenting the lowest. The results suggest that Sn and Nb rich regions on surface seems to promote hFOB 1.19 cell proliferation and may therefore be considered as implant material candidates that deserve further analysis.

Vacuum arc plasma deposition of thin titanium dioxide films on silicone elastomer as a functional coating for medical applications.

PubMed

Boudot, Cécile; Kühn, Marvin; Kühn-Kauffeldt, Marina; Schein, Jochen

2017-05-01

Silicone elastomer is a promising material for medical applications and is widely used for implants with blood and tissue contact. However, its strong hydrophobicity limits adhesion of tissue cells to silicone surfaces, which can impair the healing process. To improve the biological properties of silicone, a triggerless pulsed vacuum cathodic arc plasma deposition technique was applied to deposit titanium dioxide (TiO 2 ) films onto the surface. Scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, Raman spectroscopy and contact angle measurements were used for coating characterization. Deposited films were about 150nm thick and exhibited good adhesion to the underlying silicone substrate. Surface wettability and roughness both increased after deposition of the TiO 2 layer. In addition, cell-biological investigations demonstrated that the in-vitro cytocompatibility of TiO 2 -coated samples was greatly improved without impacting silicone's nontoxicity. For validation of use in medical devices, further investigations were conducted and demonstrated stability of surface properties in an aqueous environment for a period of 68days and the coating's resistance to several sterilization methods. Copyright © 2016 Elsevier B.V. All rights reserved.

Coating stainless steel plates with Ag/TiO2 for chlorpyrifos decontamination

NASA Astrophysics Data System (ADS)

Abdel Fattah, Wafa I.; Gobara, Mohammed M.; El-Hotaby, Walid; Mostafa, Sherif F. M.; Ali, Ghareib W.

2016-05-01

Spray coatings of either nanosilver (Ag), titanium (TiO2) or nanosilver titanium (Ag/TiO2) on stainless steel substrates prepared by sol-gel process were successfully achieved. The efficiency of the Ag/TiO2 coat onto 316 stainless steel surface towards cloropyrifos degradation as a chemical warfare agent (CWA) was proved. The crystalline structure and morphological characterization, as well as surface roughness measurements, were assessed. X-ray diffraction results proved the crystalline TiO2 anatase phase. The uniform distribution of Ag along with TiO2 nanoparticles was evidenced through transmission electron microscopy and scanning electron microscopy mapping. The hydrophilic nature of individual Ag, TiO2 and Ag/TiO2 coats was proved by contact angle measurements. The loading of Ag nanoparticles influenced positively the Ag/TiO2 coats surface roughness. The photocatalytic cloropyrifos degradation achieved about 50% within one-hour post UV treatment proving, therefore, the promising Ag/TiO2 continued decontamination efficiency. In conclusion, tuning the physical and morphological properties of TiO2 coated on stainless steel surface could be significantly enhanced by Ag nanoparticles incorporation. The developed Ag/TiO2 coat could be conveniently applied as CWA decontaminant.

Wettability modification of porous PET by atmospheric femtosecond PLD

NASA Astrophysics Data System (ADS)

Assaf, Youssef; Forstmann, Guillaume; Kietzig, Anne-Marie

2018-04-01

In this study, porous structures were created on poly(ethylene terephthalate) (PET) by femtosecond (fs) laser micromachining. While such structures offer a texture that is desirable for several applications, their wettability does not always match the application in question. The aim of this investigation is to tune the wettability of such surfaces by incorporating a controlled amount of nanoparticles into the structure. The machined PET samples were thus used as substrates for fs pulsed laser deposition (PLD) of titanium under ambient conditions. The nanoparticles were deposited as nanochain clusters due to the formation of an oxide layer between individual nanoparticles. The stability of nanoparticle incorporation was tested by placing the samples in an ultrasonic ethanol bath. Results indicated that nanoparticles were still successfully incorporated into the microstructure after sonication. Nanoparticle surface coverage was observed to be controllable through the operating fluence. The dynamic contact angles of the resulting composite surface were observed to decrease with increasing titanium incorporation. Therefore, this work highlights atmospheric fs PLD as a method for wettability modification of high surface area microstructures without undermining their topology. In addition, this technique uses almost the same equipment as the machining process by which the microstructures are initially created, further highlighting its practicality.

Structural changes of anodic layer on titanium in sulfate solution as a function of anodization duration in constant current mode

NASA Astrophysics Data System (ADS)

Komiya, Shinji; Sakamoto, Kouta; Ohtsu, Naofumi

2014-03-01

The present study investigated the effect of anodization time, in constant current mode, on the anodic oxide layer formed on titanium (Ti). Anodization of the Ti substrate was　carried out in a 0.1 M (NH4)2SO4 aqueous solution with reaction times of various durations, after which the characteristics and photocatalytic activity were investigated in detail. The TiO2 layer fabricated in a short duration exhibited comparatively flat surface morphology and an anatase-type crystal structure. This layer acted as a photocatalyst only under ultraviolet light (UV) illumination. Upon prolonging the anodization, the layer structure changed drastically. The surface morphology became rough, and the crystal structure changed to rutile-type TiO2. Furthermore, the layer showed photocatalytic activity both under UV and visible light illumination. Further anodization increased the amount of methylene blue (MB) adsorbed on the surface, but did not cause additional change to the structure of the anodic layer. The surface morphology and crystal structure of the anodic layer were predominantly controlled by the anodization time; thus, the anodization time is an important parameter for controlling the characteristics of the anodic layer.

Titanium nitride films for micro-supercapacitors: Effect of surface chemistry and film morphology on the capacitance

NASA Astrophysics Data System (ADS)

Achour, Amine; Porto, Raul Lucio; Soussou, Mohamed-Akram; Islam, Mohammad; Boujtita, Mohammed; Aissa, Kaltouma Ait; Le Brizoual, Laurent; Djouadi, Abdou; Brousse, Thierry

2015-12-01

Electrochemical capacitors (EC) in the form of packed films can be integrated in various electronic devices as power source. A fabrication process of EC electrodes, which is compatible with micro-fabrication, should be addressed for practical applications. Here, we show that titanium nitride films with controlled porosity can be deposited on flat silicon substrates by reactive DC-sputtering for use as high performance micro-supercapacitor electrodes. A superior volumetric capacitance as high as 146.4 F cm-3, with an outstanding cycling stability over 20,000 cycles, was measured in mild neutral electrolyte of potassium sulfate. The specific capacitance of the films as well as their capacitance retentions were found to depend on thickness, porosity and surface chemistry of electrodes. The one step process used to fabricate these TiN electrodes and the wide use of this material in the field of semiconductor technology make it promising for miniaturized energy storage systems.

Electrodeposited silk coatings for bone implants.

PubMed

Elia, Roberto; Michelson, Courtney D; Perera, Austin L; Brunner, Teresa F; Harsono, Masly; Leisk, Gray G; Kugel, Gerard; Kaplan, David L

2015-11-01

The aim of this study was to characterize the mechanical properties and drug elution features of silk protein-based electrodeposited dental implant coatings. Silk processing conditions were modified to obtain coatings with a range of mechanical properties on titanium studs. These coatings were assessed for adhesive strength and dissolution, with properties tuned using water vapor annealing or glycerol incorporation to modulate crystalline content. Coating reproducibility was demonstrated over a range of silk concentrations from 1% to 10%. Surface roughness of titanium substrates was altered using industry relevant acid etching and grit blasting, and the effect of surface topography on silk coating adhesion was assessed. Florescent compounds were incorporated into the silk coatings, which were modulated for crystalline content, to achieve four days of sustained release of the compounds. This silk electrogelation technique offers a safe and relatively simple approach to generate mechanically robust, biocompatible, and degradable implant coatings that can also be functionalized with bioactive compounds to modulate the local regenerative tissue environment. © 2014 Wiley Periodicals, Inc.

Electrodeposited silk coatings for bone implants

PubMed Central

Elia, Roberto; Michelson, Courtney D.; Perera, Austin L.; Brunner, Teresa F.; Harsono, Masly; Leisk, Gray G.; Kugel, Gerard; Kaplan, David L.

2014-01-01

The aim of this study was to characterize the mechanical properties and drug elution features of silk protein-based electrodeposited dental implant coatings. Silk processing conditions were modified to obtain coatings with a range of mechanical properties on titanium studs. These coatings were assessed for adhesive strength and dissolution, with properties tuned using water vapor annealing or glycerol incorporation to modulate crystalline content. Coating reproducibility was demonstrated over a range of silk concentrations from 1 to 10%. Surface roughness of titanium substrates was altered using industry relevant acid etching and grit blasting, and the effect of surface topography on silk coating adhesion was assessed. Florescent compounds were incorporated into the silk coatings, which were modulated for crystalline content, to achieve four days of sustained release of the compounds. This silk electrogelation technique offers a safe and relatively simple approach to generate mechanically robust, biocompatible and degradable implant coatings that can also be functionalized with bioactive compounds to modulate the local regenerative tissue environment. PMID:25545462

Bioactivity evaluation of titanium/hydroxyapatite composite coating on stainless steel prepared by thermal spraying

NASA Astrophysics Data System (ADS)

Azhar, Nurul Humaira; Talari, Mahesh Kumar; Koong, Chue Keen

2015-08-01

In this study, titanium powder mixed with different wt % of HA was coated on stainless steel (SS) substrate using high velocity oxy-fuel (HVOF) technique to produce composite coating for biomedical applications. As the addition of HA is expected to influence the bioactivity of the coatings, these coatings were investigated for bioactivity by immersing the samples in a simulated body fluid (SBF) solution for 14 days. The apatite growth rate was evaluated by measuring Ca and P concentration in the SBF using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). The concentrations of Ca and P have decreased over time in the SBF, suggesting a bone like apatite precipitation on the sample surface. It was observed that pH value increased with the increase of immersion time during initial three days and a subsequent drop after 7 days. Microstructure analysis done using FESEM technique showed nucleation and growth of bone-like apatite on the surface of the coating.

Titanium Surface Roughing Treatments contribute to Higher Interaction with Salivary Proteins MG2 and Lactoferrin.

PubMed

Cavalcanti, Yuri Wanderley; Soare, Rodrigo Villamarim; Leite Assis, Marina Araújo; Zenóbio, Elton Gonçalves; Girundi, Francisco Mauro da Silva

2015-02-01

Some surface treatments performed on titanium can alter the composition of salivary pellicle formed on this abiotic surface. Such treatments modify the titanium's surface properties and can promote higher adsorption of proteins, which allow better integration of titanium to the biotic system. This study aimed to evaluate the interactions between salivary proteins and titanium disks with different surface treatments. Machined titanium disks (n = 48) were divided into four experimental groups (n = 12), according to their surface treatments: surface polishing (SP); acid etching (A); spot-blasting plus acid etching (SB-A); spot-blasting followed by acid etching and nano-functionalization (SB-A-NF). Titanium surfaces were characterized by surface roughness and scanning electron microscopy (SEM). Specimens were incubated with human saliva extracted from submandibular and sublingual glands. Total salivary protein adsorbed to titanium was quantified and samples were submitted to western blotting for mucin glycoprotein 2 (MG2) and lactoferrin identification. Surface roughness was statistically higher for SB-A and SB-A-NF groups. Scanning electron microscopy images confirmed that titanium surface treatments increased surface roughness with higher number of porous and scratches for SB-A and SB-A-NF groups. Total protein adsorption was significantly higher for SB-A and SB-A-NF groups (p < 0.05), which also presented higher interactions with MG2 and lactoferrin proteins. The roughing of titanium surface by spot-blasting plus acid etching treatments contribute to higher interaction with salivary proteins, such as MG2 and lactoferrin. Titanium surface roughing increases the interactions of the substratum with salivary proteins, which can influence the integration of dental implants and their components to the oral environment. However, those treatments should be used carefully intraorally, avoiding increase biofilm formation.

Erosion-resistant composite material

DOEpatents

Finch, C.B.; Tennery, V.J.; Curlee, R.M.

A highly erosion-resistant composite material is formed of chemical vapor-deposited titanium diboride on a sintered titanium diboride-nickel substrate. This material may be suitable for use in cutting tools, coal liquefaction systems, etc.

Ceramic coating system or water oxidation environments

DOEpatents

Hong, Glenn T.

1996-01-01

A process for water oxidation of combustible materials in which during at least a part of the oxidation corrosive material is present and makes contact with at least a portion of the apparatus over a contact area on the apparatus. At least a portion of the contact surface area comprises titanium dioxide coated onto a titanium metal substrate. Such ceramic composites have been found to be highly resistant to environments encountered in the process of supercritical water oxidation. Such environments typically contain greater than 50 mole percent water, together with oxygen, carbon dioxide, and a wide range of acids, bases, and salts. Pressures are typically about 27.5 to about 1000 bar while temperatures range as high as 700.degree. C. The ceramic composites are also resistant to degradation mechanisms caused by thermal stresses.

SURFACE HARDENING OF TITANIUM BY TREATMENT IN MOLTEN BORAX

DOE Office of Scientific and Technical Information (OSTI.GOV)

Minkevich, A.N.; Shul'ga, Yu.N.

1957-01-01

The surface hardening of titanium and titanium alloys by treatment in molten borax was investigated. Commercial titanium, a titanium-tungsten alloy, and an aluminum-chromium-titanium alloy were used for the experiments. To prevent oxidation of the titanium and to protect the surface, electro-chemical protection was applied, the current density being 0.1 amp/cm/sup 2/ and the the specimens were coated with a thin layer of borax. The results showed that treatment in molten borax is an effective method of increasing surface hardness. However, the strength, mmalleabiltiy, and toughness of the hardness increase is discussed. (J.S.R.)

Function of Platelet-Induced Epithelial Attachment at Titanium Surfaces Inhibits Microbial Colonization.

PubMed

Maeno, M; Lee, C; Kim, D M; Da Silva, J; Nagai, S; Sugawara, S; Nara, Y; Kihara, H; Nagai, M

2017-06-01

The aim of this study was to evaluate the barrier function of platelet-induced epithelial sheets on titanium surfaces. The lack of functional peri-implant epithelial sealing with basal lamina (BL) attachment at the interface of the implant and the adjacent epithelium allows for bacterial invasion, which may lead to peri-implantitis. Although various approaches have been reported to combat bacterial infection by surface modifications to titanium, none of these have been successful in a clinical application. In our previous study, surface modification with protease-activated receptor 4-activating peptide (PAR4-AP), which induced platelet activation and aggregation, was successful in demonstrating epithelial attachment via BL and epithelial sheet formation on the titanium surface. We hypothesized that the platelet-induced epithelial sheet on PAR4-AP-modified titanium surfaces would reduce bacterial attachment, penetration, and invasion. Titanium surface was modified with PAR4-AP and incubated with platelet-rich plasma (PRP). The aggregated platelets released collagen IV, a critical BL component, onto the PAR4-AP-modified titanium surface. Then, human gingival epithelial cells were seeded on the modified titanium surface and formed epithelial sheets. Green fluorescent protein (GFP)-expressing Escherichia coli was cultured onto PAR4-AP-modified titanium with and without epithelial sheet formation. While Escherichia coli accumulated densely onto the PAR4-AP titanium lacking epithelial sheet, few Escherichia coli were observed on the epithelial sheet on the PAR4-AP surface. No bacterial invasion into the interface of the epithelial sheet and the titanium surface was observed. These in vitro results indicate the efficacy of a platelet-induced epithelial barrier that functions to prevent bacterial attachment, penetration, and invasion on PAR4-AP-modified titanium.

Titanium Surface Chemical Composition Interferes in the Pseudomonas aeruginosa Biofilm Formation.

PubMed

Nunes Filho, Antonio; Aires, Michelle de Medeiros; Braz, Danilo Cavalcante; Hinrichs, Ruth; Macedo, Alexandre José; Alves, Clodomiro

2018-02-01

Bacterial adhesion on three different surfaces: untreated Ti, plasma nitriding, and plasma carbonitriding Ti substrates were investigated. The samples were placed in bacterial cultures of Pseudomonas aeruginosa to assess biofilm formation. The correlation between the amount of bacteria attached to the surface after a lapse of time with nanotopography and physicochemical properties was performed. TiN showed the highest capacity to avoid bacterial adhesion, while presenting intermediate roughness and wettability. Although the surface of TiCN had the highest surface roughness and low contact angle (high wettability), bacterial adhesion was intermediate on this sample. Untreated Ti, even though presenting a smooth surface and low wettability, had the highest tendency to form biofilms. © 2018 International Center for Artificial Organs and Transplantation and Wiley Periodicals, Inc.

Preparation and characterisation of titania/hydroxyapatite composite coatings obtained by sol-gel process.

PubMed

Milella, E; Cosentino, F; Licciulli, A; Massaro, C

2001-06-01

In the present work a titania network encapsulating a hydroxyapatite particulate phase is proposed as a bioceramic composite coating. The coating on a titanium substrate was produced starting from a sol containing a mixture of titania colloidal particles and hydroxyapatite submicron particles using the dip-coating technique. The microstructure, the morphology and the surface chemical composition of the coating were characterised using X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS), respectively. Adhesion tests were also performed. These analyses showed that the obtained coating was chemically clean, homogeneous, rough, porous, with a low thickness and well-defined phase composition as well as a good adhesion to the substrate.

Surface Properties of the IN SITU Formed Ceramics Reinforced Composite Coatings on TI-3AL-2V Alloys

NASA Astrophysics Data System (ADS)

Liu, Peng; Guo, Wei; Hu, Dakui; Luo, Hui; Zhang, Yuanbin

2012-04-01

The synthesis of hard composite coating on titanium alloy by laser cladding of Al/Fe/Ni+C/Si3N4 pre-placed powders has been investigated in detail. SEM result indicated that a composite coating with metallurgical joint to the substrate was formed. XRD result indicated that the composite coating mainly consisted of γ-(Fe, Ni), FeAl, Ti3Al, TiC, TiNi, TiC0.3N0.7, Ti2N, SiC, Ti5Si3 and TiNi. Compared with Ti-3Al-2V substrate, an improvement of the micro-hardness and the wear resistance was observed for this composite coating.

Anodization: a promising nano-modification technique of titanium implants for orthopedic applications.

PubMed

Yao, Chang; Webster, Thomas J

2006-01-01

Anodization is a well-established surface modification technique that produces protective oxide layers on valve metals such as titanium. Many studies have used anodization to produce micro-porous titanium oxide films on implant surfaces for orthopedic applications. An additional hydrothermal treatment has also been used in conjunction with anodization to deposit hydroxyapatite on titanium surfaces; this is in contrast to using traditional plasma spray deposition techniques. Recently, the ability to create nanometer surface structures (e.g., nano-tubular) via anodization of titanium implants in fluorine solutions have intrigued investigators to fabricate nano-scale surface features that mimic the natural bone environment. This paper will present an overview of anodization techniques used to produce micro-porous titanium oxide structures and nano-tubular oxide structures, subsequent properties of these anodized titanium surfaces, and ultimately their in vitro as well as in vivo biological responses pertinent for orthopedic applications. Lastly, this review will emphasize why anodized titanium structures that have nanometer surface features enhance bone forming cell functions.

Adhesion of osteoblasts to a nanorough titanium implant surface

PubMed Central

Gongadze, Ekaterina; Kabaso, Doron; Bauer, Sebastian; Slivnik, Tomaž; Schmuki, Patrik; van Rienen, Ursula; Iglič, Aleš

2011-01-01

This work considers the adhesion of cells to a nanorough titanium implant surface with sharp edges. The basic assumption was that the attraction between the negatively charged titanium surface and a negatively charged osteoblast is mediated by charged proteins with a distinctive quadrupolar internal charge distribution. Similarly, cation-mediated attraction between fibronectin molecules and the titanium surface is expected to be more efficient for a high surface charge density, resulting in facilitated integrin mediated osteoblast adhesion. We suggest that osteoblasts are most strongly bound along the sharp convex edges or spikes of nanorough titanium surfaces where the magnitude of the negative surface charge density is the highest. It is therefore plausible that nanorough regions of titanium surfaces with sharp edges and spikes promote the adhesion of osteoblasts. PMID:21931478

Toughened and corrosion- and wear-resistant composite structures and fabrication methods thereof

DOEpatents

Seals, Roland D.; Ripley, Edward B.; Hallman, Russell L.

2017-06-20

Composite structures having a reinforced material interjoined with a substrate, wherein the reinforced material comprises a compound selected from the group consisting of titanium monoboride, titanium diboride, and combinations thereof.

Osteogenic response of human MSCs and osteoblasts to hydrophilic and hydrophobic nanostructured titanium implant surfaces.

PubMed

Lotz, Ethan M; Olivares-Navarrete, Rene; Berner, Simon; Boyan, Barbara D; Schwartz, Zvi

2016-12-01

Microstructured implant surfaces created by grit blasting and acid etching titanium (Ti) support osseointegration. This effect is further enhanced by storing in aqueous solution to retain hydrophilicity, but this also leads to surface nanostructure formation. The purpose of this study was to assess the contributions of nanostructures on the improved osteogenic response of osteoblast lineage cells to hydrophilic microstructured Ti. Human mesenchymal stem cells (MSCs) and normal human osteoblasts (NHOsts) were cultured separately on non-nanostructured/hydrophobic (SLA), nanostructured/hydrophilic (modSLA), or nanostructured/hydrophobic (SLAnano) Ti surfaces. XPS showed elevated carbon levels on SLA and SLAnano compared to modSLA. Contact angle measurements indicated only modSLA was hydrophilic. Confocal laser microscopy revealed minor differences in mean surface roughness. SEM showed the presence of nanostructures on modSLA and SLAnano. MSCs and NHOst cells exhibited similar morphology on the substrates and osteoblastic differentiation and maturation were greatest on modSLA. These results suggest that when the appropriate microstructure is present, hydrophilicity may play a greater role in stimulating MSC and NHOst osteoblastic differentiation and maturation than the presence of nanostructures generated during storage in an aqueous environment. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 3137-3148, 2016. © 2016 Wiley Periodicals, Inc.

Superconducting composite with multilayer patterns and multiple buffer layers

DOEpatents

Wu, Xin D.; Muenchausen, Ross E.

1993-01-01

An article of manufacture including a substrate, a patterned interlayer of a material selected from the group consisting of magnesium oxide, barium-titanium oxide or barium-zirconium oxide, the patterned interlayer material overcoated with a secondary interlayer material of yttria-stabilized zirconia or magnesium-aluminum oxide, upon the surface of the substrate whereby an intermediate article with an exposed surface of both the overcoated patterned interlayer and the substrate is formed, a coating of a buffer layer selected from the group consisting of cerium oxide, yttrium oxide, curium oxide, dysprosium oxide, erbium oxide, europium oxide, iron oxide, gadolinium oxide, holmium oxide, indium oxide, lanthanum oxide, manganese oxide, lutetium oxide, neodymium oxide, praseodymium oxide, plutonium oxide, samarium oxide, terbium oxide, thallium oxide, thulium oxide, yttrium oxide and ytterbium oxide over the entire exposed surface of the intermediate article, and, a ceramic superco n FIELD OF THE INVENTION The present invention relates to the field of superconducting articles having two distinct regions of superconductive material with differing in-plane orientations whereby the conductivity across the boundary between the two regions can be tailored. This invention is the result of a contract with the Department of Energy (Contract No. W-7405-ENG-36).

Thin-film preparation by back-surface irradiation pulsed laser deposition using metal powder targets

NASA Astrophysics Data System (ADS)

Kawasaki, Hiroharu; Ohshima, Tamiko; Yagyu, Yoshihito; Ihara, Takeshi; Yamauchi, Makiko; Suda, Yoshiaki

2017-01-01

Several kinds of functional thin films were deposited using a new thin-film preparation method named the back-surface irradiation pulsed laser deposition (BIPLD) method. In this BIPLD method, powder targets were used as the film source placed on a transparent target holder, and then a visible-wavelength pulsed laser was irradiated from the holder side to the substrate. Using this new method, titanium oxide and boron nitride thin films were deposited on the silicon substrate. Surface scanning electron microscopy (SEM) images suggest that all of the thin films were deposited on the substrate with some large droplets irrespective of the kind of target used. The deposition rate of the films prepared by using this method was calculated from film thickness and deposition time to be much lower than that of the films prepared by conventional PLD. X-ray diffraction (XRD) measurement results suggest that rutile and anatase TiO2 crystal peaks were formed for the films prepared using the TiO2 rutile powder target. Crystal peaks of hexagonal boron nitride were observed for the films prepared using the boron nitride powder target. The crystallinity of the prepared films was changed by annealing after deposition.

Real-time assessment of surface interactions with titanium passivation layer by surface plasmon resonance

PubMed Central

Hirata, Isao; Yoshida, Yasuhiro; Nagaoka, Noriyuki; Hiasa, Kyou; Abe, Yasuhiko; Maekawa, Kenji; Kuboki, Takuo; Akagawa, Yasumasa; Suzuki, Kazuomi; Van Meerbeek, Bart; Messersmith, Phillip B.; Okazaki, Masayuki

2011-01-01

The high corrosion resistance and strength-to-density ratio makes titanium widely used in major industry, but also in a gamut of medical applications. Here we report for the first time on our development of a titanium passivation layer sensor that makes use of surface plasmon resonance (SPR). The deposited titanium metal layer on the sensor was passivated in air, like titanium medical devices. Our ‘Ti-SPR sensor’ enables analysis of biomolecules interactions with the passivated surface of titanium in real time. As a proof of concept, corrosion of titanium passivation layer exposed to acid was monitored in real time. Also, the Ti-SPR sensor can accurately measure the time-dependence of protein adsorption onto titanium passivation layer with a sub-nanogram per square millimeter accuracy. Besides such SPR analyses, an SPR-imaging (SPRI) enables real-time assessment of chemical surface processes that occur simultaneously at ‘multiple independent spots’ on the Ti-SPR sensor, such as acid-corrosion or adhesion of cells. Our Ti-SPR sensor will therefore be very useful to study titanium-corrosion phenomena and biomolecular titanium-surface interactions with application in a broad range of industrial and biomedical fields. PMID:22154862

Correlating single-molecule and ensemble-average measurements of peptide adsorption onto different inorganic materials.

PubMed

Kim, Seong-Oh; Jackman, Joshua A; Mochizuki, Masahito; Yoon, Bo Kyeong; Hayashi, Tomohiro; Cho, Nam-Joon

2016-06-07

The coating of solid-binding peptides (SBPs) on inorganic material surfaces holds significant potential for improved surface functionalization at nano-bio interfaces. In most related studies, the goal has been to engineer peptides with selective and high binding affinity for a target material. The role of the material substrate itself in modulating the adsorption behavior of a peptide molecule remains less explored and there are few studies that compare the interaction of one peptide with different inorganic substrates. Herein, using a combination of two experimental techniques, we investigated the adsorption of a 16 amino acid-long random coil peptide to various inorganic substrates - gold, silicon oxide, titanium oxide and aluminum oxide. Quartz crystal microbalance-dissipation (QCM-D) experiments were performed in order to measure the peptide binding affinity for inorganic solid supports at the ensemble average level, and atomic force microscopy (AFM) experiments were conducted in order to determine the adhesion force of a single peptide molecule. A positive trend was observed between the total mass uptake of attached peptide and the single-molecule adhesion force on each substrate. Peptide affinity for gold was appreciably greater than for the oxide substrates. Collectively, the results obtained in this study offer insight into the ways in which inorganic materials can differentially influence and modulate the adhesion of SBPs.

Ceramic material suitable for repair of a space vehicle component in a microgravity and vacuum environment, method of making same, and method of repairing a space vehicle component

NASA Technical Reports Server (NTRS)

Riedell, James A. (Inventor); Easler, Timothy E. (Inventor)

2009-01-01

A precursor of a ceramic adhesive suitable for use in a vacuum, thermal, and microgravity environment. The precursor of the ceramic adhesive includes a silicon-based, preceramic polymer and at least one ceramic powder selected from the group consisting of aluminum oxide, aluminum nitride, boron carbide, boron oxide, boron nitride, hafnium boride, hafnium carbide, hafnium oxide, lithium aluminate, molybdenum silicide, niobium carbide, niobium nitride, silicon boride, silicon carbide, silicon oxide, silicon nitride, tin oxide, tantalum boride, tantalum carbide, tantalum oxide, tantalum nitride, titanium boride, titanium carbide, titanium oxide, titanium nitride, yttrium oxide, zirconium diboride, zirconium carbide, zirconium oxide, and zirconium silicate. Methods of forming the ceramic adhesive and of repairing a substrate in a vacuum and microgravity environment are also disclosed, as is a substrate repaired with the ceramic adhesive.

Characteristics of hydroxyapatite coated titanium porous coatings on Ti-6Al-4V substrates by plasma sprayed method.

PubMed

Yang, C Y; Chen, C R; Chang, E; Lee, T M

2007-08-01

A porous metal coating applied to solid substrate implants has been shown, in vivo, to anchor implants by bone ingrowth. Calcium phosphate ceramics, in particular hydroxyapatite [Ca(10)(PO(4))(6)(OH)(2), HA], are bioactive ceramics, which are known to be biocompatible and osteoconductive, and these ceramics deposited on to porous-coated devices may enhance bone ingrowth and implant fixation. In this study, bi-feedstock of the titanium powder and composite (Na(2)CO(3)/HA) powder were simultaneously deposited on a Ti-6Al-4V substrate by a plasma sprayed method. At high temperature of plasma torch, the solid state of Na(2)CO(3) would decompose to release CO(2) gas and then eject the molten Ti powder to induce the interconnected pores in the coatings. After cleaning and soaking in deionized water, the residual Na(2)CO(3) in the coating would dissolve to form the open pores, and the HA would exist at the surface of pores in the inner coatings. By varying the particle size of the composite powder, the porosity of porous coating could be varied from 25.0 to 34.0%, and the average pore size of the porous coating could be varied to range between 158.5 and 202.0 microm. Using a standard adhesive test (ASTM C-633), the bonding strength of the coating is between 27.3 and 38.2 MPa. By SEM, the HA was observed at the surface of inner pore in the porous coating. These results suggest that the method exhibits the potential to manufacture the bioactive ceramics on to porous-coated specimen to achieve bone ingrowth fixation for biomedical applications.

Silica-polyethylene glycol hybrids synthesized by sol-gel: Biocompatibility improvement of titanium implants by coating.

PubMed

Catauro, M; Bollino, F; Papale, F; Ferrara, C; Mustarelli, P

2015-10-01

Although metallic implants are the most used in dental and orthopaedic fields, they can early fail due to low tissue tolerance or osseointegration ability. To overcome this drawback, functional coatings can be applied on the metallic surface to provide a firm fixation of the implants. The objective of the present study was twofold: to synthesize and to characterize silica/polyethylene glycol (PEG) hybrid materials using sol-gel technique and to investigate their capability to dip-coat titanium grade 4 (Ti-gr4) substrates to improve their biological properties. Various hybrid systems have been synthesized by changing the ratio between the organic and inorganic phases in order to study the influence of the polymer amount on the structure and, thus, on the properties of the coatings. Fourier transform infrared (FTIR) spectroscopy and solid state Nuclear Magnetic Resonance (NMR) allowed us to detect the formation of hydrogen bonds between the inorganic sol-gel matrix and the organic component. SEM analysis showed that high PEG content enables to obtain crack free-coating. Moreover, the effective improvement in biological properties of Ti-gr4 implants has been evaluated by performing in vitro tests. The bioactivity of the hybrid coatings has been showed by the hydroxyapatite formation on the surface of SiO2/PEG coated Ti-gr4 substrates after soaking in a simulated body fluid and the lack of cytotoxicity by the WST-8 Assay. The results showed that the coated substrates are more bioactive and biocompatible than the uncoated ones and that the bioactivity is not significantly affected by PEG amount whereas its addition makes the films more biocompatible. Copyright © 2015. Published by Elsevier B.V.

Influence of charged defects on the interfacial bonding strength of tantalum- and silver-doped nanograined TiO2.

PubMed

Azadmanjiri, Jalal; Wang, James; Berndt, Christopher C; Kapoor, Ajay; Zhu, De Ming; Ang, Andrew S M; Srivastava, Vijay K

2017-05-17

A nano-grained layer including line defects was formed on the surface of a Ti alloy (Ti alloy , Ti-6Al-4V ELI). Then, the micro- and nano-grained Ti alloy with the formation of TiO 2 on its top surface was coated with a bioactive Ta layer with or without incorporating an antibacterial agent of Ag that was manufactured by magnetron sputtering. Subsequently, the influence of the charged defects (the defects that can be electrically charged on the surface) on the interfacial bonding strength and hardness of the surface system was studied via an electronic model. Thereby, material systems of (i) Ta coated micro-grained titanium alloy (Ta/MGTi alloy ), (ii) Ta coated nano-grained titanium alloy (Ta/NGTi alloy ), (iii) TaAg coated micro-grained titanium alloy (TaAg/MGTi alloy ) and (iv) TaAg coated nano-grained titanium alloy (TaAg/NGTi alloy ) were formed. X-ray photoelectron spectroscopy was used to probe the electronic structure of the micro- and nano-grained Ti alloy , and so-formed heterostructures. The thin film/substrate interfaces exhibited different satellite peak intensities. The satellite peak intensity may be related to the interfacial bonding strength and hardness of the surface system. The interfacial layer of TaAg/NGTi alloy exhibited the highest satellite intensity and maximum hardness value. The increased bonding strength and hardness in the TaAg/NGTi alloy arises due to the negative core charge of the dislocations and neighbor space charge accumulation, as well as electron accumulation in the created semiconductor phases of larger band gap at the interfacial layer. These two factors generate interfacial polarization and enhance the satellite intensity. Consequently, the interfacial bonding strength and hardness of the surface system are improved by the formation of mixed covalent-ionic bonding structures around the dislocation core area and the interfacial layer. The bonding strength relationship by in situ XPS on the metal/TiO 2 interfacial layer may be examined with other noble metals and applied in diverse fields.

Plasma sprayed hydroxyapatite coatings on titanium substrates. Part 2: optimisation of coating properties.

PubMed

Tsui, Y C; Doyle, C; Clyne, T W

1998-11-01

Heat treatment and the introduction of a Ti bond coat have been applied to hydroxyapatite (HA) coatings sprayed using different plasma powers and gas mixtures. Attempts were made in this way to achieve optimal coating properties for orthopaedic implants. In particular, the effects on the degree of crystallinity, the adhesion, the OH ion content and the purity were evaluated. Heat treatment at 700 C for 1 h in air proved to be effective in increasing the crystallinity, regaining the OH- ion and removing other non-HA compounds, although it caused a significant decrease in the degree of adhesion (interfacial fracture toughness) for those specimens sprayed at high powers. This heat treatment was found to induce significant transformation of amorphous HA to the crystalline form, while not detrimentally changing the properties of the underlying Ti-6Al-4V substrates. Precoating with a 100 microm Ti layer increased the adhesion of the HA coatings on Ti-6Al-4V substrates, primarily by providing a rougher surface and promoting better mechanical interlocking. Changes in coating properties during immersion in biological fluids were also studied and were found to depend critically on the chemical composition of the fluids. Small precipitates formed on the coating surfaces when immersed in Ringers solution. These might account for the apparent drop in the degree of crystallinity when measured using X-ray diffraction. A significant drop in the interfacial adhesion was found for those coatings sprayed at high powers. This could be offset by prior precoating with a titanium bond coat and suitable heat treatment. In summary, the following processing sequence is suggested in order to achieve optimum coating properties: precoating the substrate with a layer of Ti (approximately 100 microm), spraying HA at a sufficiently high-power level (depending on particle size and gas mixture) and heat treatment at 700 degrees C for 1 h in air.

Molecular plasma deposition: biologically inspired nanohydroxyapatite coatings on anodized nanotubular titanium for improving osteoblast density

PubMed Central

Balasundaram, Ganesan; Storey, Daniel M; Webster, Thomas J

2015-01-01

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. PMID:25609958

Contrast image formation based on thermodynamic approach and surface laser oxidation process for optoelectronic read-out system

NASA Astrophysics Data System (ADS)

Scherbak, Aleksandr; Yulmetova, Olga

2018-05-01

A pulsed fiber laser with the wavelength 1.06 μm was used to treat titanium nitride film deposited on beryllium substrates in the air with intensities below an ablation threshold to provide oxide formation. Laser oxidation results were predicted by the chemical thermodynamic method and confirmed by experimental techniques (X-ray diffraction). The developed technology of contrast image formation is intended to be used for optoelectronic read-out system.

Characterization of Sputtered Nickel-Titanium (NiTi) Stress and Thermally Actuated Cantilever Bimorphs Based on NiTi Shape Memory Alloy (SMA)

DTIC Science & Technology

2015-11-01

necessary anneal . Following this, a thin film of NiTi was blanket sputtered at 600 °C. This NiTi blanket layer was then wet -etch patterned using a...varying the sputter parameters during NiTi deposition, such as thickness, substrate temperature during deposition and anneal , and argon pressure during...6 Fig. 4 Surface texture comparison between NiTi sputtered at RT, then annealed at 600 °C, and NiTi

Histomorphometric and histologic evaluation of titanium-zirconium (aTiZr) implants with anodized surfaces.

PubMed

Sharma, Ajay; McQuillan, A James; Shibata, Yo; Sharma, Lavanya A; Waddell, John Neil; Duncan, Warwick John

2016-05-01

The choice of implant surface has a significant influence on osseointegration. Modification of TiZr surface by anodization is reported to have the potential to modulate the osteoblast cell behaviour favouring more rapid bone formation. The aim of this study is to investigate the effect of anodizing the surface of TiZr discs with respect to osseointegration after four weeks implantation in sheep femurs. Titanium (Ti) and TiZr discs were anodized in an electrolyte containing DL-α-glycerophosphate and calcium acetate at 300 V. The surface characteristics were analyzed by scanning electron microscopy, electron dispersive spectroscopy, atomic force microscopy and goniometry. Forty implant discs with thickness of 1.5 and 10 mm diameter (10 of each-titanium, titanium-zirconium, anodized titanium and anodized titanium-zirconium) were placed in the femoral condyles of 10 sheep. Histomorphometric and histologic analysis were performed 4 weeks after implantation. The anodized implants displayed hydrophilic, porous, nano-to-micrometer scale roughened surfaces. Energy dispersive spectroscopy analysis revealed calcium and phosphorous incorporation into the surface of both titanium and titanium-zirconium after anodization. Histologically there was new bone apposition on all implanted discs, slightly more pronounced on anodised discs. The percentage bone-to-implant contact measurements of anodized implants were higher than machined/unmodified implants but there was no significant difference between the two groups with anodized surfaces (P > 0.05, n = 10). The present histomorphometric and histological findings confirm that surface modification of titanium-zirconium by anodization is similar to anodised titanium enhances early osseointegration compared to machined implant surfaces.

Establishment of Epithelial Attachment on Titanium Surface Coated with Platelet Activating Peptide

PubMed Central

Sugawara, Shiho; Maeno, Masahiko; Lee, Cliff; Nagai, Shigemi; Kim, David M.; Da Silva, John; Kondo, Hisatomo

2016-01-01

The aim of this study was to produce epithelial attachment on a typical implant abutment surface of smooth titanium. A challenging complication that hinders the success of dental implants is peri-implantitis. A common cause of peri-implantitis may results from the lack of epithelial sealing at the peri-implant collar. Histologically, epithelial sealing is recognized as the attachment of the basement membrane (BM). BM-attachment is promoted by activated platelet aggregates at surgical wound sites. On the other hand, platelets did not aggregate on smooth titanium, the surface typical of the implant abutment. We then hypothesized that epithelial BM-attachment was produced when titanium surface was modified to allow platelet aggregation. Titanium surfaces were coated with a protease activated receptor 4-activating peptide (PAR4-AP). PAR4-AP coating yielded rapid aggregation of platelets on the titanium surface. Platelet aggregates released robust amount of epithelial chemoattractants (IGF-I, TGF-β) and growth factors (EGF, VEGF) on the titanium surface. Human gingival epithelial cells, when they were co-cultured on the platelet aggregates, successfully attached to the PAR4-AP coated titanium surface with spread laminin5 positive BM and consecutive staining of the epithelial tight junction component ZO1, indicating the formation of complete epithelial sheet. These in-vitro results indicate the establishment of epithelial BM-attachment to the titanium surface. PMID:27741287

Wrinkle-free graphene electrodes in zinc tin oxide thin-film transistors for large area applications.

PubMed

Lee, Se-Hee; Kim, Jae-Hee; Park, Byeong-Ju; Park, Jozeph; Kim, Hyun-Suk; Yoon, Soon-Gil

2017-02-17

Wrinkle-free graphene was used to form the source-drain electrodes in thin film transistors based on a zinc tin oxide (ZTO) semiconductor. A 10 nm thick titanium adhesion layer was applied prior to transferring a conductive graphene film on top of it by chemical detachment. The formation of an interlayer oxide between titanium and graphene allows the achievement of uniform surface roughness over the entire substrate area. The resulting devices were thermally treated in ambient air, and a substantial decrease in field effect mobility is observed with increasing annealing temperature. The increase in electrical resistivity of the graphene film at higher annealing temperatures may have some influence, however the growth of the oxide interlayer at the ZTO/Ti boundary is suggested to be most influential, thereby inducing relatively high contact resistance.

Wrinkle-free graphene electrodes in zinc tin oxide thin-film transistors for large area applications

NASA Astrophysics Data System (ADS)

Lee, Se-Hee; Kim, Jae-Hee; Park, Byeong-Ju; Park, Jozeph; Kim, Hyun-Suk; Yoon, Soon-Gil

2017-02-01

Wrinkle-free graphene was used to form the source-drain electrodes in thin film transistors based on a zinc tin oxide (ZTO) semiconductor. A 10 nm thick titanium adhesion layer was applied prior to transferring a conductive graphene film on top of it by chemical detachment. The formation of an interlayer oxide between titanium and graphene allows the achievement of uniform surface roughness over the entire substrate area. The resulting devices were thermally treated in ambient air, and a substantial decrease in field effect mobility is observed with increasing annealing temperature. The increase in electrical resistivity of the graphene film at higher annealing temperatures may have some influence, however the growth of the oxide interlayer at the ZTO/Ti boundary is suggested to be most influential, thereby inducing relatively high contact resistance.

Tribological Properties of Surface-Textured and Plasma-Nitrided Pure Titanium Under Oil Lubrication Condition

NASA Astrophysics Data System (ADS)

Zhang, Baosen; Dong, Qiangsheng; Ba, Zhixin; Wang, Zhangzhong; Shi, Hancheng; Xue, Yanting

2018-01-01

Plasma nitriding was conducted as post-treatment for surface texture on pure titanium to obtain a continuous nitriding layer. Supersonic fine particles bombarding (SFPB) was carried out to prepare surface texture. The surface morphologies and chemical composition were analyzed using scanning electron microscope and energy disperse spectroscopy. The microstructures of modified layers were characterized by transmission electron microscope. The tribological properties of surface-textured and duplex-treated pure titanium under oil lubrication condition were systematically investigated in the ball-on-plate reciprocating mode. The effects of applied load and sliding velocity on the tribological behavior were analyzed. The results show that after duplex treatments, the grains size in modified layer becomes slightly larger, and hardness is obviously improved. Wear resistance of duplex-treated pure titanium is significantly improved referenced to untreated and surface-textured pure titanium, which is 3.22 times as much as untreated pure titanium and 2.15 times of that for surface-textured pure titanium, respectively.

Surface modification of an aluminum alloy by electron beam introducing TiCN nanoparticles

NASA Astrophysics Data System (ADS)

Kolev, M.; Dimitrova, R.; Parshorov, St.; Valkov, St.; Lazarova, R.; Petrov, P.

2018-03-01

TiCN nanopowder deposited in an appropriate way on the surface of an AlSi12Cu2NiMg substrate was incorporated in the matrix using an electron beam technology. The samples were studied by means of light microscopy, SEM, and EDX; their microhardness was also determined. The formation was found of a uniform and dense coating with a thickness of 7 – 10 μgm with a good adherence to the substrate. A modified zone appeared under the coating with a thickness of 100 – 150 μgm containing dendrites of an α-solid solution and a fine eutectic between them, as well as primary silicon crystals. The microhardness of this modified zone was up to 2.4 times higher than that of the matrix. The results of SEM and EDX studies revealed unambiguously the presence of titanium in the coating and in the zones below it. Obviously, the electron beam treatment resulted in the TiCN nanoparticles penetrating into the coating and the substrate immediately below the coating.

Air Purification Pavement Surface Coating by Atmospheric Pressure Cold Plasma

NASA Astrophysics Data System (ADS)

Westergreen, Joe; Pedrow, Patrick; Shen, Shihui; Jobson, Bertram

2011-10-01

This study develops an atmospheric pressure cold plasma (APCP) reactor to produce activated radicals from precursor molecules, and to immobilize nano titanium dioxide (TiO2) powder to substrate pavement materials. TiO2 has photocatalytic properties and under UV light can be used to oxidize and remove volatile organic compounds (VOCs) and nitrogen oxides (NOx) from the atmosphere. Although TiO2 treated paving materials have great potential to improve air quality, current techniques to adhere TiO2 to substrate materials are either not durable or reduce direct contact of TiO2 with UV light, reducing the photocatalytic effect. To solve this technical difficulty, this study introduces APCP techniques to transportation engineering to coat TiO2 to pavement. Preliminary results are promising and show that TiO2 can be incorporated successfully into an APCP environment and can be immobilized at the surface of the asphalt substrate. The TiO2 coated material with APCP shows the ability to reduce nitrogen oxides when exposed to UV light in an environmental chamber. The plasma reactor utilizes high voltage streamers as the plasma source.

Microstructure characteristics and properties of in-situ formed TiC/Ni based alloy composite coating by laser cladding

NASA Astrophysics Data System (ADS)

Yang, Sen; Liu, Wenjin; Zhong, Minlin

2003-03-01

Different weight ratio of nickel based alloy, titanium and graphite powders were mixed and then laser cladded onto carbon steel substrate to produce a surface metal matrix composite layer. The experimental results showed that the coating was uniform, continuous and free of cracks. An excellent bonding between the coating and the carbon steel substrate was ensured by the strong metallurgical interface. The microstructures of the coating were mainly composed of γ-Ni dendrite, M23C6, a small amount of CrB, and dispersed TiC particles, and the in-situ generated TiCp/matrix interfaces were clean and free from deleterious surface reaction. The morphologies of TiC particles changed from the global, cluster to flower-like shape, the volume fraction of TiCp and the microhardness gradually increased from the bottom to the top of the coating layer, and the maximum microhardness of the coating was about HV0.2850, 3 times larger than that of steel substrate. The volume fraction of TiC particles increased with increasing of volume fraction of Ti and C too.

Surface modification of titanium and titanium alloys by ion implantation.

PubMed

Rautray, Tapash R; Narayanan, R; Kwon, Tae-Yub; Kim, Kyo-Han

2010-05-01

Titanium and titanium alloys are widely used in biomedical devices and components, especially as hard tissue replacements as well as in cardiac and cardiovascular applications, because of their desirable properties, such as relatively low modulus, good fatigue strength, formability, machinability, corrosion resistance, and biocompatibility. However, titanium and its alloys cannot meet all of the clinical requirements. Therefore, to improve the biological, chemical, and mechanical properties, surface modification is often performed. In view of this, the current review casts new light on surface modification of titanium and titanium alloys by ion beam implantation. (c) 2010 Wiley Periodicals, Inc.

Enhanced human bone marrow mesenchymal stem cell functions on cathodic arc plasma-treated titanium.

PubMed

Zhu, Wei; Teel, George; O'Brien, Christopher M; Zhuang, Taisen; Keidar, Michael; Zhang, Lijie Grace

2015-01-01

Surface modification of titanium for use in orthopedics has been explored for years; however, an ideal method of integrating titanium with native bone is still required to this day. Since human bone cells directly interact with nanostructured extracellular matrices, one of the most promising methods of improving titanium's osseointegration involves inducing bio-mimetic nanotopography to enhance cell-implant interaction. In this regard, we explored an approach to functionalize the surface of titanium by depositing a thin film of textured titanium nanoparticles via a cathodic arc discharge plasma. The aim is to improve human bone marrow mesenchymal stem cell (MSC) attachment and differentiation and to reduce deleterious effects of more complex surface modification methods. Surface functionalization was analyzed by scanning electron microscopy, atomic force microscopy, contact angle testing, and specific protein adsorption. Scanning electron microscopy and atomic force microscopy examination demonstrate the deposition of titanium nanoparticles and the surface roughness change after coating. The specific fibronectin adsorption was enhanced on the modified titanium surface that associates with the improved hydrophilicity. MSC adhesion and proliferation were significantly promoted on the nanocoated surface. More importantly, compared to bare titanium, greater production of total protein, deposition of calcium mineral, and synthesis of alkaline phosphatase were observed from MSCs on nanocoated titanium after 21 days. The method described herein presents a promising alternative method for inducing more cell favorable nanosurface for improved orthopedic applications.

Enhanced in vitro biological activity generated by surface characteristics of anodically oxidized titanium--the contribution of the oxidation effect.

PubMed

Wurihan; Yamada, A; Suzuki, D; Shibata, Y; Kamijo, R; Miyazaki, T

2015-05-20

Anodically oxidized titanium surfaces, prepared by spark discharge, have micro-submicron surface topography and nano-scale surface chemistry, such as hydrophilic functional groups or hydroxyl radicals in parallel. The complexity of the surface characteristics makes it difficult to draw a clear conclusion as to which surface characteristic, of anodically oxidized titanium, is critical in each biological event. This study examined the in vitro biological changes, induced by various surface characteristics of anodically oxidized titanium with, or without, release of hydroxyl radicals onto the surface. Anodically oxidized titanium enhanced the expression of genes associated with differentiating osteoblasts and increased the degree of matrix mineralization by these cells in vitro. The phenotypes of cells on the anodically oxidized titanium were the same with, or without, release of hydroxyl radicals. However, the nanomechanical properties of this in vitro mineralized tissue were significantly enhanced on surfaces, with release of hydroxyl radicals by oxidation effects. In addition, the mineralized tissue, produced in the presence of bone morphogenetic protein-2 on bare titanium, had significantly weaker nanomechanical properties, despite there being higher osteogenic gene expression levels. We show that enhanced osteogenic cell differentiation on modified titanium is not a sufficient indicator of enhanced in vitro mineralization. This is based on the inferior mechanical properties of mineralized tissues, without either being cultured on a titanium surface with release of hydroxyl radicals, or being supplemented with lysyl oxidase family members.

Analytical investigations of poly(acrylic acid) coatings electrodeposited on titanium-based implants: a versatile approach to biocompatibility enhancement.

PubMed

De Giglio, E; Cometa, S; Cioffi, N; Torsi, L; Sabbatini, L

2007-12-01

A polyacrylic acid film was synthesized on titanium substrates from aqueous solutions via an electroreductive process for the first time. This work was done in order to develop a versatile coating for titanium-based orthopaedic implants that acts as both an effective bioactive surface and an effective anti-corrosion barrier. The chemical structure of the PAA coating was investigated by X-ray photoelectron spectroscopy (XPS). Scanning electron microscopy (SEM) was employed to evaluate the effect of annealing treatment on the morphology of the coatings in terms of their uniformity and porosity. Inductively coupled plasma mass spectrometry was used to measure ion concentrations in ion release tests performed on Ti-6Al-4V sheets modified with PAA coatings (annealed and unannealed). Results indicate that the annealing process produces coatings that possess considerable anti-corrosion performance. Moreover, the availability and the reactivity of the surface carboxylic groups were exploited in order to graft biological molecules onto the PAA-modified titanium implants. The feasibility of the grafting reaction was tested using a single aminoacid residue. A fluorinated aminoacid was selected, and the grafting reaction was monitored both by XPS, using fluorine as a marker element, and via quartz crystal microbalance (QCM) measurements. The success of the grafting reaction opens the door to the synthesis of a wide variety of PAA-based coatings that are functionalized with selected bioactive molecules and promote positive reactions with the biological system interfacing the implant while considerably reducing ion release into surrounding tissues.

Preparation and study of Titanium Nitride films by reactive sputtering and an investigation of target poisoning during the process

NASA Astrophysics Data System (ADS)

Aziz, Tareque; Rumaiz, Abdul

Titanium Nitride (TiNx) thin films were prepared by reactive dc sputtering in presence of Ar-N2 plasma. The thin films were grown on Quartz and pure Si surfaces. The Ar-N2 content ratio was gradually varied while the substrate and the Titanium target were kept at room temperature. Structural properties, optical and electrical properties of the thin films were studied by using X-ray Photoelectron Spectroscopy (XPS) and XRD and 4 probe resistivity measurement. Target poisoning of the Ti target was also studied by varying reactive gas concentration and measuring the target current. A study of target current vs growth rate of the films was performed to investigate the onset of ``poison'' mode.Although there was an insignificant drop in plasma current, we noticed a drop in the deposition rate. This result was tested against Monte Carlo simulations using SRIM simulations. Effects of annealing on the crystallinity and the sheet resistance will also be discussed. The work has been supported by BSA,DOE.

Improved bonding strength of bioactive cermet Cold Gas Spray coatings.

PubMed

Gardon, M; Concustell, A; Dosta, S; Cinca, N; Cano, I G; Guilemany, J M

2014-12-01

The fabrication of cermet biocompatible coatings by means Cold Gas Spray (CGS) provides prosthesis with outstanding mechanical properties and the required composition for enhancing the bioactivity of prosthetic materials. In this study, hydroxyapatite/Titanium coatings were deposited by means of CGS technology onto titanium alloy substrates with the aim of building-up well-bonded homogeneous coatings. Powders were blended in different percentages and sprayed; as long as the amount of hydroxyapatite in the feedstock increased, the quality of the coating was reduced. Besides, the relation between the particle size distribution of ceramic and metallic particles is of significant consideration. Plastic deformation of titanium particles at the impact eased the anchoring of hard hydroxyapatite particles present at the top surface of the coating, which assures the looked-for interaction with the cells. Coatings were immersed in Hank's solution for 1, 4 and 7 days; bonding strength value was above 60 MPa even after 7 days, which enhances common results of HAp coatings obtained by conventional thermal spray technologies. Copyright © 2014 Elsevier B.V. All rights reserved.

Mechanical properties of titanium-hydroxyapatite (Ti-HA) composite coating on stainless steel prepared by thermal spraying

NASA Astrophysics Data System (ADS)

Rosmamuhamadani, R.; Azhar, N. H.; Talari, M. K.; Yahaya, Sabrina M.; Sulaiman, S.; Ismail, M. I. S.

2017-09-01

Addition of hydroxyapatite (HA) can enhance the bioactivity of the common metallic implant due to its similarity with natural bones and teeth. In this investigation, high velocity oxy-fuel (HVOFT) technique was used to deposit titanium-hydroxyapatite (Ti-HA) composite on stainless steel substrate plate with different percentage of HA for biomedical applications. The aim of this research is to investigate the mechanical properties of Ti-HA coating such as hardness, adhesion strength and wear behaviour. The hardness and strength was determined by using SHIMADZU-microhardness Vickers tester and PosiTest AT portable adhesion tester respectively. The wear test was performed by using pin-on-disk equipment and field emission scanning electron microscope (FESEM) used to determine the extent of surface damage. From the results obtained, mechanical properties such as hardness and adhesion strength of titanium (Ti) coating decreased with the increased of HA contents. Meanwhile, the coefficient of friction of Ti-10% HA coating shows the highest value compare to others as three-body abrasion had occurred during the test.

Electrical Polarization of Titanium Surfaces for the Enhancement of Osteoblast Differentiation

PubMed Central

Gittens, Rolando A.; Olivares-Navarrete, Rene; Rettew, Robert; Butera, Robert J.; Alamgir, Faisal M.; Boyan, Barbara D.; Schwartz, Zvi

2014-01-01

Electrical stimulation has been used clinically to promote bone regeneration in cases of fractures with delayed union or nonunion, with several in vitro and in vivo reports suggesting its beneficial effects on bone formation. However, the use of electrical stimulation of titanium (Ti) implants to enhance osseointegration is less understood, in part because of the few in vitro models that attempt to represent the in vivo environment. In this article, the design of a new in vitro system that allows direct electrical stimulation of osteoblasts through their Ti substrates without the flow of exogenous currents through the media is presented, and the effect of applied electrical polarization on osteoblast differentiation and local factor production was evaluated. A custom-made polycarbonate tissue culture plate was designed to allow electrical connections directly underneath Ti disks placed inside the wells, which were supplied with electrical polarization ranging from 100 to 500 mV to stimulate MG63 osteoblasts. Our results show that electrical polarization applied directly through Ti substrates on which the cells are growing in the absence of applied electrical currents may increase osteoblast differentiation and local factor production in a voltage-dependent manner. PMID:23996899

MAO-derived hydroxyapatite/TiO2 nanostructured multi-layer coatings on titanium substrate

NASA Astrophysics Data System (ADS)

Abbasi, S.; Golestani-Fard, F.; Rezaie, H. R.; Mirhosseini, S. M. M.

2012-11-01

In this study, titanium substrates which previously oxidized through Micro arc oxidation method, was coated by Hydroxyapatite (HAp) coating once more by means of the same method. Morphology, topography and chemical properties as well as phase composition and thickness of layers were studied to reveal the effect of the electrolyte concentration on coating features. According to results, the obtained coatings are consisted of HAp and titania as the major phases along with minor amounts of calcium titanate and α-tri calcium phosphate. Ca and P are present on surface of obtained layers as well as predictable Ti and O based on the XPS results. Thickness profile of coatings figured out that by increasing the electrolyte concentration, especially by addition of more Calcium Acetate (CA) to electrolyte, the thickness of HAp layer would rise, consequently. However, the influence of coating time on thickness of obtained coatings would be more considerable than electrolyte concentration. High specific area coatings with nest morphology were obtained in Electrolyte containing 5 g/L β-Glycero Phosphate (β-GP) and 5 g/L CA. Increasing coating duration time in this kind of coatings would cause deduction of the nesting in their structure.

MC3T3-E1 Cells on Titanium Surfaces with Nanometer Smoothness and Fibronectin Immobilization

PubMed Central

Hayakawa, Tohru; Yoshida, Eiji; Yoshimura, Yoshitaka; Uo, Motohiro; Yoshinari, Masao

2012-01-01

The present study was aimed to evaluate the viability and total protein contents of osteoblast-like cells on the titanium surface with different surface mechanical treatment, namely, nanometer smoothing (Ra: approximately 2.0 nm) and sandblasting (Ra: approximately 1.0 μm), and biochemical treatment, namely, with or without fibronectin immobilization. Fibronectin could be easily immobilized by tresyl chloride-activation technique. MC3T3-E1 cells were seeded on the different titanium surfaces. Cell viability was determined by MTT assay. At 1 day of cell culture, there were no significant differences in cell viability among four different titanium surfaces. At 11 days, sandblasted titanium surface with fibronectin immobilization showed the significantly highest cell viability than other titanium surface. No significant differences existed for total protein contents among four different titanium surfaces at 11 days of cell culture. Scanning electron microscopy observation revealed that smoothness of titanium surface produced more spread cell morphologies, but that fibronectin immobilization did not cause any changes of the morphologies of attached cells. Fibronectin immobilization provided greater amount of the number of attached cells and better arrangement of attached cells. In conclusion, the combination of sandblasting and fibronectin immobilization enhanced the cell viability and fibronectin immobilization providing better arrangements of attached cells. PMID:22675359

Effect of applied voltage on surface properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

NASA Astrophysics Data System (ADS)

Chuan, Lee Te; Rathi, Muhammad Fareez Mohamad; Abidin, Muhamad Yusuf Zainal; Abdullah, Hasan Zuhudi; Idris, Maizlinda Izwana

2015-07-01

Anodic oxidation is a surface modification method which combines electric field driven metal and oxygen ion diffusion for formation of oxide layer on the anode surface. This method has been widely used to modify the surface morphology of biomaterial especially titanium. This study aimed to investigate the effect of applied voltage on titanium. Specifically, the titanium foil was anodised in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) with different applied voltage (50-350 V), electrolyte concentration (0.04 M β-GP + 0.4 M CA), anodising time (10minutes) and current density (50 and 70 mA.cm-2) at room temperature. Surface oxide properties of anodised titanium were characterised by digital single-lens reflex camera (DSLR camera), field emission scanning electron microscope (FESEM) and atomic force microscopy (AFM). At lower applied voltage (≤150 V), surface of titanium foils were relatively smooth. With increasing applied voltage (≥250 V), the oxide layer became more porous and donut-shaped pores were formed on the surface of titanium foils. The AFM results indicated that the surface roughness of anodised titanium increases with increasing of applied voltage. The porous and rough surface is able to promote the osseointegration and reduce the suffering time of patient.

Nickel titanium alloy: Cytotoxicity evaluation on microorganism culture

NASA Astrophysics Data System (ADS)

Dinca, V. C.; Soare, S.; Barbalat, A.; Dinu, C. Z.; Moldovan, A.; Stoica, I.; Vassu, T.; Purice, A.; Scarisoareanu, N.; Birjega, R.; Craciun, V.; DeStefano, V. Ferrari; Dinescu, M.

2006-04-01

High purity nickel (Ni) and titanium (Ti) targets have been used to form well-defined thin films of nitinol on Ti substrate by pulsed laser deposition (PLD) technique. Their chemical composition, crystalline structure and surface properties have been investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM) and atomic force microscopy (AFM). We have shown that by varying the deposition parameters such as laser fluence and number of laser pulses, we are able to control the film thickness as well as film's uniformity and roughness. Cytocompatibility tests have been performed through in vitro assays using microorganisms culture cells such as yeasts ( Saccharomyces cerevisiae) and bacteria ( Escherichia coli), in order to determine the thin film's toxic potential at the in vitro cellular level. Microorganism's adhesion on the nitinol surface was observed and the biofilm formation has been analyzed and quantified. Our results have shown no reactivity detected in cell culture exposed to NiTi films in comparison with the negative controls and a low adherence of the microorganisms on the nitinol surface that is an important factor for biofilm prevention. We can, therefore, conclude that NiTi is a good candidate material to be used for implants and medical devices.

Surface modification of porous titanium with rice husk as space holder

NASA Astrophysics Data System (ADS)

Wang, Xinsheng; Hou, Junjian; Liu, Yanpei

2018-06-01

Porous titanium was characterized after its surface modification by acid and alkali solution immersion. The results show that the acid surface treatment caused the emergence of flocculent sodium titanate and induced apatite formation. The surface modification of porous titanium promotes biological activation, and the application of porous titanium is also improved as an implant material because of the existence of C and Si.

Nanotextured titanium surfaces stimulate spreading, migration, and growth of rat mast cells.

PubMed

Marcatti Amarú Maximiano, William; Marino Mazucato, Vivian; Tambasco de Oliveira, Paulo; Célia Jamur, Maria; Oliver, Constance

2017-08-01

Titanium is a biomaterial widely used in dental and orthopedic implants. Since tissue-implant interactions occur at the nanoscale level, nanotextured titanium surfaces may affect cellular activity and modulate the tissue response that occurs at the tissue-implant interface. Therefore, the characterization of diverse cell types in response to titanium surfaces with nanotopography is important for the rational design of implants. Mast cells are multifunctional cells of the immune system that release a range of chemical mediators involved in the inflammatory response that occurs at the tissue-implant interface. Therefore, the aim of this study was to investigate the effects of the nanotopography of titanium surfaces on the physiology of mast cells. The results show that the nanotopography of titanium surfaces promoted the spreading of mast cells, which was accompanied by the reorganization of the cytoskeleton. Also, the nanotopography of titanium surfaces enhanced cell migration and cell growth, but did not alter the number of adherent cells in first hours of culture or affect focal adhesions and mediator release. Thus, the results show that nanotopography of titanium surfaces can affect mast cell physiology, and represents an improved strategy for the rational production of surfaces that stimulate tissue integration with the titanium implants. © 2017 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 2150-2161, 2017. © 2017 Wiley Periodicals, Inc.

Micromachined electrode array

DOEpatents

Okandan, Murat; Wessendorf, Kurt O.

2007-12-11

An electrode array is disclosed which has applications for neural stimulation and sensing. The electrode array, in certain embodiments, can include a plurality of electrodes each of which is flexibly attached to a common substrate using a plurality of springs to allow the electrodes to move independently. In other embodiments of the electrode array, the electrodes can be fixed to the substrate. The electrode array can be formed from a combination of bulk and surface micromachining, and can include electrode tips having an electroplated metal (e.g. platinum, iridium, gold or titanium) or a metal oxide (e.g. iridium oxide) for biocompatibility. The electrode array can be used to form a part of a neural prosthesis, and is particularly well adapted for use in an implantable retinal prosthesis.

Microstructure and Sliding Wear Behaviour of In-Situ TiC-Reinforced Composite Surface Layers Fabricated on Ductile Cast Iron by Laser Alloying.

PubMed

Janicki, Damian

2018-01-05

TiC-reinforced composite surface layers (TRLs) on a ductile cast iron EN-GJS-700-2 grade (DCI) substrate were synthesized using a diode laser surface alloying with a direct injection of titanium powder into the molten pool. The experimental results were compared with thermodynamic calculations. The TRLs having a uniform distribution of the TiC particles and their fraction up to 15.4 vol % were achieved. With increasing titanium concentration in the molten pool, fractions of TiC and retained austenite increase and the shape of TiC particles changes from cubic to dendritic form. At the same time, the cementite fraction decreases, lowering the overall hardness of the TRL. A good agreement between experimental and calculated results was achieved. Comparative dry sliding wear tests between the as-received DCI, the TRLs and also laser surface melted layers (SMLs) have been performed following the ASTM G 99 standard test method under contact pressures of 2.12 and 4.25 MPa. For both the as-received DCI and the SMLs, the wear rates increased with increasing contact pressure. The TRLs exhibited a significantly higher wear resistance than the others, which was found to be load independent.

Microstructure and Sliding Wear Behaviour of In-Situ TiC-Reinforced Composite Surface Layers Fabricated on Ductile Cast Iron by Laser Alloying

PubMed Central

Janicki, Damian

2018-01-01

TiC-reinforced composite surface layers (TRLs) on a ductile cast iron EN-GJS-700-2 grade (DCI) substrate were synthesized using a diode laser surface alloying with a direct injection of titanium powder into the molten pool. The experimental results were compared with thermodynamic calculations. The TRLs having a uniform distribution of the TiC particles and their fraction up to 15.4 vol % were achieved. With increasing titanium concentration in the molten pool, fractions of TiC and retained austenite increase and the shape of TiC particles changes from cubic to dendritic form. At the same time, the cementite fraction decreases, lowering the overall hardness of the TRL. A good agreement between experimental and calculated results was achieved. Comparative dry sliding wear tests between the as-received DCI, the TRLs and also laser surface melted layers (SMLs) have been performed following the ASTM G 99 standard test method under contact pressures of 2.12 and 4.25 MPa. For both the as-received DCI and the SMLs, the wear rates increased with increasing contact pressure. The TRLs exhibited a significantly higher wear resistance than the others, which was found to be load independent. PMID:29304001

Activation of Osteoblastic Function on Titanium Surface with Titanium-Doped Hydroxyapatite Nanoparticle Coating: An In Vitro Study.

PubMed

Nakazawa, Masahiro; Yamada, Masahiro; Wakamura, Masato; Egusa, Hiroshi; Sakurai, Kaoru

Titanium-doped hydroxyapatite (TiHA) nanoparticles contain titanium atoms in the hydroxyapatite lattice, which can physicochemically functionalize the titanium surface without modification of the surface topography. This study aimed to evaluate the physicochemical properties of machined or microroughened titanium surfaces coated with TiHA nanoparticles and the functions of osteoblasts cultured on them. Titanium disks with commercially available surface topography, such as machined or sandblasted, large-grit, and acid-etched (SLA) surfaces, were coated with TiHA. The disks with original or TiHA-coated surfaces were evaluated in topography, wettability, and chemical composition. Osteoblastic cells from rat femurs were cultured on the disks and evaluated in proliferation and differentiation. TiHA coating changed from hydrophobicity to hydrophilicity on both machined and SLA surfaces. Calcium and phosphate atoms were detected all over the surface with TiHA coating regardless of the surface topography. However, the considerable change in the inherent surface topographies was not observed on both types of surfaces after TiHA coating. Osteoblastic proliferative activity at day 4 was increased by TiHA coating on both types of surfaces. TiHA coating did not enhance expressions of bone matrix-related genes such as osteocalcin, osteopontin, bone sialoprotein, alkaline phosphatase, and collagen I. However, depositions of collagen, osteocalcin, and calcium in the culture at days 7 and 20 were increased on both types of surface topographies with TiHA coating. TiHA coating enhanced extracellular matrix formation on smooth and microroughened titanium surfaces by increasing osteoblastic proliferative activity without the deterioration of differentiation through hydrophilic and chemical functionalization.

Cytocompatibility of Direct Laser Interference-patterned Titanium Surfaces for Implants.

PubMed

Hartjen, Philip; Nada, Ola; Silva, Thiago Gundelwein; Precht, Clarissa; Henningsen, Anders; Holthaus, Marzellus GROßE; Gulow, Nikolai; Friedrich, Reinhard E; Hanken, Henning; Heiland, Max; Zwahr, Christoph; Smeets, Ralf; Jung, Ole

2017-01-01

In an effort to generate titanium surfaces for implants with improved osseointegration, we used direct laser interference patterning (DLIP) to modify the surface of pure titanium grade 4 of four different structures. We assessed in vitro cytoxicity and cell attachment, as well as the viability and proliferation of cells cultured directly on the surfaces. Attachment of the cells to the modified surfaces was comparably good compared to that of cells on grit-blasted and acid-etched reference titanium surfaces. In concordance with this, viability and proliferation of the cells directly cultured on the specimens were similar on all the titanium surfaces, regardless of the laser modification, indicating good cytocompatibility. Copyright© 2017, International Institute of Anticancer Research (Dr. George J. Delinasios), All rights reserved.

Effect of cathodic polarization on coating doxycycline on titanium surfaces.

PubMed

Geißler, Sebastian; Tiainen, Hanna; Haugen, Håvard J

2016-06-01

Cathodic polarization has been reported to enhance the ability of titanium based implant materials to interact with biomolecules by forming titanium hydride at the outermost surface layer. Although this hydride layer has recently been suggested to allow the immobilization of the broad spectrum antibiotic doxycycline on titanium surfaces, the involvement of hydride in binding the biomolecule onto titanium remains poorly understood. To gain better understanding of the influence this immobilization process has on titanium surfaces, mirror-polished commercially pure titanium surfaces were cathodically polarized in the presence of doxycycline and the modified surfaces were thoroughly characterized using atomic force microscopy, electron microscopy, secondary ion mass spectrometry, and angle-resolved X-ray spectroscopy. We demonstrated that no hydride was created during the polarization process. Doxycycline was found to be attached to an oxide layer that was modified during the electrochemical process. A bacterial assay using bioluminescent Staphylococcus epidermidis Xen43 showed the ability of the coating to reduce bacterial colonization and planktonic bacterial growth. Copyright © 2016 Elsevier B.V. All rights reserved.

Cicada-inspired cell-instructive nanopatterned arrays

NASA Astrophysics Data System (ADS)

Diu, Ting; Faruqui, Nilofar; Sjöström, Terje; Lamarre, Baptiste; Jenkinson, Howard F.; Su, Bo; Ryadnov, Maxim G.

2014-11-01

Biocompatible surfaces hold key to a variety of biomedical problems that are directly related to the competition between host-tissue cell integration and bacterial colonisation. A saving solution to this is seen in the ability of cells to uniquely respond to physical cues on such surfaces thus prompting the search for cell-instructive nanoscale patterns. Here we introduce a generic rationale engineered into biocompatible, titanium, substrates to differentiate cell responses. The rationale is inspired by cicada wing surfaces that display bactericidal nanopillar patterns. The surfaces engineered in this study are titania (TiO2) nanowire arrays that are selectively bactericidal against motile bacteria, while capable of guiding mammalian cell proliferation according to the type of the array. The concept holds promise for clinically relevant materials capable of differential physico-mechanical responses to cellular adhesion.

Cicada-inspired cell-instructive nanopatterned arrays.

PubMed

Diu, Ting; Faruqui, Nilofar; Sjöström, Terje; Lamarre, Baptiste; Jenkinson, Howard F; Su, Bo; Ryadnov, Maxim G

2014-11-20

Biocompatible surfaces hold key to a variety of biomedical problems that are directly related to the competition between host-tissue cell integration and bacterial colonisation. A saving solution to this is seen in the ability of cells to uniquely respond to physical cues on such surfaces thus prompting the search for cell-instructive nanoscale patterns. Here we introduce a generic rationale engineered into biocompatible, titanium, substrates to differentiate cell responses. The rationale is inspired by cicada wing surfaces that display bactericidal nanopillar patterns. The surfaces engineered in this study are titania (TiO2) nanowire arrays that are selectively bactericidal against motile bacteria, while capable of guiding mammalian cell proliferation according to the type of the array. The concept holds promise for clinically relevant materials capable of differential physico-mechanical responses to cellular adhesion.

Comparative evaluation of the three different surface treatments - conventional, laser and Nano technology methods in enhancing the surface characteristics of commercially pure titanium discs and their effects on cell adhesion: An in vitro study.

PubMed

Vignesh; Nayar, Sanjna; Bhuminathan; Mahadevan; Santhosh, S

2015-04-01

The surface area of the titanium dental implant materials can be increased by surface treatments without altering their shape and form, thereby increasing the biologic properties of the biomaterial. A good biomaterial helps in early cell adhesion and cell signaling. In this study, the commercially pure titanium surfaces were prepared to enable machined surfaces to form a control material and to be compared with sandblasted and acid-etched surfaces, laser treated surfaces and titanium dioxide (20 nm) Nano-particle coated surfaces. The surface elements were characterized. The biocompatibility was evaluated by cell culture in vitro using L929 fibroblasts. The results suggested that the titanium dioxide Nano-particle coated surfaces had good osteoconductivity and can be used as a potential method for coating the biomaterial.

Synthesis and characterization of MoS2/Ti composite coatings on Ti6Al4V prepared by laser cladding

NASA Astrophysics Data System (ADS)

Yang, Rongjuan; Liu, Zongde; Wang, Yongtian; Yang, Guang; Li, Hongchuan

2013-02-01

The MoS2/Ti composite coating with sub-micron grade structure has been prepared on Ti6Al4V by laser method under argon protection. The morphology, microstructure, microhardness and friction coefficient of the coating were examined. The results indicated that the molybdenum disulfide was decomposed during melting and resolidification. The phase organization of composite coating mainly consisted of ternary element sulfides, molybdenum sulfides and titanium sulfides. The friction coefficient of and the surface roughness the MoS2/Ti coating were lower than those of Ti6Al4V. The composite coating exhibits excellent adhesion to the substrates, less surface roughness, good wear resistance and harder surface.

Microstructure analysis and wear behavior of titanium cermet femoral head with hard TiC layer.

PubMed

Luo, Yong; Ge, Shirong; Liu, Hongtao; Jin, Zhongmin

2009-12-11

Titanium cermet was successfully synthesized and formed a thin gradient titanium carbide coating on the surface of Ti6Al4V alloy by using a novel sequential carburization under high temperature, while the titanium cermet femoral head was produced. The titanium cermet phase and surface topography were characterized with X-ray diffraction (XRD) and backscattered electron imaging (BSE). And then the wear behavior of titanium cermet femoral head was investigated by using CUMT II artificial joint hip simulator. The surface characterization indicates that carbon effectively diffused into the titanium alloys and formed a hard TiC layer on the Ti6Al4V alloys surface with a micro-porous structure. The artificial hip joint experimental results show that titanium cermet femoral head could not only improve the wear resistance of artificial femoral head, but also decrease the wear of UHMWPE joint cup. In addition, the carburized titanium alloy femoral head could effectively control the UHMWPE debris distribution, and increase the size of UHMWPE debris. All of the results suggest that titanium cermet is a prospective femoral head material in artificial joint.

Adsorption performance of titanium dioxide (TiO2) coated air filters for volatile organic compounds.

PubMed

Zhong, Lexuan; Lee, Chang-Seo; Haghighat, Fariborz

2012-12-01

The photocatalytic oxidation (PCO) technology as an alternative method for air purification has been studied for decades and a variety of PCO models indicate that the adsorption of reactants on the catalyst surface is one of the major physical and chemical processes occurring at a heterogeneous photocatalytic reaction. However, limited study explored the adsorption effect of a photocatalyst. This study carried out a systematic evaluation of adsorption performance of titanium dioxide (TiO(2)) coated fiberglass fibers (FGFs), TiO(2) coated carbon cloth fibers (CCFs), and original CCFs air filters at various relative humidity conditions for nine volatile organic compounds. TiO(2)/FGFs, TiO(2)/CCFs, and CCFs were characterized by SEM for morphology and N(2) adsorption isotherm for BET surface area and pore structure. A bench-scale adsorption test setup was constructed and adsorption tests were performed at various relative humidity conditions and four different injected concentrations for each compound. The isothermal adsorption curves at low concentration levels were obtained and they were well described by Langmuir isotherm model. It was noticed that there were significant differences between the adsorption behaviors and photocatalytic activities of TiO(2)/FGFs and TiO(2)/CCFs. It was concluded that adsorption performance is closely related to the characteristics of substrates and therefore, the development of a substrate with high adsorption ability is a promising trend for improving the performance of the UV-PCO technology. Copyright © 2012 Elsevier B.V. All rights reserved.

Study of nitrogen ion doping of titanium dioxide films

NASA Astrophysics Data System (ADS)

Ramos, Raul; Scoca, Diego; Borges Merlo, Rafael; Chagas Marques, Francisco; Alvarez, Fernando; Zagonel, Luiz Fernando

2018-06-01

This study reports on the properties of nitrogen doped titanium dioxide (TiO2) thin films considering the application as a transparent conducting oxide (TCO). Sets of thin films were prepared by sputtering a titanium target under oxygen atmosphere on a quartz substrate at 400 or 500 °C. Films were then doped at the same temperature by 150 eV nitrogen ions. The films were prepared in Anatase phase which was maintained after doping. Up to 30 at% nitrogen concentration was obtained at the surface, as determined by in situ X-ray photoelectron spectroscopy (XPS). Such high nitrogen concentration at the surface lead to nitrogen diffusion into the bulk which reached about 25 nm. Hall measurements indicate that average carrier density reached over 1019 cm-3 with mobility in the range of 0.1-1 cm2 V-1 s-1. Resistivity about 3 · 10-1 Ω cm could be obtained with 85% light transmission at 550 nm. These results indicate that low energy implantation is an effective technique for TiO2 doping that allows an accurate control of the doping process independently from the TiO2 preparation. Moreover, this doping route seems promising to attain high doping levels without significantly affecting the film structure. Such approach could be relevant for preparation of N:TiO2 transparent conducting electrodes (TCE).

Morphological Observations of Mesenchymal Stem Cell Adhesion to a Nanoperiodic-Structured Titanium Surface Patterned Using Femtosecond Laser Processing

NASA Astrophysics Data System (ADS)

Oya, Kei; Aoki, Shun; Shimomura, Kazunori; Sugita, Norihiko; Suzuki, Kenji; Nakamura, Norimasa; Fujie, Hiromichi

2012-12-01

It is known that the adhesive and anisotropic properties of cell-derived biomaterials are affected by micro- or nanoscale structures processed on culture surfaces. In the present study, the femtosecond laser processing technique was used to scan a laser beam at an intensity of approximately the ablation threshold level on a titanium surface for nanoscale processing. Microscopy observation revealed that the processed titanium exhibited a periodic-patterned groove structure at the surface; the width and depth of the groove were 292 ±50 and 99 ±31 nm, respectively, and the periodic pitch of the groove was 501 ±100 nm. Human synovium-derived mesenchymal stem cells were cultured on the surface at a cell density of 3.0×103 cells/cm2 after 4 cell passages. For comparison, the cells were also cultured on a nonprocessed titanium surface under the condition identical to that of the processed surface. Results revealed that the duration for cell attachment to the surface was markedly reduced on the processed titanium as compared with the nonprocessed titanium. Moreover, on the processed titanium, cell extension area significantly increased while cell orientation was aligned along the direction of the periodic grooves. These results suggest that the femtosecond laser processing improves the adhesive and anisotropic properties of cells by producing the nanoperiodic structure on titanium culture surfaces.

Laser engravings as reason for mechanical failure of titanium-alloyed total hip stems.

PubMed

Kluess, Daniel; Steinhauser, Erwin; Joseph, Micheal; Koch, Ursula; Ellenrieder, Martin; Mittelmeier, Wolfram; Bader, Rainer

2015-07-01

Two revisions of broken β-titanium total hip stems had to be performed in our hospital after 2 and 4 years in situ. Since both fractures were located at the level of a laser engraving, a failure analysis was conducted. Both retrieved hip stems were disinfected and collected in our retrieval database after patient's signed agreement. Each fragment was macroscopically photographed. Fracture surfaces were analyzed using scanning electron microscopy (SEM). Quantification of element content was conducted using energy dispersive X-ray (EDX) analysis. Both stems show fatigue fracture, as displayed by the lines of rest on the fracture surface. The origin of fracture was identified directly at the laser engraving of the company logo at both stems by means of SEM. The EDX analysis showed an oxygen level beneath the laser engraving about twice as high as in the substrate, causing material embrittlement. Laser engravings need to be reduced to a minimum of necessary information, and should be placed at locations with minimum mechanical load. Biomechanical analyses are recommended to identify less loaded areas in implant components to avoid such implant failures.

Sodium Aluminate Concentration Effects on Microstructure and Corrosion Behavior of the Plasma Electrolytic Oxidation Coatings on Pure Titanium

NASA Astrophysics Data System (ADS)

Molaei, Maryam; Fattah-Alhosseini, Arash; Gashti, Seyed Omid

2018-01-01

Sodium aluminate (NaAlO2) concentration was varied in order to understand the influence of the chemical composition of electrolyte on the spark characteristics, microstructure, and corrosion behavior of plasma electrolytic oxidation (PEO) coatings. For this purpose, PEO coatings were formed on the pure titanium substrate surface using solutions of four diverse sodium aluminate concentrations (6, 8, 10, and 12 g/L). The PEO process was carried out at constant time and voltage (180 seconds and 420 V). Studying the microstructures of samples by scanning electron microscope (SEM) and their corrosion behavior in 3.5 wt pct NaCl solutions indicated that the increase in NaAlO2 concentration (up to 10 g/L) led to an increase in uniformity and compactness, thus decreasing the size of micro-pores and increment of corrosion resistance. However, at a certain level of NaAlO2 concentration (12 g/L), large and severe sparks were created on the surface of the sample during the process, worsening the corrosion resistance and microstructure of coating.

Enhanced human bone marrow mesenchymal stem cell functions on cathodic arc plasma-treated titanium

PubMed Central

Zhu, Wei; Teel, George; O’Brien, Christopher M; Zhuang, Taisen; Keidar, Michael; Zhang, Lijie Grace

2015-01-01

Surface modification of titanium for use in orthopedics has been explored for years; however, an ideal method of integrating titanium with native bone is still required to this day. Since human bone cells directly interact with nanostructured extracellular matrices, one of the most promising methods of improving titanium’s osseointegration involves inducing bio-mimetic nanotopography to enhance cell–implant interaction. In this regard, we explored an approach to functionalize the surface of titanium by depositing a thin film of textured titanium nanoparticles via a cathodic arc discharge plasma. The aim is to improve human bone marrow mesenchymal stem cell (MSC) attachment and differentiation and to reduce deleterious effects of more complex surface modification methods. Surface functionalization was analyzed by scanning electron microscopy, atomic force microscopy, contact angle testing, and specific protein adsorption. Scanning electron microscopy and atomic force microscopy examination demonstrate the deposition of titanium nanoparticles and the surface roughness change after coating. The specific fibronectin adsorption was enhanced on the modified titanium surface that associates with the improved hydrophilicity. MSC adhesion and proliferation were significantly promoted on the nanocoated surface. More importantly, compared to bare titanium, greater production of total protein, deposition of calcium mineral, and synthesis of alkaline phosphatase were observed from MSCs on nanocoated titanium after 21 days. The method described herein presents a promising alternative method for inducing more cell favorable nanosurface for improved orthopedic applications. PMID:26677327

Electrophoretic deposition of silicon substituted hydroxyapatite coatings from n-butanol-chloroform mixture.

PubMed

Xiao, Xiu Feng; Liu, Rong Fang; Tang, Xiao Lian

2008-01-01

Silicon Substituted Hydroxyapatite (Si-HA) coatings were prepared on titanium substrates by electrophoretic deposition (EPD). The stability of Si-HA suspension in n-butanol and chloroform mixture has been studied by electricity conductivity and sedimentation test. The microstructure, shear strength and bioactivity in vitro has been tested. The stability of Si-HA suspension containing n-butanol and chloroform mixture as medium is better than that of pure n-butanol as medium. The good adhesion of the particles with the substrate and good cohesion between the particles were obtained in n-butanol and chloroform mixture. Adding triethanolamine (TEA) as additive into the suspension is in favor of the formation of uniform and compact Si-HA coatings on the titanium substrates by EPD. The shear strength of the coatings can reach 20.43 MPa after sintering at 700 degrees C for 2 h, when the volume ratio of n-butanol: chloroform is 2:1 and the concentration of TEA is 15 ml/L. Titanium substrates etched in H(2)O(2)/NH(3) solution help to improve the shear strength of the coatings. After immersion in simulated body fluid for 7 days, Si-HA coatings have the ability to induce the bone-like apatite formation.

Diamond Composite Films for Protective Coatings on Metals and Method of Formation

NASA Technical Reports Server (NTRS)

Ong, Tiong P. (Inventor); Shing, Yuh-Han (Inventor)

1997-01-01

Composite films consisting of diamond crystallites and hard amorphous films such as diamond-like carbon, titanium nitride, and titanium oxide are provided as protective coatings for metal substrates against extremely harsh environments. A composite layer having diamond crystallites and a hard amorphous film is affixed to a metal substrate via an interlayer including a bottom metal silicide film and a top silicon carbide film. The interlayer is formed either by depositing metal silicide and silicon carbide directly onto the metal substrate, or by first depositing an amorphous silicon film, then allowing top and bottom portions of the amorphous silicon to react during deposition of the diamond crystallites, to yield the desired interlayer structure.

Comparative study of ITO and TiN fabricated by low-temperature RF biased sputtering

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simon, Daniel K., E-mail: daniel.simon@namlab.com; Schenk, Tony; Dirnstorfer, Ingo

2016-03-15

Radio frequency (RF) biasing induced by a second plasma source at the substrate is applied to low-temperature sputtering processes for indium tin oxide (ITO) and titanium nitride (TiN) thin films. Investigations on crystal structure and surface morphology show that RF-biased substrate plasma processes result in a changed growth regime with different grain sizes and orientations than those produced by processes without a substrate bias. The influence of the RF bias is shown comparatively for reactive RF-sputtered ITO and reactive direct-current-sputtered TiN. The ITO layers exhibit an improved electrical resistivity of 0.5 mΩ cm and an optical absorption coefficient of 0.5 × 10{sup 4 }cm{supmore » −1} without substrate heating. Room-temperature sputtered TiN layers are deposited that possess a resistivity (0.1 mΩ cm) of 3 orders of magnitude lower than, and a density (5.4 g/cm{sup 3}) up to 45% greater than, those obtained from layers grown using the standard process without a substrate plasma.« less

The comparison of phosphate-titanate-silicate layers on the titanium and Ti6Al4V alloy base.

PubMed

Rokita, M

2011-08-15

The studied layers were composed of two parts: titanate-silicate underlayer for better adhesion and titanate-phosphate-silicate layers for potential bioparameters. The layers with different amounts of hydroxyapatite were deposited on titanium and Ti6Al4V alloy substrates using dipping sol-gel method and electrophoresis. The selection of sol/suspension composition, deposition time and heat treatment conditions have the decisive influence on the layers parameters. The obtained layers should be very thin and almost amorphous. The specific nature of ceramic layers on the metal substrates excludes the use of some measurements methods or makes it difficult to interpret the measurement results. All the obtained samples were compared using XRD analysis data (GID technique), SEM with EDX measurements and FTIR spectroscopy (transmission and reflection techniques) before and after soaking in simulated body fluid. FTIR spectroscopy with mathematical treatment of the spectra (BIO-RAD Win-IR program, Arithmetic-subtract function) was used to detect the increase or decrease of any phosphate phases during SBF soaking. Based on the FTIR results the processes of hydroxyapatite (HAp) growth or layer dissolution were estimated. The layers deposited on titanium substrate are more crystalline then the ones deposited on Ti6Al4V. During SBF soaking process the growth of small amount of microcrystalline carbonate hydroxyapatite was observed on titanium substrate. The layer on Ti6Al4V base contained amorphous carbonate apatite. During heating treatment above about 870-920 K this apatite transforms into carbonate hydroxyapatite. The Ti6Al4V substrate seems to be more advantageous in context of potentially bioactive materials obtaining. Copyright © 2010 Elsevier B.V. All rights reserved.

Lateral and axial cutting efficiency of instruments manufactured with conventional nickel-titanium and novel gold metallurgy.

PubMed

Vasconcelos, R A; Arias, A; Peters, O A

2018-05-01

To isolate the effect of metallurgy in lateral and axial cutting efficacy against plastic and bovine dentine substrates by comparing two rotary systems with identical design but manufactured with either conventional nickel-titanium or heat-treated gold alloy. A total of 258 ProTaper Universal (PTU) and ProTaper Gold (PTG) Shaping instruments were used. Bending behaviour was assessed to determine the appropriate displacement associated with a 2 N force in lateral cutting. Ten instruments of each type were used in lateral action for 60 s against bovine dentine or plastic substrates four consecutive times producing four notches in each specimen. Ten further instruments of each type were used in on axial action in four standardized simulated root canals fabricated from 4-mm thick plastic or dentine discs. Both tests were performed at 300 rpm in a computer-controlled testing platform. Notch area and torsional load were compared with Student's t-tests. Repeated measures ANOVA was used to compare cutting efficiency across the four different time-points. Pearson correlation coefficients between substrates were also determined. For lateral action, all three PTG instruments cut significantly more effectively (P < 0.05) than PTU on the plastic substrate. S1 and S2 PTG cut significantly more after 120 and 180 s (P < 0.05) on bovine dentine substrate. For axial action, S1 and S2 PTG were significantly more efficient in cutting at 180 s on plastic and 120 s on bovine dentine (P < 0.05). Instruments made from heat-treated nickel-titanium gold alloy had equal or greater cutting efficiency when compared to those made from conventional nickel-titanium. © 2017 International Endodontic Journal. Published by John Wiley & Sons Ltd.

The comparison of phosphate-titanate-silicate layers on the titanium and Ti6Al4V alloy base

NASA Astrophysics Data System (ADS)

Rokita, M.

2011-08-01

The studied layers were composed of two parts: titanate-silicate underlayer for better adhesion and titanate-phosphate-silicate layers for potential bioparameters. The layers with different amounts of hydroxyapatite were deposited on titanium and Ti6Al4V alloy substrates using dipping sol-gel method and electrophoresis. The selection of sol/suspension composition, deposition time and heat treatment conditions have the decisive influence on the layers parameters. The obtained layers should be very thin and almost amorphous. The specific nature of ceramic layers on the metal substrates excludes the use of some measurements methods or makes it difficult to interpret the measurement results. All the obtained samples were compared using XRD analysis data (GID technique), SEM with EDX measurements and FTIR spectroscopy (transmission and reflection techniques) before and after soaking in simulated body fluid. FTIR spectroscopy with mathematical treatment of the spectra (BIO-RAD Win-IR program, Arithmetic-subtract function) was used to detect the increase or decrease of any phosphate phases during SBF soaking. Based on the FTIR results the processes of hydroxyapatite (HAp) growth or layer dissolution were estimated. The layers deposited on titanium substrate are more crystalline then the ones deposited on Ti6Al4V. During SBF soaking process the growth of small amount of microcrystalline carbonate hydroxyapatite was observed on titanium substrate. The layer on Ti6Al4V base contained amorphous carbonate apatite. During heating treatment above about 870-920 K this apatite transforms into carbonate hydroxyapatite. The Ti6Al4V substrate seems to be more advantageous in context of potentially bioactive materials obtaining.

Particles induced surface nanoroughness of titanium surface and its influence on adhesion of osteoblast-like MG-63 cells

NASA Astrophysics Data System (ADS)

Solař, P.; Kylián, O.; Marek, A.; Vandrovcová, M.; Bačáková, L.; Hanuš, J.; Vyskočil, J.; Slavínská, D.; Biederman, H.

2015-01-01

Titanium is one of the most common materials employed for production of implants, which is due to its good biocompatibility. However, the colonization of titanium surface by osteoblast cells may be influenced by its roughness and therefore precise control of roughness of titanium surface as well as identification of its optimal value for growth of cells is of high importance. In this study the nanorough titanium surfaces were prepared on polished disks of TiAlV by two step method of deposition. In the first step TiAlV were coated by nanoparticles generated by gas aggregation sources. Such prepared films of nanoparticles were subsequently covered with a titanium overlayer. Different values of surface roughness in the range 1-100 nm were achieved by variation of the size and number of the nanoparticles. Such prepared surfaces were subsequently used for investigation of influence of roughness of titanium surfaces on the adhesion of human osteoblast-like MG-63 cells. It was found out that 7 days after seeding the highest number of adhering cells was observed for samples with root-mean-square roughness of 30 nm.

Synergistic responses of superficial chemistry and micro topography of titanium created by wire-type electric discharge machining.

PubMed

Kataoka, Yu; Tamaki, Yukimichi; Miyazaki, Takashi

2011-01-01

Wire-type electric discharge machining has been applied to the manufacture of endosseous titanium implants as this computer associated technique allows extremely accurate complex sample shaping with an optimal micro textured surface during the processing. Since the titanium oxide layer is sensitively altered by each processing, the authors hypothesized that this technique also up-regulates biological responses through the synergistic effects of the superficial chemistry and micro topography. To evaluate the respective in vitro cellular responses on the superficial chemistry and micro topography of titanium surface processed by wire-type electric discharge, we used titanium-coated epoxy resin replica of the surface. An oxide layer on the titanium surface processed by wire-type electric discharge activated the initial responses of osteoblastic cells through an integrin-mediated mechanism. Since the mRNA expression of ALP on those replicas was up-regulated compared to smooth titanium samples, the micro topography of a titanium surface processed by wire-type electric discharge promotes the osteogenic potential of cells. The synergistic response of the superficial chemistry and micro topography of titanium processed by wire-type electric discharge was demonstrated in this study.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clausing, R.E.

Results are summarized for an investigation of the sorption rates of gases on vapor-deposited titanium films. The usefulness of such films for ultrahigh speed vacuum pumping is appraised. The sorption of hydrogen, deuterium, oxygen, nitrogen, carbon monoxide, carbon dioxide, water vapor, helium, argon, and methane onto titanium films was measured for a variety of circumstances using techniques and apparatus developed for this specific purpose. The information obtained and techniques evolved in this study have shown that large-scale getter pumping is feasible and can be a very effective means of pumping many gases. Sticking fractions larger than 0.8 were obtained formore » hydrogen, deuterium, oxygen, nitrogen, carbon monoxide, and carbon dioxide. The experiments have shown that the sticking fraction for gases on vapor-deposited films is a function of the deposition conditions. There is strong evidence to support the supposition that conditions which favor the formation of a porous, fine-grained film structure with a large surface-to-volume ratio produce films with the highest sorption rates. The technique for measuring sticking fractions is new and in many respects unique. It utilizes a very large sorption surface, thus minimizing the perturbing effect of the instrumentation and evaporation apparatus and reducing the hazard of film contamination due to small leaks in the system or outgassing of system components. The method gives especially good accuracy for measurements of sticking fractions approaching unity. The quantity of gas adsorbed, the gas flux onto the getter surface, and the gas flux leaving the getter surface are measured directly. Any two of these three independent measurements can be used to determine the sticking fraction, thereby providing a means of checking the data. The evaporation techniques, substrate surface, and substrate area were chosen to very nearly duplicate the conditions likely to be encountered in the practical application of large-scale getter pumping. (auth)« less

Surface Modifications and Their Effects on Titanium Dental Implants

PubMed Central

Jemat, A.; Ghazali, M. J.; Razali, M.; Otsuka, Y.

2015-01-01

This review covers several basic methodologies of surface treatment and their effects on titanium (Ti) implants. The importance of each treatment and its effects will be discussed in detail in order to compare their effectiveness in promoting osseointegration. Published literature for the last 18 years was selected with the use of keywords like titanium dental implant, surface roughness, coating, and osseointegration. Significant surface roughness played an important role in providing effective surface for bone implant contact, cell proliferation, and removal torque, despite having good mechanical properties. Overall, published studies indicated that an acid etched surface-modified and a coating application on commercial pure titanium implant was most preferable in producing the good surface roughness. Thus, a combination of a good surface roughness and mechanical properties of titanium could lead to successful dental implants. PMID:26436097

Light and transmission electron microscopy of the intact interfaces between non-submerged titanium-coated epoxy resin implants and bone or gingiva.

PubMed

Listgarten, M A; Buser, D; Steinemann, S G; Donath, K; Lang, N P; Weber, H P

1992-02-01

This experiment was aimed at studying the intact tissue/implant interface of non-submerged dental implants with a titanium surface. Epoxy-resin replicas were fabricated from 3.05 x 8 mm cylindrical titanium implants with a plasma-sprayed apical portion and a smooth coronal collar. The replicas were coated with a 90-120-nm-thick layer of pure titanium and autoclaved. The coated replicas were inserted as non-submerged endosseous implants in the edentulous premolar region of dog mandibles and allowed to heal for three months. Jaw sections containing the implants were processed for light and electron microscopic study of the intact tissue/implant interface with and without prior demineralization. Gingival connective tissue fibers were closely adapted to the titanium layer, in an orientation more or less parallel to the implant surface. There was no evidence of any fiber insertions into the surface irregularities of the smooth or rough titanium surface. Undemineralized bone was intimately adapted to the titanium surface without any intervening space. In demineralized sections, the collagen fibers of the bone matrix tended to be somewhat thinner and occasionally less densely packed in the vicinity of the implant surface. However, they extended all the way to the titanium surface, without any intervening fibril-free layer.

Synthesis of transparent BaTiO3 nanoparticle/polymer composite film using DC field

NASA Astrophysics Data System (ADS)

Kondo, Yusuke; Okumura, Yasuko; Oi, Chifumi; Sakamoto, Wataru; Yogo, Toshinobu

2008-10-01

Transparent BaTiO3 nanoparticle/polymer composite films were synthesized from titanium-organic film and barium ion in aqueous solution under direct current (DC) field. Titanium-organic precursor was synthesized from titanium isopropoxide, acetylacetone and methacrylate derivative. The UV treatment was effective to increase the anti-solubility of the titanium-organic film during DC processing. BaTiO3 nanoparticles were crystallized in the precursor films on stainless substrates without high temperature process, as low as 40°C. The crystallite size of BaTiO3 increased with increasing reaction temperature from 40 to 50 °C at 3.0 V/cm. BaTiO3 nanoparticles also grew in size with increasing reaction time from 15 min to 45 min at 3.0 V/cm and 50 °C. Transparent BaTiO3 nanoparticle/polymer films were synthesized on stainless substrates at 3.0 V/cm and 50°C for 45 min.

Modification of electrochemically deposited apatite using supercritical water.

PubMed

Ban, S; Hasegawa, J

2001-12-01

Supercritical water was used as a modification method of electrochemically deposited apatite on pure titanium. The apatites were coated on a commercially pure titanium plate using a hydrothermal-electrochemical method. A constant direct current at 12.5 mA/cm2 was loaded for 1 hr at 25, 60, 100, 150 and 200 degrees C in an electrolyte containing calcium and phosphate ions. The deposited apatite on the titanium substrate was stored in supercritical water at 450 degrees C under 45 MPa for 8 hr. With this treatment, the crystallinity of the apatites increased, sharp edges of the deposited apatites were rounded off, and the bonding strength of the titanium substrate to the deposited apatites significantly increased. On the other hand, weight loss in 0.01 N HCl decreased and the weight gain rate in a simulated body fluid also decreased with this treatment. It is suggested that the modification using supercritical water improved the mechanical strength of the deposited apatite, but worsened its bioactivity.

A novel bifunctional Ni-doped TiO2 inverse opal with enhanced SERS performance and excellent photocatalytic activity

NASA Astrophysics Data System (ADS)

Li, Xuehong; Wu, Yun; Shen, Yuhua; Sun, Yan; Yang, Ying; Xie, Anjian

2018-01-01

Three-dimensional inverse opal photonic microarray (IOPM) structure exhibits good qualities in structural regularity and interconnectivity, such as high specific surface area, large pore volume, uniform pore size, and ordered periodic construction. Here, a novel nickel-doped titanium dioxide IOPM (Ni-TiO2 IOPM) was fabricated for the first time as a bifunctional material for the applications of surface-enhanced Raman scattering (SERS) substrate and photocatalyst. The Ni doping could change the defect concentration of the substrate to enhance the SERS effect, and could increase the light absorption of the substrate in visible region. The synergistic effect of Ni doping and the periodically ordered porous structure enhanced both SERS sensitivity and photocatalytic activity. As a SERS substrate, the Ni-TiO2 IOPM exhibited highly sensitive detection capability for 4-mercaptobenzoic acid (4-MBA) at a concentration as low as 1 × 10-11 M. Under simulated sunlight, about 95% of the methylene blue (MB) was degraded within 90 min when Ni-TiO2 IOPM was used as the photocatalytst. The Ni-TiO2 IOPM prepared in this work may be a promising bifunctional SERS substrate candidate for organic sewage detection and environment protection. In addition, the fabrication strategy can be extended to synthesize other nanomaterials with orderly and porous structure.

Titanium Dioxide Coatings Sprayed by a Water-Stabilized Plasma Gun (WSP) with Argon and Nitrogen as the Powder Feeding Gas: Differences in Structural, Mechanical and Photocatalytic Behavior

NASA Astrophysics Data System (ADS)

Ctibor, P.; Pala, Z.; Sedláček, J.; Štengl, V.; Píš, I.; Zahoranová, T.; Nehasil, V.

2012-06-01

Titanium dioxide coatings were sprayed by a water-stabilized plasma gun to form robust self-supporting bodies with a photocatalytically active surface. Agglomerated nanometric powder was used as a feedstock. In one case argon was used as a powder-feeding as well as coating-cooling gas whereas in the other case nitrogen was used. Stainless steel was used as a substrate and the coatings were released after the cooling. Over one millimeter thick self-supporting bodies were studied by XRD, HR-TEM, XPS, Raman spectroscopy, UV-VIS spectrophotometry and photocatalytic tests. Selected tests were done at the surface as well as at the bottom side representing the contact surface with the substrate during the spray process. Porosity was studied by image analysis on polished cross sections where also microhardness was measured. The dominant phase present in the sprayed samples was rutile, whereas anatase was only a minor component. The hydrogen content in the nitrogen-assisted coating was higher, but the character of the optical absorption edge remained the same for both samples. Photoelectron spectroscopy revealed differences in the character of the O1s peak between both samples. The photocatalytic activity was tested by decomposition of acetone at UV illumination, whereas also the end products—CO and CO2—were monitored. The nitrogen-assisted coating was revealed as a more efficient photocatalyst. Certain aspects of a thermal post-treatment on the coatings are discussed as well. Color and electrical conductivity are markedly changed at annealing at 760 °C, whereas only very small changes of the as-sprayed coating character correspond to annealing at 500 °C.

Characterization of N3 dye adsorption on TiO2 using quartz-crystal microbalance with dissipation monitoring

NASA Astrophysics Data System (ADS)

Wayment-Steele, Hannah K.; Johnson, Lewis E.; Dixon, Matthew C.; Johal, Malkiat S.

2013-09-01

Understanding the kinetics of dye adsorption on semiconductors is crucial for designing dye-sensitized solar cells (DSSCs) with enhanced efficiency. Harms et al. recently applied the Quartz-Crystal Microbalance with Dissipation Monitoring (QCM-D) to study in situ dye adsorption on flat TiO2 surfaces. QCM-D measures adsorption in real time and therefore allows one to determine the kinetics of the process. In this work, we characterize the adsorption of N3, a commercial RuBipy dye, using the native oxide layer of a titanium sensor to simulate the TiO2 substrate of a DSSC. We report equilibrium constants that are in agreement with previous absorbance studies of N3 adsorption, and therefore demonstrate the native oxide layer of a titanium sensor as a valid and readily available planar TiO2 morphology to study dye adsorption.

Deposition of TiOxNy Thin Films with Various Nitrogen Flow Rate:. Growth Behavior and Structural Properties

NASA Astrophysics Data System (ADS)

Cho, S.-J.; Jung, C.-K.; Bae, I.-S.; Song, Y.-H.; Boo, J.-H.

2011-06-01

We have deposited TiOxNy thin films on Si(100) substrates at 500 °C using RF PECVD system. Titanium iso-propoxide was used as precursor with different nitrogen flow rate to control oxygen and nitrogen contents in the films. Changes of chemical states of constituent elements in the deposited films were examined by XPS analysis. The data showed that with increasing nitrogen flow rate, the total amounts of nitrogen and titanium were increased while that of oxygen was decreased, resulting in a binding energy shift toward high energy side. The characteristics of film growth orientation and structure as well as morphology change behavior were also analyzed by XRD, TED, FT-IR, TEM, and SEM. Deposition at higher nitrogen flow rate results in finer clusters with a nanograin size and more effective photocatalytic TiOxNy thin films with hydrophilic surface.

The recognition and interpretation of micro-particle impacts on space craft surfaces

NASA Astrophysics Data System (ADS)

Kearsley, Anton

Modern analysis instruments now allow the rapid examination of returned spacecraft surfaces, enabling the location and identification of impact features, and the attribution of their impactor origins. This paper describes application of novel electron, ion and micro-X-ray Fluorescence techniques to impacts on diverse compositions of substrate, including solar cell glass, poly-sulfone and fluoro-polymer-impregnated glass fibre composites, multilayer insulation foils, aluminium and titanium alloys. Examples will include two generations of solar cells and stiffener materials from the Hubble Space Telescope (HST), Beta-cloth from the NASA Mir-Trek cover blanket, aluminised Kapton foils from the Japanese Space Flyer Unit (SFU) and the European Retrievable Carrier (EuReCa), Al-alloy plates from the Long Duration Exposure Facility (LDEF), Al foils from the NASA Stardust mission, Al-alloy and Zinc orthotitanate (ZOT) painted alloy plate from HST, and titanium alloys from a re-entered titanium pressure tank. Each type of spacecraft surface poses unique problems of analysis, especially in the recognition of extraneous signatures from the impacting particle, especially if a complex chemical composition is already present in the target. For example, solar cells provide an excellent capture and analysis medium for monitoring fluxes of micrometre-scale orbital debris from solid rocket motor firings in low Earth orbit. However, they provide a hard and dense capture medium upon which substantial modification of the impactor may occur, making the precise identification of micrometeoroid components difficult. Unfortunately, extensive spallation by larger (> 100 micrometre) particle impacts on the thin and brittle structure of solar cells also usually results in complete loss of impactor signature. Although thick alloy surfaces may prevent complete impact penetration, the analysis of particle residues within their deep concavity has proven difficult, until the recent introduction of new high-efficiency energy dispersive X-ray (EDX) detectors. Along with Particle Induced X-ray Emission and micro-XRF imaging systems, the new EDX detectors allow recognition of subtle trace quantities of residue from even millimetre-scale craters and thin foil penetrations. Data from these differing substrates and techniques need to be integrated if we are to fully document micro-particle populations from the wide range of natural (cometary and asteroidal, i.e. micrometeoroid) and artificial (i.e. orbital debris) sources.

Effect of applied voltage on surface properties of anodised titanium in mixture of β-glycerophosphate (β-GP) and calcium acetate (CA)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chuan, Lee Te, E-mail: gd130079@siswa.uthm.edu.my; Rathi, Muhammad Fareez Mohamad, E-mail: cd110238@siswa.uthm.edu.my; Abidin, Muhamad Yusuf Zainal, E-mail: cd110221@siswa.uthm.edu.my

Anodic oxidation is a surface modification method which combines electric field driven metal and oxygen ion diffusion for formation of oxide layer on the anode surface. This method has been widely used to modify the surface morphology of biomaterial especially titanium. This study aimed to investigate the effect of applied voltage on titanium. Specifically, the titanium foil was anodised in mixture of β-glycerophosphate disodium salt pentahydrate (β-GP) and calcium acetate monohydrate (CA) with different applied voltage (50-350 V), electrolyte concentration (0.04 M β-GP + 0.4 M CA), anodising time (10minutes) and current density (50 and 70 mA.cm{sup −2}) at room temperature. Surfacemore » oxide properties of anodised titanium were characterised by digital single-lens reflex camera (DSLR camera), field emission scanning electron microscope (FESEM) and atomic force microscopy (AFM). At lower applied voltage (≤150 V), surface of titanium foils were relatively smooth. With increasing applied voltage (≥250 V), the oxide layer became more porous and donut-shaped pores were formed on the surface of titanium foils. The AFM results indicated that the surface roughness of anodised titanium increases with increasing of applied voltage. The porous and rough surface is able to promote the osseointegration and reduce the suffering time of patient.« less

Laser-modified titanium surfaces enhance the osteogenic differentiation of human mesenchymal stem cells.

PubMed

Bressel, Tatiana A B; de Queiroz, Jana Dara Freires; Gomes Moreira, Susana Margarida; da Fonseca, Jéssyca T; Filho, Edson A; Guastaldi, Antônio Carlos; Batistuzzo de Medeiros, Silvia Regina

2017-11-28

Titanium surfaces have been modified by various approaches with the aim of improving the stimulation of osseointegration. Laser beam (Yb-YAG) treatment is a controllable and flexible approach to modifying surfaces. It creates a complex surface topography with micro and nano-scaled patterns, and an oxide layer that can improve the osseointegration of implants, increasing their usefulness as bone implant materials. Laser beam irradiation at various fluences (132, 210, or 235 J/cm 2 ) was used to treat commercially pure titanium discs to create complex surface topographies. The titanium discs were investigated by scanning electron microscopy, X-ray diffraction, and measurement of contact angles. The surface generated at a fluence of 235 J/cm 2 was used in the biological assays. The behavior of mesenchymal stem cells from an umbilical cord vein was evaluated using a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay, a mineralization assay, and an alkaline phosphatase activity assay and by carrying out a quantitative real-time polymerase chain reaction for osteogenic markers. CHO-k1 cells were also exposed to titanium discs in the MTT assay. The best titanium surface was that produced by laser beam irradiation at 235 J/cm 2 fluence. Cell proliferation analysis revealed that the CHO-k1 and mesenchymal stem cells behaved differently. The laser-processed titanium surface increased the proliferation of CHO-k1 cells, reduced the proliferation of mesenchymal stem cells, upregulated the expression of the osteogenic markers, and enhanced alkaline phosphatase activity. The laser-treated titanium surface modulated cellular behavior depending on the cell type, and stimulated osteogenic differentiation. This evidence supports the potential use of laser-processed titanium surfaces as bone implant materials, and their use in regenerative medicine could promote better outcomes.

Nanoscale Visualization of Elastic Inhomogeneities at TiN Coatings Using Ultrasonic Force Microscopy

NASA Astrophysics Data System (ADS)

Hidalgo, J. A.; Montero-Ocampo, C.; Cuberes, M. T.

2009-12-01

Ultrasonic force microscopy has been applied to the characterization of titanium nitride coatings deposited by physical vapor deposition dc magnetron sputtering on stainless steel substrates. The titanium nitride layers exhibit a rich variety of elastic contrast in the ultrasonic force microscopy images. Nanoscale inhomogeneities in stiffness on the titanium nitride films have been attributed to softer substoichiometric titanium nitride species and/or trapped subsurface gas. The results show that increasing the sputtering power at the Ti cathode increases the elastic homogeneity of the titanium nitride layers on the nanometer scale. Ultrasonic force microscopy elastic mapping on titanium nitride layers demonstrates the capability of the technique to provide information of high value for the engineering of improved coatings.

Surface characteristics and bioactivity of oxide film on titanium metal formed by thermal oxidation.

PubMed

Park, Yeong-Joon; Song, Ho-Jun; Kim, In; Yang, Hong-So

2007-04-01

In this study, we characterized the surface of oxide film formed on titanium metal through the use of thermal treatment and investigated the effect of surface characteristics on the bioactivity of titanium. The as-received sample group was prepared by polishing and cleaning CP-Ti as a control group, and thermally oxidized sample groups were prepared by heat treating at 530, 600, 700, 800, 900, and 1000 degrees C respectively. Micro-morphology, crystalline structure, chemical composition, and binding state were evaluated using FE-SEM, XRD, and XPS. The bioactivity of sample groups was investigated by observing the degree of calcium phosphate formation from immersion testing in MEM. The surface characterization tests showed that hydroxyl group content in titanium oxide film was increased, as the density of titanium atoms was high and the surface area was large. In MEM immersion test, initial calcium phosphate formation was dependent upon the thickness of titanium oxide, and resultant calcium phosphate formation depended on the content of the hydroxyl group of the titanium oxide film surface.

Nanosilver particle formation on a high surface area titanate.

PubMed

Shi, Meng; Lin, Christopher C H; Wu, Lan; Holt, Christopher M B; Mitlin, David; Kuznicki, Steven M

2010-12-01

Titanium based molecular sieves, such as ETS-10, have the ability to exchange silver ions and subsequently support self assembly of stable silver nanoparticles when heated. We report that a high surface area sodium titanate (resembling ETS-2) displays a similar ability to self template silver nanoparticles on its surface. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show high concentrations of silver nanoparticles on the surface of this sodium titanate, formed by thermal reduction of exchanged silver cations. The nanoparticles range in size from 4 to 12 nm, centered at around 6 nm. In addition to SEM and TEM, XRD and surface area analysis were used to characterize the material. The results indicate that this sodium titanate has a high surface area (>263 m2/g), and high ion exchange capacity for silver (30+ wt%) making it an excellent substrate for the exchange and generation of uniform, high-density silver nanoparticles.

Visible-Light-Induced Bactericidal Activity of a Nitrogen-Doped Titanium Photocatalyst against Human Pathogens

PubMed Central

Wong, Ming-Show; Chu, Wen-Chen; Sun, Der-Shan; Huang, Hsuan-Shun; Chen, Jiann-Hwa; Tsai, Pei-Jane; Lin, Nien-Tsung; Yu, Mei-Shiuan; Hsu, Shang-Feng; Wang, Shih-Lien; Chang, Hsin-Hou

2006-01-01

The antibacterial activity of photocatalytic titanium dioxide (TiO2) substrates is induced primarily by UV light irradiation. Recently, nitrogen- and carbon-doped TiO2 substrates were shown to exhibit photocatalytic activities under visible-light illumination. Their antibacterial activity, however, remains to be quantified. In this study, we demonstrated that nitrogen-doped TiO2 substrates have superior visible-light-induced bactericidal activity against Escherichia coli compared to pure TiO2 and carbon-doped TiO2 substrates. We also found that protein- and light-absorbing contaminants partially reduce the bactericidal activity of nitrogen-doped TiO2 substrates due to their light-shielding effects. In the pathogen-killing experiment, a significantly higher proportion of all tested pathogens, including Shigella flexneri, Listeria monocytogenes, Vibrio parahaemolyticus, Staphylococcus aureus, Streptococcus pyogenes, and Acinetobacter baumannii, were killed by visible-light-illuminated nitrogen-doped TiO2 substrates than by pure TiO2 substrates. These findings suggest that nitrogen-doped TiO2 has potential application in the development of alternative disinfectants for environmental and medical usages. PMID:16957236

[The influence of surface conditioning on the shear bond strength of La-Porcelain and titanium].

PubMed

Mo, Anchun; Cen, Yuankun; Liao, Yunmao

2003-04-20

To determine the influence of different surface conditioning methods on bonding strength of low fusing porcelain (La-Porcelain) and titanium. The surface of the samples were sandblasted for 2 min with 80-250 microns Al2O3 or coated for two times with Si-couple agent or conditioned by pre-oxidation. The shear bond strength was examined by push-type shear test with a speed of 0.5 mm/min in a universal testing machine. Scanning electron microscopy (SEM) and electron probe micro-analyzer (EPMA) were employed to explore the relationship between bonding strength and microstructures, as well as the element diffusion at the interface between porcelain coating and titanium when heated at 800 degrees C. Bonding strength was not statistically different (P > 0.05) after sandblasting with Al2O3 in particle size ranged from 80 microns to 250 microns. When a Si-couple agent was used, bond of porcelain to titanium was significantly lower (P < 0.05). The shear bond strength of the porcelain to the pre-oxidized titanium surface remained unchanged after heating (P > 0.05). The SEM results revealed integrity of porcelain and titanium. La-Porcelain showed a small effect of surface coarseness. Sandblasting the titanium surface with 150-180 microns Al2O3 can be recommended as a method for better bonding between La-Porcelain and titanium. The Si-couple agent coating and pre-oxidation of titanium surface is unnecessary.

Relating Chemical and Topographical Modification of Materials to Macroscopic Adhesion

DTIC Science & Technology

2011-11-14

CFRP, T800H/3900-2) and titanium alloy (Ti- 6Al - 4V ) surfaces are presented, before and after surface treatment, using a number of surface...Experimental: Titanium alloy (Ti- 6Al - 4V , an alloy consisting of 90% titanium , 6% aluminum and 4% vanadium, 0.063" thick) was purchased from...spectrum indicates a dramatic decrease in oxygen content and a concomitant increase in titanium metal alloy (Ti- 6Al - 4V ) at the surface. This

TiO2 micro-nano-hybrid surface to alleviate biological aging of UV-photofunctionalized titanium

PubMed Central

Iwasa, Fuminori; Tsukimura, Naoki; Sugita, Yoshihiko; Kanuru, Rajita Kodali; Kubo, Katsutoshi; Hasnain, Hafiz; Att, Wael; Ogawa, Takahiro

2011-01-01

Bioactivity and osteoconductivity of titanium degrade over time after surface processing. This time-dependent degradation is substantial and defined as the biological aging of titanium. UV treatment has shown to reactivate the aged surfaces, a process known as photofunctionalization. This study determined whether there is a difference in the behavior of biological aging for titanium with micro-nano-hybrid topography and titanium with microtopography alone, following functionalization. Titanium disks were acid etched to create micropits on the surface. Micro-nano-hybrid surfaces were created by depositioning 300-nm diameter TiO2 nodules onto the micropits using a previously established self-assembly protocol. These disks were stored for 8 weeks in the dark to allow sufficient aging, then treated with UV light for 48 hours. Rat bone marrow–derived osteoblasts were cultured on fresh disks (immediately after UV treatment), 3-day-old disks (disks stored for 3 days after UV treatment), and 7-day- old disks. The rates of cell attachment, spread, proliferation, and levels of alkaline phosphatase activity, and calcium deposition were reduced by 30%–50% on micropit surfaces, depending on the age of the titanium. In contrast, 7-day-old hybrid surfaces maintained equivalent levels of bioactivity compared with the fresh surfaces. Both micropit and micro-nano-hybrid surfaces were superhydrophilic immediately after UV treatment. However, after 7 days, the micro-nano- hybrid surfaces became hydrorepellent, while the micropit surfaces remained hydrophilic. The sustained bioactivity levels of the micro-nano-hybrid surfaces were nullified by treating these surfaces with Cl−anions. A thin TiO2 coating on the micropit surface without the formation of nanonodules did not result in the prevention or alleviation of the time-dependent decrease in biological activity. In conclusion, the micro-nano-hybrid titanium surfaces may slow the rate of time-dependent degradation of titanium bioactivity after UV photofunctionalization compared with titanium surfaces with microtopography alone. This antibiological aging effect was largely regulated by its sustained electropositivity uniquely conferred in TiO2 nanonodules, and was independent of the degree of hydrophilicity. These results demonstrate the potential usefulness of these hybrid surfaces to effectively utilize the benefits of UV photofunctionalization and provide a model to explore the mechanisms underlying antibiological aging properties. PMID:21760728

TiO2 micro-nano-hybrid surface to alleviate biological aging of UV-photofunctionalized titanium.

PubMed

Iwasa, Fuminori; Tsukimura, Naoki; Sugita, Yoshihiko; Kanuru, Rajita Kodali; Kubo, Katsutoshi; Hasnain, Hafiz; Att, Wael; Ogawa, Takahiro

2011-01-01

Bioactivity and osteoconductivity of titanium degrade over time after surface processing. This time-dependent degradation is substantial and defined as the biological aging of titanium. UV treatment has shown to reactivate the aged surfaces, a process known as photofunctionalization. This study determined whether there is a difference in the behavior of biological aging for titanium with micro-nano-hybrid topography and titanium with microtopography alone, following functionalization. Titanium disks were acid etched to create micropits on the surface. Micro-nano-hybrid surfaces were created by depositioning 300-nm diameter TiO(2) nodules onto the micropits using a previously established self-assembly protocol. These disks were stored for 8 weeks in the dark to allow sufficient aging, then treated with UV light for 48 hours. Rat bone marrow-derived osteoblasts were cultured on fresh disks (immediately after UV treatment), 3-day-old disks (disks stored for 3 days after UV treatment), and 7-day- old disks. The rates of cell attachment, spread, proliferation, and levels of alkaline phosphatase activity, and calcium deposition were reduced by 30%-50% on micropit surfaces, depending on the age of the titanium. In contrast, 7-day-old hybrid surfaces maintained equivalent levels of bioactivity compared with the fresh surfaces. Both micropit and micro-nano-hybrid surfaces were superhydrophilic immediately after UV treatment. However, after 7 days, the micro-nano- hybrid surfaces became hydrorepellent, while the micropit surfaces remained hydrophilic. The sustained bioactivity levels of the micro-nano-hybrid surfaces were nullified by treating these surfaces with Cl(-)anions. A thin TiO(2) coating on the micropit surface without the formation of nanonodules did not result in the prevention or alleviation of the time-dependent decrease in biological activity. In conclusion, the micro-nano-hybrid titanium surfaces may slow the rate of time-dependent degradation of titanium bioactivity after UV photofunctionalization compared with titanium surfaces with microtopography alone. This antibiological aging effect was largely regulated by its sustained electropositivity uniquely conferred in TiO(2) nanonodules, and was independent of the degree of hydrophilicity. These results demonstrate the potential usefulness of these hybrid surfaces to effectively utilize the benefits of UV photofunctionalization and provide a model to explore the mechanisms underlying antibiological aging properties.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Honda, Mitsuhiro; Saito, Yuika, E-mail: yuika@ap.eng.osaka-u.ac.jp; Kawata, Satoshi

We report plasmonic nanoparticle enhanced photocatalysis on titanium dioxide (TiO{sub 2}) in the deep-UV range. Aluminum (Al) nanoparticles fabricated on TiO{sub 2} film increases the reaction rate of photocatalysis by factors as high as 14 under UV irradiation in the range of 260–340 nm. The reaction efficiency has been determined by measuring the decolorization rate of methylene blue applied on the TiO{sub 2} substrate. The enhancement of photocatalysis shows particle size and excitation wavelength dependence, which can be explained by the surface plasmon resonance of Al nanoparticles.

Covalent Functionalization of NiTi Surfaces with Bioactive Peptide Amphiphile Nanofibers

PubMed Central

Sargeant, Timothy D.; Rao, Mukti S.; Koh, Chung-Yan

2009-01-01

Surface modification enables the creation of bioactive implants using traditional material substrates without altering the mechanical properties of the bulk material. For applications such as bone plates and stents, it is desirable to modify the surface of metal alloy substrates to facilitate cellular attachment, proliferation, and possibly differentiation. In this work we present a general strategy for altering the surface chemistry of nickel-titanium shape memory alloy (NiTi) in order to covalently attach self-assembled peptide amphiphile (PA) nanofibers with bioactive functions. Bioactivity in the systems studied here includes biological adhesion and proliferation of osteoblast and endothelial cell types. The optimized surface treatment creates a uniform TiO2 layer with low levels of Ni on the NiTi surface, which is subsequently covered with an aminopropylsilane coating using a novel, lower temperature vapor deposition method. This method produces an aminated surface suitable for covalent attachment of PA molecules containing terminal carboxylic acid groups. The functionalized NiTi surfaces have been characterized by X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectroscopy (ToF-SIMS), and atomic force microscopy (AFM). These techniques offer evidence that the treated metal surfaces consist primarily of TiO2 with very little Ni, and also confirm the presence of the aminopropylsilane overlayer. Self-assembled PA nanofibers presenting the biological peptide adhesion sequence Arg-Gly-Asp-Ser are capable of covalently anchoring to the treated substrate, as demonstrated by spectrofluorimetry and AFM. Cell culture and scanning electron microscopy (SEM) demonstrate cellular adhesion, spreading, and proliferation on these functionalized metal surfaces. Furthermore, these experiments demonstrate that covalent attachment is crucial for creating robust PA nanofiber coatings, leading to confluent cell monolayers. PMID:18083225

Silicon based multilayer photoelectrodes for photoelectrolysis of water to produce hydrogen from the sun

NASA Astrophysics Data System (ADS)

Faruque, Faisal

The main objective of this work is to study different materials for the direct photosynthesis of hydrogen from water. A variety of photocatalysts such as titanium dioxide, titanium oxy-nitride, silicon carbide, and gallium nitride are being investigated by others for the clean production of hydrogen for fuel cells and hydrogen economy. Our approach was to deposit suitable metallic regions on photocatalyst nanoparticles to direct the efficient synthesis of hydrogen to a particular site for convenient collection. We studied different electrode metals such as gold, platinum, titanium, palladium, and tungsten. We also studied different solar cell materials such as silicon (p- and n-types), silicon carbide and titanium dioxide semiconductors in order to efficiently generate electrons under illumination. We introduced a novel silicon-based multilayer photosynthesis device to take advantage of suitable properties of silicon and tungsten to efficiently produce hydrogen. The device consisted of a silicon (0.5mm) substrate, a deposited atomic layer of Al2O 3 (1nm), a doped polysilicon (0.1microm), and finally a tungsten nanoporous (5-10nm) layer acting as an interface electrode with water. The Al2O 3 layer was introduced to reduce leakage current and to prevent the spreading of the diffused p-n junction layer between the silicon and doped polysilicon layers. The surface of the photoelectrode was coated with nanotextured tungsten nanopores (TNP), which increased the surface area of the electrodes to the electrolyte, assisting in electron-hole mobility, and acting as a photocatalyst. The reported device exhibited a fill factor (%FF) of 27.22% and solar-to-hydrogen conversion efficiency of 0.03174%. This thesis describes the structures of the device, and offers a characterization and comparison between different photoelectrodes.

Direct morphological comparison of vacuum plasma sprayed and detonation gun sprayed hydroxyapatite coatings for orthopaedic applications.

PubMed

Gledhill, H C; Turner, I G; Doyle, C

1999-02-01

Hydroxyapatite coatings on titanium substrates were produced using two thermal spray techniques vacuum plasma spraying and detonation gun spraying. X-ray diffraction was used to compare crystallinity and residual stresses in the coatings. Porosity was measured using optical microscopy in conjunction with an image analysis system. Scanning electron microscopy and surface roughness measurements were used to characterise the surface morphologies of the coatings. The vacuum plasma sprayed coatings were found to have a lower residual stress, a higher crystallinity and a higher level of porosity than the detonation gun coatings. It is concluded that consideration needs to be given to the significance of such variations within the clinical context.

Effect of Novel Quercetin Titanium Dioxide-Decorated Multi-Walled Carbon Nanotubes Nanocomposite on Bacillus subtilis Biofilm Development

PubMed Central

Raie, Diana S.; Mhatre, Eisha; El-Desouki, Doaa S.; Labena, Ahmed; El-Ghannam, Gamal; Farahat, Laila A.; Youssef, Tareq; Fritzsche, Wolfgang; Kovács, Ákos T.

2018-01-01

The present work was targeted to design a surface against cell seeding and adhering of bacteria, Bacillus subtilis. A multi-walled carbon nanotube/titanium dioxide nano-power was produced via simple mixing of carbon nanotube and titanium dioxide nanoparticles during the sol-gel process followed by heat treatment. Successfully, quercetin was immobilized on the nanocomposite via physical adsorption to form a quercetin/multi-walled carbon nanotube/titanium dioxide nanocomposite. The adhesion of bacteria on the coated-slides was verified after 24 h using confocal laser-scanning microscopy. Results indicated that the quercetin/multi-walled carbon nanotube/titanium dioxide nanocomposite had more negativity and higher recovery by glass surfaces than its counterpart. Moreover, coating surfaces with the quercetin-modified nanocomposite lowered both hydrophilicity and surface-attached bacteria compared to surfaces coated with the multi-walled carbon nanotubes/titanium dioxide nanocomposite. PMID:29346268

STEM and APT characterization of scale formation on a La,Hf,Ti-doped NiCrAl model alloy.

PubMed

Unocic, Kinga A; Chen, Yimeng; Shin, Dongwon; Pint, Bruce A; Marquis, Emmanuelle A

2018-06-01

A thermally grown scale formed on a cast NiCrAl model alloy doped with lanthanum, hafnium, and titanium was examined after isothermal exposure at 1100 °C for 100 h in dry flowing O 2 to understand the dopant segregation along scale grain boundaries. The complex scale formed on the alloy surface was composed of two types of substrates: phase-dependent, thin (<250 nm) outer layers and a columnar-grained ∼3.5 μm inner alumina layer. Two types of oxides formed between the inner and outer scale layers: small (3-15 nm) La 2 O 3 and larger (≤50 nm) HfO 2 oxide precipitates. Nonuniform distributions of the hafnium, lanthanum, and titanium dopants were observed along the inner scale grain boundaries, with hafnium dominating in most of the grain boundaries of α-Al 2 O 3. The concentration of reactive elements (RE) seemed to strongly depend on the grain boundary structure. The level of titanium grain boundary segregation in the inner scale decreased toward the model alloy (substrate), confirming the fast outward diffusion of titanium. Hafnium was also observed at the metal-scale interface and in the γ' (Ni 3 Al) phase of the alloy. High-resolution scanning transmission electron microscopy (STEM) confirmed the substitution of REs for aluminum atoms at the scale grain boundaries, consistent with both the semiconducting band structure and the site-blocking models. Both STEM and atom probe tomography allowed quantification of REs along the scale grain boundaries across the scale thickness. Analysis of the scale morphology after isothermal exposure in flowing oxygen revealed a myriad of new precipitate phases, RE segregation dependence on grain boundary type, and atomic arrangement along scale grain boundaries, which is expected to influence the scale growth rate, stability, and mechanical properties. Copyright © 2018 Elsevier Ltd. All rights reserved.

Oriented conductive oxide electrodes on SiO2/Si and glass

DOEpatents

Jia, Quanxi; Arendt, Paul N.

2001-01-01

A thin film structure is provided including a silicon substrate with a layer of silicon dioxide on a surface thereof, and a layer of cubic oxide material deposited upon the layer of silicon dioxide by ion-beam-assisted-deposition, said layer of cubic oxide material characterized as biaxially oriented. Preferably, the cubic oxide material is yttria-stabilized zirconia. Additional thin layers of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide are deposited upon the layer of yttria-stabilized zirconia. An intermediate layer of cerium oxide is employed between the yttria-stabilized zirconia layer and the lanthanum strontium cobalt oxide layer. Also, a layer of barium strontium titanium oxide can be upon the layer of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide. Also, a method of forming such thin film structures, including a low temperature deposition of a layer of a biaxially oriented cubic oxide material upon the silicon dioxide surface of a silicon dioxide/silicon substrate is provided.

Solid Lubricant For Alumina

NASA Technical Reports Server (NTRS)

Dellacorte, Christopher; Pepper, Stephen V.; Honecy, Frank S.

1993-01-01

Outer layer of silver lubricates, while intermediate layer of titanium ensures adhesion. Lubricating outer films of silver deposited on thin intermediate films of titanium on alumina substrates found to reduce sliding friction and wear. Films provide effective lubrication for ceramic seals, bearings, and other hot sliding components in advanced high-temperature engines.

Tuning the surface microstructure of titanate coatings on titanium implants for enhancing bioactivity of implants

PubMed Central

Wang, Hui; Lai, Yue-Kun; Zheng, Ru-Yue; Bian, Ye; Zhang, Ke-Qin; Lin, Chang-Jian

2015-01-01

Biological performance of artificial implant materials is closely related to their surface characteristics, such as microtopography, and composition. Therefore, convenient fabrication of artificial implant materials with a cell-friendly surface structure and suitable composition was of great significance for current tissue engineering. In this work, titanate materials with a nanotubular structure were successfully fabricated through a simple chemical treatment. Immersion test in a simulated body fluid and in vitro cell culture were used to evaluate the biological performance of the treated samples. The results demonstrate that the titanate layer with a nanotubular structure on Ti substrates can promote the apatite-inducing ability remarkably and greatly enhance cellular responses. This highlights the potential of such titanate biomaterials with the special nanoscale structure and effective surface composition for biomedical applications such as bone implants. PMID:26089665

Dimensional accuracy and surface property of titanium casting using gypsum-bonded alumina investment.

PubMed

Yan, Min; Takahashi, Hidekazu; Nishimura, Fumio

2004-12-01

The aim of the present study was to evaluate the dimensional accuracy and surface property of titanium casting obtained using a gypsum-bonded alumina investment. The experimental gypsum-bonded alumina investment with 20 mass% gypsum content mixed with 2 mass% potassium sulfate was used for five cp titanium castings and three Cu-Zn alloy castings. The accuracy, surface roughness (Ra), and reaction layer thickness of these castings were investigated. The accuracy of the castings obtained from the experimental investment ranged from -0.04 to 0.23%, while surface roughness (Ra) ranged from 7.6 to 10.3microm. A reaction layer of about 150 microm thickness under the titanium casting surface was observed. These results suggested that the titanium casting obtained using the experimental investment was acceptable. Although the reaction layer was thin, surface roughness should be improved.

Mechanically Robust, Stretchable Solar Absorbers with Submicron-Thick Multilayer Sheets for Wearable and Energy Applications.

PubMed

Lee, Hye Jin; Jung, Dae-Han; Kil, Tae-Hyeon; Kim, Sang Hyeon; Lee, Ki-Suk; Baek, Seung-Hyub; Choi, Won Jun; Baik, Jeong Min

2017-05-31

A facile method to fabricate a mechanically robust, stretchable solar absorber for stretchable heat generation and an enhanced thermoelectric generator (TEG) is demonstrated. This strategy is very simple: it uses a multilayer film made of titanium and magnesium fluoride optimized by a two-dimensional finite element frequency-domain simulation, followed by the application of mechanical stresses such as bending and stretching to the film. This process produces many microsized sheets with submicron thickness (∼500 nm), showing great adhesion to any substrates such as fabrics and polydimethylsiloxane. It exhibits a quite high light absorption of approximately 85% over a wavelength range of 0.2-4.0 μm. Under 1 sun illumination, the solar absorber on various stretchable substrates increased the substrate temperature to approximately 60 °C, irrespective of various mechanical stresses such as bending, stretching, rubbing, and even washing. The TEG with the absorber on the top surface also showed an enhanced output power of 60%, compared with that without the absorber. With an incident solar radiation flux of 38.3 kW/m 2 , the output power significantly increased to 24 mW/cm 2 because of the increase in the surface temperature to 141 °C.

Architecture for coated conductors

DOEpatents

Foltyn, Stephen R.; Arendt, Paul N.; Wang, Haiyan; Stan, Liliana

2010-06-01

Articles are provided including a base substrate having a layer of an oriented cubic oxide material with a rock-salt-like structure layer thereon, and, a layer of epitaxial titanium nitride upon the layer of an oriented cubic oxide material having a rock-salt-like structure. Such articles can further include thin films of high temperature superconductive oxides such as YBCO upon the layer of epitaxial titanium nitride or upon a intermediate buffer layer upon the layer of epitaxial titanium nitride.

Effects of Titanium Surface Microtopography and Simvastatin on Growth and Osteogenic Differentiation of Human Mesenchymal Stem Cells in Estrogen-Deprived Cell Culture.

PubMed

Arpornmaeklong, Premjit; Pripatnanont, Prisana; Chookiatsiri, Chonticha; Tangtrakulwanich, Boonsin

This study aimed to investigate the effects of titanium surface topography and simvastatin on growth and osteogenic differentiation of human bone marrow stromal cells (hBMSCs) in estrogen-deprived (ED) cell culture. Human BMSCs were seeded on cell culture plates, smooth-surface titanium (Ti) disks, and sandblasted with large grits and acid etched (SLA)-surface Ti disks; and subsequently cultured in regular (fetal bovine serum [FBS]), ED, and ED-with 100 nM simvastatin (ED-SIM) culture media for 14 to 21 days. Live/dead cell staining, scanning electron microscope examination, and cell viability assay were performed to determine cell attachment, morphology, and growth. Expression levels of osteoblast-associated genes, Runx2 and bone sialoprotein and levels of alkaline phosphatase (ALP) activity, calcium content, and osteocalcin in culture media were measured to determine osteoblastic differentiation. Expression levels of bone morphogenetic protein-2 (BMP-2) were investigated to examine stimulating effects of simvastatin (n = 4 to 5, mean ± SD). In vitro mineralization was verified by calcein staining. Human BMSCs exhibited different attachment and shapes on smooth and SLA titanium surfaces. Estrogen-deprived cell culture decreased cell attachment and growth, particularly on the SLA titanium surface, but cells were able to grow to reach confluence on day 21 in the ED-osteogenic (OS) culture medium. Promoting effects of the SLA titanium surface in ED-OS were significantly decreased. Simvastatin significantly increased osteogenic differentiation of human BMSCs on the SLA titanium surface in the ED-OS medium, and the promoting effects of simvastatin corresponded with the increasing of BMP-2 gene expression on the SLA titanium surface in ED-OS-SIM culture medium. The ED cell culture model provided a well-defined platform for investigating the effects of hormones and growth factors on cells and titanium surface interaction. Titanium, the SLA surface, and simvastatin synergistically promoted osteoblastic differentiation of hBMSCs in ED condition and might be useful to promote osteointegration in osteoporotic bone.

Surface characterization and cytotoxicity analysis of plasma sprayed coatings on titanium alloys.

PubMed

Rahman, Zia Ur; Shabib, Ishraq; Haider, Waseem

2016-10-01

In the realm of biomaterials, metallic materials are widely used for load bearing joints due to their superior mechanical properties. Despite the necessity for long term metallic implants, there are limitations to their prolonged use. Naturally, oxides of titanium have low solubilities and form passive oxide film spontaneously. However, some inclusion and discontinuity spots in oxide film make implant to adopt the decisive nature. These defects heighten the dissolution of metal ions from the implant surface, which results in diminishing bio-integration of titanium implant. To increase the long-term metallic implant stability, surface modifications of titanium alloys are being carried out. In the present study, biomimetic coatings of plasma sprayed hydroxyapatite and titanium were applied to the surface of commercially pure titanium and Ti6Al4V. Surface morphology and surface chemistry were studied using scanning electron microscopy and X-ray photoelectron spectroscopy, respectively. Cyclic potentiodynamic polarization and electrochemical impedance spectroscopy were carried out in order to study their electrochemical behavior. Moreover, cytotoxicity analysis was conducted for osteoblast cells by performing MTS assay. It is concluded that both hydroxyapatite and titanium coatings enhance corrosion resistance and improve cytocompatibility. Copyright © 2016 Elsevier B.V. All rights reserved.

Nanolayer formation on titanium by phosphonated gelatin for cell adhesion and growth enhancement

PubMed Central

Zhou, Xiaoyue; Park, Shin-Hye; Mao, Hongli; Isoshima, Takashi; Wang, Yi; Ito, Yoshihiro

2015-01-01

Phosphonated gelatin was prepared for surface modification of titanium to stimulate cell functions. The modified gelatin was synthesized by coupling with 3-aminopropylphosphonic acid using water-soluble carbodiimide and characterized by 31P nuclear magnetic resonance and gel permeation chromatography. Circular dichroism revealed no differences in the conformations of unmodified and phosphonated gelatin. However, the gelation temperature was changed by the modification. Even a high concentration of modified gelatin did not form a gel at room temperature. Time-of-flight secondary ion mass spectrometry showed direct bonding between the phosphonated gelatin and the titanium surface after binding. The binding behavior of phosphonated gelatin on the titanium surface was quantitatively analyzed by a quartz crystal microbalance. Ellipsometry showed the formation of a several nanometer layer of gelatin on the surface. Contact angle measurement indicated that the modified titanium surface was hydrophobic. Enhancement of the attachment and spreading of MC-3T3L1 osteoblastic cells was observed on the phosphonated gelatin-modified titanium. These effects on cell adhesion also led to growth enhancement. Phosphonation of gelatin was effective for preparation of a cell-stimulating titanium surface. PMID:26366080

UV photofunctionalization promotes nano-biomimetic apatite deposition on titanium

PubMed Central

Saita, Makiko; Ikeda, Takayuki; Yamada, Masahiro; Kimoto, Katsuhiko; Lee, Masaichi Chang-Il; Ogawa, Takahiro

2016-01-01

Background Although biomimetic apatite coating is a promising way to provide titanium with osteoconductivity, the efficiency and quality of deposition is often poor. Most titanium implants have microscale surface morphology, and an addition of nanoscale features while preserving the micromorphology may provide further biological benefit. Here, we examined the effect of ultraviolet (UV) light treatment of titanium, or photofunctionalization, on the efficacy of biomimetic apatite deposition on titanium and its biological capability. Methods and results Micro-roughed titanium disks were prepared by acid-etching with sulfuric acid. Micro-roughened disks with or without photofunctionalization (20-minute exposure to UV light) were immersed in simulated body fluid (SBF) for 1 or 5 days. Photofunctionalized titanium disks were superhydrophilic and did not form surface air bubbles when immersed in SBF, whereas non-photofunctionalized disks were hydrophobic and largely covered with air bubbles during immersion. An apatite-related signal was observed by X-ray diffraction on photofunctionalized titanium after 1 day of SBF immersion, which was equivalent to the one observed after 5 days of immersion of control titanium. Scanning electron microscopy revealed nodular apatite deposition in the valleys and at the inclines of micro-roughened structures without affecting the existing micro-configuration. Micro-roughened titanium and apatite-deposited titanium surfaces had similar roughness values. The attachment, spreading, settling, proliferation, and alkaline phosphate activity of bone marrow-derived osteoblasts were promoted on apatite-coated titanium with photofunctionalization. Conclusion UV-photofunctionalization of titanium enabled faster deposition of nanoscale biomimetic apatite, resulting in the improved biological capability compared to the similarly prepared apatite-deposited titanium without photofunctionalization. Photofunctionalization-assisted biomimetic apatite deposition may be a novel method to effectively enhance micro-roughened titanium surfaces without altering their microscale morphology. PMID:26834469

Modification of implant material surface properties by means of oxide nano-structured coatings deposition

NASA Astrophysics Data System (ADS)

Safonov, Vladimir; Zykova, Anna; Smolik, Jerzy; Rogowska, Renata; Lukyanchenko, Vladimir; Kolesnikov, Dmitrii

2014-08-01

The deposition of functional coatings on the metal surface of artificial joints is an effective way of enhancing joint tribological characteristics. It is well-known that nanostructured oxide coatings have specific properties advantageous for future implant applications. In the present study, we measured the high hardness parameters, the adhesion strength and the low friction coefficient of the oxide magnetron sputtered coatings. The corrosion test results show that the oxide coating deposition had improved the corrosion resistance by a factor of ten for both stainless steel and titanium alloy substrates. Moreover, the hydrophilic nature of coated surfaces in comparison with the metal ones was investigated in the tensiometric tests. The surfaces with nanostructured oxide coatings demonstrated improved biocompatibility for in vitro and in vivo tests, attributed to the high dielectric constants and the high values of the surface free energy parameters.

Human alveolar bone cell proliferation, expression of osteoblastic phenotype, and matrix mineralization on porous titanium produced by powder metallurgy.

PubMed

Rosa, Adalberto Luiz; Crippa, Grasiele Edilaine; de Oliveira, Paulo Tambasco; Taba, Mario; Lefebvre, Louis-Philippe; Beloti, Marcio Mateus

2009-05-01

This study aimed at investigating the influence of the porous titanium (Ti) structure on the osteogenic cell behaviour. Porous Ti discs were fabricated by the powder metallurgy process with the pore size typically between 50 and 400 microm and a porosity of 60%. Osteogenic cells obtained from human alveolar bone were cultured until subconfluence and subcultured on dense Ti (control) and porous Ti for periods of up to 17 days. Cultures grown on porous Ti exhibited increased cell proliferation and total protein content, and lower levels of alkaline phosphatase (ALP) activity than on dense Ti. In general, gene expression of osteoblastic markers-runt-related transcription factor 2, collagen type I, alkaline phosphatase, bone morphogenetic protein-7, and osteocalcin was lower at day 7 and higher at day 17 in cultures grown on porous Ti compared with dense Ti, a finding consistent with the enhanced growth rate for such cultures. The amount of mineralized matrix was greater on porous Ti compared with the dense one. These results indicate that the porous Ti is an appropriate substrate for osteogenic cell adhesion, proliferation, and production of a mineralized matrix. Because of the three-dimensional environment it provides, porous Ti should be considered an advantageous substrate for promoting desirable implant surface-bone interactions.

A new pulsed laser deposition technique: scanning multi-component pulsed laser deposition method.

PubMed

Fischer, D; de la Fuente, G F; Jansen, M

2012-04-01

The scanning multi-component pulsed laser deposition (PLD) method realizes uniform depositions of desired coatings by a modified pulsed laser deposition process, preferably with a femto-second laser-system. Multi-component coatings (single or multilayered) are thus deposited onto substrates via laser induced ablation of segmented targets. This is achieved via horizontal line-scanning of a focused laser beam over a uniformly moving target's surface. This process allows to deposit the desired composition of the coating simultaneously, starting from the different segments of the target and adjusting the scan line as a function of target geometry. The sequence and thickness of multilayers can easily be adjusted by target architecture and motion, enabling inter/intra layer concentration gradients and thus functional gradient coatings. This new, simple PLD method enables the achievement of uniform, large-area coatings. Case studies were performed with segmented targets containing aluminum, titanium, and niobium. Under the laser irradiation conditions applied, all three metals were uniformly ablated. The elemental composition within the rough coatings obtained was fixed by the scanned area to Ti-Al-Nb = 1:1:1. Crystalline aluminum, titanium, and niobium were found to coexist side by side at room temperature within the substrate, without alloy formation up to 600 °C. © 2012 American Institute of Physics

The black and white coatings on Ti-6Al-4V alloy or pure titanium by plasma electrolytic oxidation in concentrated silicate electrolyte

NASA Astrophysics Data System (ADS)

Han, Jun-xiang; Cheng, Yu-lin; Tu, Wen-bin; Zhan, Ting-Yan; Cheng, Ying-liang

2018-01-01

Black TiO2 has triggered scientific interest due to its unique properties such as enhanced solar-driven photocatalytic activity. In this paper, plasma electrolytic oxidation (PEO) treatment of Ti-6Al-4V alloy has been carried out in concentrated sodium silicate electrolyte. Silica-based black and white TiO2 coatings respectively have been obtained by controlling the oxidation time. The black coating, which was formed with a short treatment time, shows good corrosion resistance and the black appearance can be attributed to the presence of Ti2+ and Ti3+ in the coating. The lower valence titanium ions are absent in the white coatings and they also contain relatively higher Na content compared to the black coatings. The white coatings have great surface roughnesses and super hydrophilicity. The bonding strengths of the black and white coatings on the Ti-6Al-4V alloy are ∼14.4 and 4.3 MPa, respectively. The vanadium contributes little to the black appearance of the coating on Ti6Al4V alloy, since the same phenomena occur for the PEO of a pure titanium substrate.

Influence of pulse ratio on codeposition of copper species with calcium phosphate coatings on titanium by means of electrochemically assisted deposition.

PubMed

Wolf-Brandstetter, Cornelia; Oswald, Steffen; Bierbaum, Susanne; Wiesmann, Hans-Peter; Scharnweber, Dieter

2014-01-01

Aim of this study was to combine the well-known biocompatibility and ostoeconductivity of thin calcium phosphate coatings on titanium with proangiogenic signals from codeposited copper species. Copper species could be integrated in mineral layers based on hydroxyapatite by means of electrochemically assisted deposition from electrolytes containing calcium, phosphate, and copper ions. Different combinations of duration and intensity of galvanostatic pulses result in different amounts of deposited calcium phosphate and of copper species even for the same applied total charge. Absolute amounts of copper varied between 2.1 and 6.9 μg/cm², and the copper was distributed homogeneously as shown by EDX mapping. The presence of copper did not change the crystalline phase of deposited calcium phosphate (hydroxyapatite) but provoked a significant decrease in deposited amounts by factor 3 to 4. The copper was deposited mainly as Cu(I) species with a minor fraction of basic copper phosphates. Reduction of copper occurred not only at the surface of titanium but also within the hydroxyapatite coating due to the reaction with hydrogen produced by the electrolysis of water during the cathodic polarization of the substrate. Copyright © 2013 Wiley Periodicals, Inc.

Low temperature formation of electrode having electrically conductive metal oxide surface

DOEpatents

Anders, Simone; Anders, Andre; Brown, Ian G.; McLarnon, Frank R.; Kong, Fanping

1998-01-01

A low temperature process is disclosed for forming metal suboxides on substrates by cathodic arc deposition by either controlling the pressure of the oxygen present in the deposition chamber, or by controlling the density of the metal flux, or by a combination of such adjustments, to thereby control the ratio of oxide to metal in the deposited metal suboxide coating. The density of the metal flux may, in turn, be adjusted by controlling the discharge current of the arc, by adjusting the pulse length (duration of on cycle) of the arc, and by adjusting the frequency of the arc, or any combination of these parameters. In a preferred embodiment, a low temperature process is disclosed for forming an electrically conductive metal suboxide, such as, for example, an electrically conductive suboxide of titanium, on an electrode surface, such as the surface of a nickel oxide electrode, by such cathodic arc deposition and control of the deposition parameters. In the preferred embodiment, the process results in a titanium suboxide-coated nickel oxide electrode exhibiting reduced parasitic evolution of oxygen during charging of a cell made using such an electrode as the positive electrode, as well as exhibiting high oxygen overpotential, resulting in suppression of oxygen evolution at the electrode at full charge of the cell.

Tribological coating of titanium alloys by laser processing

NASA Astrophysics Data System (ADS)

Pang, Wang

Titanium-based alloys have been used for aerospace materials for many years. Recently, these alloys are now being increasingly considered for automotive, industrial and consumer applications. Their excellent creep resistance, corrosion resistance and relative higher specific strength ratio are attractive for many applications. However, the main obstacle for the wide adoption of Ti alloys in various industries is their poor tribological properties. In slide wear, Ti deforms and adhesive wear readily occurs. Their poor tribological properties are mainly due to low hardness and absolute values of tensile and shear strength. Different surface modification techniques have been studied in order to improve the tribological characteristics of Ti alloys, i.e. PVD, nitrding, carburizing, boriding, plating etc. Coatings produced by these techniques have their own limitations such as thermal distortion and grain growth. A different approach is to introduce hard particles in the Ti alloy matrix to form a MMC coating, which has tailor-made hardness and wear resistance properties. Laser cladding or laser alloying techniques facilitate the fabrication of surface MMC on Ti alloys without thermal distortion to the substrate. In this project, the fabrication of hard and wear resistant layers of metal matrix composite on titanium alloys substrate by laser surface alloying was investigated. Powder mixtures of Mo and WC were used to form the MMC layer. By optimizing the processing parameters and pre-placed powder mixture compositions, surface MMC of different properties have been successfully fabricated on CP-Ti and Ti6A14V respectively. The structure and characteristics of the MMC surface were investigated by metallography, SEM, XRD, and E-DAX. It was found that the hardness of the laser alloyed Mo/WC MMC surface was 300% higher than that of the CP-Ti substrate Excellent metallurgical bonding with the MMC layer of the substrate has been achieved. The relative kinetic frictional tests were carried out and the results showed that the kinetic coefficient of friction of the laser fabricated Ti-Mo-WC MMC coatings was much lower than that of the CP-Ti and Ti6A14V substrate. The wear resistance of this Ti-Mo-WC MMC was found to be between 60 to 150 times better than those of CP-Ti. The experimental results also identified a key issue of mixing efficiency that the density of WC was much higher than that of Ti and Mo and this rendered poor mixing between the different constituents. This resulted in a relatively poor repeatability of the coating quality. To solve this issue, a lower density carbide phase, TiC, was used. The hardness and dry sliding wear resistance of the Ti-Mo-TiC MMC was found to be lower than those of Ti-Mo-WC MMC. The mixing efficiency of the TiC in the Ti-Mo-MMC was found to be better than the WC in Ti-Mo-WC MMC. This combination gave a harder and more wear resistant MMC with more uniform properties across the width and depth of the alloyed layer formed. A mathematical model for predicting the melt depth of the alloyed MMC layer was developed together with a heat transfer mechanism between layers of powders under the laser irradiation. The model facilitates the prediction of melt depth of the alloyed layer and the dilution ratio of the MMC layer. It thus enabled the composition of the MMC layer to be predicted and tailor made. The project results contribute significantly to the knowledge of improving the wear and frictional properties of one of the most important engineering metals for the automobile and aerospace industries.

Surface characterization of nickel titanium orthodontic arch wires

PubMed Central

Krishnan, Manu; Seema, Saraswathy; Tiwari, Brijesh; Sharma, Himanshu S.; Londhe, Sanjay; Arora, Vimal

2015-01-01

Background Surface roughness of nickel titanium orthodontic arch wires poses several clinical challenges. Surface modification with aesthetic/metallic/non metallic materials is therefore a recent innovation, with clinical efficacy yet to be comprehensively evaluated. Methods One conventional and five types of surface modified nickel titanium arch wires were surface characterized with scanning electron microscopy, energy dispersive analysis, Raman spectroscopy, Atomic force microscopy and 3D profilometry. Root mean square roughness values were analyzed by one way analysis of variance and post hoc Duncan's multiple range tests. Results Study groups demonstrated considerable reduction in roughness values from conventional in a material specific pattern: Group I; conventional (578.56 nm) > Group V; Teflon (365.33 nm) > Group III; nitride (301.51 nm) > Group VI (i); rhodium (290.64 nm) > Group VI (ii); silver (252.22 nm) > Group IV; titanium (229.51 nm) > Group II; resin (158.60 nm). It also showed the defects with aesthetic (resin/Teflon) and nitride surfaces and smooth topography achieved with metals; titanium/silver/rhodium. Conclusions Resin, Teflon, titanium, silver, rhodium and nitrides were effective in decreasing surface roughness of nickel titanium arch wires albeit; certain flaws. Findings have clinical implications, considering their potential in lessening biofilm adhesion, reducing friction, improving corrosion resistance and preventing nickel leach and allergic reactions. PMID:26843749

The role of surface oxides on hydrogen sorption kinetics in titanium thin films

NASA Astrophysics Data System (ADS)

Hadjixenophontos, Efi; Michalek, Lukas; Roussel, Manuel; Hirscher, Michael; Schmitz, Guido

2018-05-01

Titanium is presently discussed as a catalyst to accelerate the hydrogenation kinetics of hydrogen storage materials. It is however known that H absorption in Ti decisively depends on the surface conditions (presence or absence of the natural surface oxide). In this work, we use Ti thin films of controlled thickness (50-800 nm) as a convenient tool for quantifying the atomic transport. XRD and TEM investigations allow us to follow the hydrogenation progress inside the film. Hydrogenation of TiO2/Ti bi-layers is studied at 300 °C, for different durations (10 s to 600 min) and at varying pressures of pure H2 atmosphere. Under these conditions, the hydrogenation is found to be linear in time. By comparing films with and without TiO2, as well as by studying the pressure dependence of hydrogenation, it is demonstrated that hydrogen transport across the oxide represents the decisive kinetic barrier rather than the splitting of H2 molecules at the surface. Hydrogenation appears by a layer-like reaction initiated by heterogeneous nucleation at the backside interface to the substrate. The linear growth constant and the H diffusion coefficient inside the oxide are quantified, as well as a reliable lower bound to the hydrogen diffusion coefficient in Ti is derived. The pressure dependence of hydrogen absorption is quantitatively modelled.

Monitoring N3 dye adsorption and desorption on TiO2 surfaces: a combined QCM-D and XPS study.

PubMed

Wayment-Steele, Hannah K; Johnson, Lewis E; Tian, Fangyuan; Dixon, Matthew C; Benz, Lauren; Johal, Malkiat S

2014-06-25

Understanding the kinetics of dye adsorption and desorption on semiconductors is crucial for optimizing the performance of dye-sensitized solar cells (DSSCs). Quartz crystal microbalance with dissipation monitoring (QCM-D) measures adsorbed mass in real time, allowing determination of binding kinetics. In this work, we characterize adsorption of the common RuBipy dye N3 to the native oxide layer of a planar, sputter-coated titanium surface, simulating the TiO2 substrate of a DSSC. We report adsorption equilibrium constants consistent with prior optical measurements of N3 adsorption. Dye binding and surface integrity were also verified by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy (XPS). We further study desorption of the dye from the native oxide layer on the QCM sensors using tetrabutylammonium hydroxide (TBAOH), a commonly used industrial desorbant. We find that using TBAOH as a desorbant does not fully regenerate the surface, though little ruthenium or nitrogen is observed by XPS after desorption, suggesting that carboxyl moieties of N3 remain bound. We demonstrate the native oxide layer of a titanium sensor as a valid and readily available planar TiO2 morphology to study dye adsorption and desorption and begin to investigate the mechanism of dye desorption in DSSCs, a system that requires further study.

Effects of titanium surface topography on morphology and in vitro activity of human gingival fibroblasts.

PubMed

Ramaglia, L; Capece, G; Di Spigna, G; Bruno, M P; Buonocore, N; Postiglione, L

2013-01-01

The aim of the present study was to evaluate in vitro the biological behavior of human gingival fibroblasts cultured on two different titanium surfaces. Titanium test disks were prepared with a machined, relatively smooth (S) surface or a rough surface (O) obtained by a double acid etching procedure. Primary cultures of human gingival fibroblasts were plated on the experimental titanium disks and cultured up to 14 days. Titanium disk surfaces were analysed by scanning electron microscopy (SEM). Cell proliferation and a quantitative analysis by ELISA in situ of ECM components as CoI, FN and TN were performed. Results have shown different effects of titanium surface microtopography on cell expression and differentiation. At 96 hours of culture on experimental surfaces human gingival fibroblasts displayed a favourable cell attachment and proliferation on both surfaces although showing some differences. Both the relatively smooth and the etched surfaces interacted actively with in vitro cultures of human gingival fibroblasts, promoting cell proliferation and differentiation. Results suggested that the microtopography of a double acid-etched rough surface may induce a greater Co I and FN production, thus conditioning in vivo the biological behaviour of human gingival fibroblasts during the process of peri-implant soft tissue healing.

Enhanced cell attachment and hemocompatibility of titanium by nanoscale surface modification through severe plastic integration of magnesium-rich islands and porosification.

PubMed

Rezaei, Masoud; Tamjid, Elnaz; Dinari, Ali

2017-10-11

Besides the wide applications of titanium and its alloys for orthopedic and biomedical implants, the biocompatible nature of titanium has emerged various surface modification techniques to enhance its bioactivity and osteointegration with living tissues. In this work, we present a new procedure for nanoscale surface modification of titanium implants by integration of magnesium-rich islands combined with controlled formation of pores and refinement of the surface grain structure. Through severe plastic deformation of the titanium surface with fine magnesium hydride powder, Mg-rich islands with varying sizes ranging from 100 nm to 1000 nm can be integrated inside a thin surface layer (100-500 µm) of the implant. Selective etching of the surface forms a fine structure of surface pores which their average size varies in the range of 200-500 nm depending on the processing condition. In vitro biocompatibility and hemocompatibility assays show that the Mg-rich islands and the induced surface pores significantly enhance cell attachment and biocompatibility without an adverse effect on the cell viability. Therefore, severe plastic integration of Mg-rich islands on titanium surface accompanying with porosification is a new and promising procedure with high potential for nanoscale modification of biomedical implants.

Oxidation-Resistant Coating For Bipolar Lead/Acid Battery

NASA Technical Reports Server (NTRS)

Bolstad, James J.

1993-01-01

Cathode side of bipolar substrate coated with nonoxidizable conductive layer. Coating prepared as water slurry of aqueous dispersion of polyethylene copolymer plus such conductive fillers as tin oxide, titanium, tantalum, or tungsten oxide. Applied easily to substrate of polyethylene carbon plastic. As slurry dries, conductive, oxidation-resistant coating forms on positive side of substrate.

Tribology of bio-inspired nanowrinkled films on ultrasoft substrates.

PubMed

Lackner, Juergen M; Waldhauser, Wolfgang; Major, Lukasz; Teichert, Christian; Hartmann, Paul

2013-01-01

Biomimetic design of new materials uses nature as antetype, learning from billions of years of evolution. This work emphasizes the mechanical and tribological properties of skin, combining both hardness and wear resistance of its surface (the stratum corneum) with high elasticity of the bulk (epidermis, dermis, hypodermis). The key for combination of such opposite properties is wrinkling, being consequence of intrinsic stresses in the bulk (soft tissue): Tribological contact to counterparts below the stress threshold for tissue trauma occurs on the thick hard stratum corneum layer pads, while tensile loads smooth out wrinkles in between these pads. Similar mechanism offers high tribological resistance to hard films on soft, flexible polymers, which is shown for diamond-like carbon (DLC) and titanium nitride thin films on ultrasoft polyurethane and harder polycarbonate substrates. The choice of these two compared substrate materials will show that ultra-soft substrate materials are decisive for the distinct tribological material. Hierarchical wrinkled structures of films on these substrates are due to high intrinsic compressive stress, which evolves during high energetic film growth. Incremental relaxation of these stresses occurs by compound deformation of film and elastic substrate surface, appearing in hierarchical nano-wrinkles. Nano-wrinkled topographies enable high elastic deformability of thin hard films, while overstressing results in zigzag film fracture along larger hierarchical wrinkle structures. Tribologically, these fracture mechanisms are highly important for ploughing and sliding of sharp and flat counterparts on hard-coated ultra-soft substrates like polyurethane. Concentration of polyurethane deformation under the applied normal loads occurs below these zigzag cracks. Unloading closes these cracks again. Even cyclic testing do not lead to film delamination and retain low friction behavior, if the adhesion to the substrate is high and the initial friction coefficient of the film against the sliding counterpart low, e.g. found for DLC.

Tribology of bio-inspired nanowrinkled films on ultrasoft substrates

PubMed Central

Lackner, Juergen M.; Waldhauser, Wolfgang; Major, Lukasz; Teichert, Christian; Hartmann, Paul

2013-01-01

Biomimetic design of new materials uses nature as antetype, learning from billions of years of evolution. This work emphasizes the mechanical and tribological properties of skin, combining both hardness and wear resistance of its surface (the stratum corneum) with high elasticity of the bulk (epidermis, dermis, hypodermis). The key for combination of such opposite properties is wrinkling, being consequence of intrinsic stresses in the bulk (soft tissue): Tribological contact to counterparts below the stress threshold for tissue trauma occurs on the thick hard stratum corneum layer pads, while tensile loads smooth out wrinkles in between these pads. Similar mechanism offers high tribological resistance to hard films on soft, flexible polymers, which is shown for diamond-like carbon (DLC) and titanium nitride thin films on ultrasoft polyurethane and harder polycarbonate substrates. The choice of these two compared substrate materials will show that ultra-soft substrate materials are decisive for the distinct tribological material. Hierarchical wrinkled structures of films on these substrates are due to high intrinsic compressive stress, which evolves during high energetic film growth. Incremental relaxation of these stresses occurs by compound deformation of film and elastic substrate surface, appearing in hierarchical nano-wrinkles. Nano-wrinkled topographies enable high elastic deformability of thin hard films, while overstressing results in zigzag film fracture along larger hierarchical wrinkle structures. Tribologically, these fracture mechanisms are highly important for ploughing and sliding of sharp and flat counterparts on hard-coated ultra-soft substrates like polyurethane. Concentration of polyurethane deformation under the applied normal loads occurs below these zigzag cracks. Unloading closes these cracks again. Even cyclic testing do not lead to film delamination and retain low friction behavior, if the adhesion to the substrate is high and the initial friction coefficient of the film against the sliding counterpart low, e.g. found for DLC. PMID:24688710

Antibacterial titanium nano-patterned arrays inspired by dragonfly wings

NASA Astrophysics Data System (ADS)

Bhadra, Chris M.; Khanh Truong, Vi; Pham, Vy T. H.; Al Kobaisi, Mohammad; Seniutinas, Gediminas; Wang, James Y.; Juodkazis, Saulius; Crawford, Russell J.; Ivanova, Elena P.

2015-11-01

Titanium and its alloys remain the most popular choice as a medical implant material because of its desirable properties. The successful osseointegration of titanium implants is, however, adversely affected by the presence of bacterial biofilms that can form on the surface, and hence methods for preventing the formation of surface biofilms have been the subject of intensive research over the past few years. In this study, we report the response of bacteria and primary human fibroblasts to the antibacterial nanoarrays fabricated on titanium surfaces using a simple hydrothermal etching process. These fabricated titanium surfaces were shown to possess selective bactericidal activity, eliminating almost 50% of Pseudomonas aeruginosa cells and about 20% of the Staphylococcus aureus cells coming into contact with the surface. These nano-patterned surfaces were also shown to enhance the aligned attachment behavior and proliferation of primary human fibroblasts over 10 days of growth. These antibacterial surfaces, which are capable of exhibiting differential responses to bacterial and eukaryotic cells, represent surfaces that have excellent prospects for biomedical applications.

Antibacterial titanium nano-patterned arrays inspired by dragonfly wings

PubMed Central

Bhadra, Chris M.; Khanh Truong, Vi; Pham, Vy T. H.; Al Kobaisi, Mohammad; Seniutinas, Gediminas; Wang, James Y.; Juodkazis, Saulius; Crawford, Russell J.; Ivanova, Elena P.

2015-01-01

Titanium and its alloys remain the most popular choice as a medical implant material because of its desirable properties. The successful osseointegration of titanium implants is, however, adversely affected by the presence of bacterial biofilms that can form on the surface, and hence methods for preventing the formation of surface biofilms have been the subject of intensive research over the past few years. In this study, we report the response of bacteria and primary human fibroblasts to the antibacterial nanoarrays fabricated on titanium surfaces using a simple hydrothermal etching process. These fabricated titanium surfaces were shown to possess selective bactericidal activity, eliminating almost 50% of Pseudomonas aeruginosa cells and about 20% of the Staphylococcus aureus cells coming into contact with the surface. These nano-patterned surfaces were also shown to enhance the aligned attachment behavior and proliferation of primary human fibroblasts over 10 days of growth. These antibacterial surfaces, which are capable of exhibiting differential responses to bacterial and eukaryotic cells, represent surfaces that have excellent prospects for biomedical applications. PMID:26576662

Cell responses to titanium treated by a sandblast-free method for implant applications.

PubMed

Zhang, Jie; Xie, Youneng; Zuo, Jun; Li, Jiaxin; Wei, Qiuping; Yu, Zhiming; Tang, Zhangui

2017-09-01

Sandblast and acid-etching (SLA) is the most prevalent treatment to titanium implants, while residual sand particles are inevitably introduced on SLA titanium surfaces. NH 4 OH and H 2 O 2 mixture was used to etch titanium plates (E) and titanium bars (EB), aiming at substituting sandblast procedure. To study the effects of different scale rough structures on cell response of Human osteoblast-like cells (MG63), traditional H 2 SO 4 and HCl mixture was also used to further etch the titanium plates above (DE). Holes of 10-20μm were obtained on E and DE surfaces, which are very close to the size of osteoblasts. Surfaces with micro/nano and micro/submicro hierarchical structures were obtained on the treated titanium. As-prepared E, DE and EB surfaces are hydrophilic, while only EB stayed hydrophilic after 5days' exposure to air. MG63 cultured on E and EB surfaces showed higher proliferation rate and attachment area than on DE and P surfaces. E and DE showed higher alkaline phosphatases (ALP) activity after 7 and 14days of osteoinduction, while EB showed the highest osteopontin (OPN) and bone sialoprotein (BSP) production after 21days of osteoinduction. These results indicate that E and EB surfaces boost the proliferation and osteogenic differentiation of MG63 without introducing sand particles. This is a promising treatment to titanium implant. Copyright © 2017. Published by Elsevier B.V.

Homogenous photocatalytic decontamination of prion infected stainless steel and titanium surfaces.

PubMed

Berberidou, Chrysanthi; Xanthopoulos, Konstantinos; Paspaltsis, Ioannis; Lourbopoulos, Athanasios; Polyzoidou, Eleni; Sklaviadis, Theodoros; Poulios, Ioannis

2013-01-01

Prions are notorious for their extraordinary resistance to traditional methods of decontamination, rendering their transmission a public health risk. Iatrogenic Creutzfeldt-Jakob disease (iCJD) via contaminated surgical instruments and medical devices has been verified both experimentally and clinically. Standard methods for prion inactivation by sodium hydroxide or sodium hypochlorite have failed, in some cases, to fully remove prion infectivity, while they are often impractical for routine applications. Prion accumulation in peripheral tissues and indications of human-to-human bloodborne prion transmission, highlight the need for novel, efficient, yet user-friendly methods of prion inactivation. Here we show both in vitro and in vivo that homogenous photocatalytic oxidation, mediated by the photo-Fenton reagent, has the potential to inactivate the pathological prion isoform adsorbed on metal substrates. Photocatalytic oxidation with 224 μg mL(-1) Fe (3+), 500 μg mL(-1) h(-1) H 2O 2, UV-A for 480 min lead to 100% survival in golden Syrian hamsters after intracranial implantation of stainless steel wires infected with the 263K prion strain. Interestingly, photocatalytic treatment of 263K infected titanium wires, under the same experimental conditions, prolonged the survival interval significantly, but failed to eliminate infectivity, a result that we correlate with the increased adsorption of PrP(Sc) on titanium, in comparison to stainless steel. Our findings strongly indicate that our, user--and environmentally--friendly protocol can be safely applied to the decontamination of prion infected stainless steel surfaces.

Initial oral biofilm formation on titanium implants with different surface treatments: An in vivo study.

PubMed

Ferreira Ribeiro, Cyntia; Cogo-Müller, Karina; Franco, Gilson Cesar; Silva-Concílio, Laís Regiane; Sampaio Campos, Márcia; de Mello Rode, Sigmar; Claro Neves, Ana Christina

2016-09-01

The aim of this study was to examine in vivo the initial bacterial adhesion on titanium implants with different surface treatments. Ten subjects wore oral splints containing machined pure titanium disks (Ti-M), acid-etched titanium (Ti-AE) and anodized and laser irradiated disks (Ti-AL) for 24h. After this period, disks were removed from the splints and adherent bacteria were quantified by an enzymatic assay to assess total viable bacteria and by Real Time PCR to evaluate total bacteria and Streptococcus oralis levels. Additionally, the initial adherent microorganisms were visualized by scanning electron microscopy (SEM). Titanium surface morphology was verified using SEM, and roughness was evaluated by profilometer analysis. Regarding titanium surface roughness, Ti-AL (1.423±0.397) showed significantly higher Ra values than did Ti-M (0.771±0.182) and Ti-AE (0.735±0.196) (p<0.05, ANOVA - Tahame). Ti-AE and Ti-AL presented roughened micro-structure surfaces characterized by open pores, whereas Ti-M showed long grooves alternating with planed areas. Comparing the Ti-M, Ti-AE and Ti-AL groups for viable bacteria (MTT assay), total bacteria and S. oralis quantification (qPCR), no significant differences were observed among these three groups (p>0.05, ANOVA - Tahame). SEM images showed similar bacterial adhesion on the three titanium surfaces, predominantly characterized by cocci and several bacilli, indicating an initial colonization of the oral biofilm. In conclusion, roughness and microtopography did not stimulate initial biofilm formation on titanium surfaces with different surface treatments. Copyright © 2016 Elsevier Ltd. All rights reserved.

Adsorption behavior of glycidoxypropyl-trimethoxy-silane on titanium alloy Ti-6.5Al-1Mo-1V-2Zr

NASA Astrophysics Data System (ADS)

Liu, Jian-hua; Zhan, Zhong-wei; Yu, Mei; Li, Song-mei

2013-01-01

The adsorption behavior of glycidoxypropyl-trimethoxy-silane (GTMS) on titanium alloy Ti-6.5Al-1Mo-1V-2Zr was investigated by using X-ray photoelectron spectroscopy (XPS), Tafel polarization test, and electrochemical impedance spectroscopy (EIS). From the XPS results, it was found that the silane coverage on the titanium surface generally increased with GTMS concentration, with a slight decrease at concentration of 0.1%. Based on the relationship between isoelectronic point (IEP) of titanium surface and the pH values of silane solutions, adsorption mechanisms at different concentrations were proposed. The surface coverage data of GTMS on titanium surface was also derived from electrochemical measurements. By linear fitting the coverage data, it revealed that the adsorption of GTMS on the titanium alloy surface at 30 °C was of a physisorption-based mechanism, and obeyed Langmuir adsorption isotherm. The adsorption equilibrium constant (Kads) and free energy of adsorption process (ΔGads) were calculated to elaborate the mechanism of GTMS adsorption.

In vitro cytotoxicity and surface topography evaluation of additive manufacturing titanium implant materials.

PubMed

Tuomi, Jukka T; Björkstrand, Roy V; Pernu, Mikael L; Salmi, Mika V J; Huotilainen, Eero I; Wolff, Jan E H; Vallittu, Pekka K; Mäkitie, Antti A

2017-03-01

Custom-designed patient-specific implants and reconstruction plates are to date commonly manufactured using two different additive manufacturing (AM) technologies: direct metal laser sintering (DMLS) and electron beam melting (EBM). The purpose of this investigation was to characterize the surface structure and to assess the cytotoxicity of titanium alloys processed using DMLS and EBM technologies as the existing information on these issues is scarce. "Processed" and "polished" DMLS and EBM disks were assessed. Microscopic examination revealed titanium alloy particles and surface flaws on the processed materials. These surface flaws were subsequently removed by polishing. Surface roughness of EBM processed titanium was higher than that of DMLS processed. The cytotoxicity results of the DMLS and EBM discs were compared with a "gold standard" commercially available titanium mandible reconstruction plate. The mean cell viability for all discs was 82.6% (range, 77.4 to 89.7) and 83.3% for the control reconstruction plate. The DMLS and EBM manufactured titanium plates were non-cytotoxic both in "processed" and in "polished" forms.

Femtosecond laser structuring of titanium implants

NASA Astrophysics Data System (ADS)

Vorobyev, A. Y.; Guo, Chunlei

2007-06-01

In this study we perform the first femtosecond laser surface treatment of titanium in order to determine the potential of this technology for surface structuring of titanium implants. We find that the femtosecond laser produces a large variety of nanostructures (nanopores, nanoprotrusions) with a size down to 20 nm, multiple parallel grooved surface patterns with a period on the sub-micron level, microroughness in the range of 1-15 μm with various configurations, smooth surface with smooth micro-inhomogeneities, and smooth surface with sphere-like nanostructures down to 10 nm. Also, we have determined the optimal conditions for producing these surface structural modifications. Femtosecond laser treatment can produce a richer variety of surface structures on titanium for implants and other biomedical applications than long-pulse laser treatments.

Titanium hydride and hydrogen concentration in acid-etched commercially pure titanium and titanium alloy implants: a comparative analysis of five implant systems.

PubMed

Szmukler-Moncler, S; Bischof, M; Nedir, R; Ermrich, M

2010-09-01

Acid etching is a popular method to texture the surface of dental implants. During etching, the titanium oxide protective layer is dissolved and small native hydrogen ions diffuse into the unprotected implant surface. They enrich the implant surface with hydrogen and precipitate into titanium hydride (TiH). The aim of this study was to measure the concentration of TiH at the implant surface and the total concentration of Hydrogen at five commercially available implant systems, made of either commercially pure (cp) titanium or titanium alloy. X-Ray diffraction (XRD) was conducted on each implant system to determine the compounds present at the implant surface. Following a TiH(2)/Ti calibration curve, the concentration of TiH was determined. Concentration of hydrogen in the implants was measured by the inert gas fusion thermal conductivity/infrared detection method. XRD data showed that TiH was present on all cp titanium implants but not on the alloyed implants. TiH concentration varied between 5% and 37%. Hydrogen concentration varied between 43 and 108 ppm, no difference in uptake was found between the cp titanium and alloyed implants. Low solubility of hydrogen in alpha-titanium is responsible for precipitation into TiH. Stronger etching conditions led to higher concentration of TiH2-x. High solubility of hydrogen in the beta-phase of the alloy is preventing hydrogen from precipitating into TiH. All implants, even those lacking TiH at the surface, were enriched with hydrogen. In all implants, hydrogen concentration was within the normative limit of 130 ppm.

Silver/hydroxyapatite composite coatings on porous titanium surfaces by sol-gel method.

PubMed

Qu, Jie; Lu, Xiong; Li, Dan; Ding, Yonghui; Leng, Yang; Weng, Jie; Qu, Shuxin; Feng, Bo; Watari, Fumio

2011-04-01

Hydroxyapatite (HA) coatings loaded with nanosilver particles is an attractive method to impart the HA coating with antibacterial properties. Producing Ag/HA coatings on porous Ti substrates have been an arduous job since commonly used line-of-sight techniques are not able to deposit uniform coatings on the inner pore surfaces of the porous Ti. In this study, porous Ti scaffolds with high porosity and interconnected structures were prepared by polymer impregnating method. A sol-gel process was used to produce uniform Ag/HA composite coatings on the surfaces of porous Ti substrates. Ca(NO(3) )(2) ·4H(2) O and P(2) O(5) in an ethyl alcohol based system was selected to prepare the sol, which ensured the homogeneous distribution of Ag in the sol. The characterization revealed that silver particles uniformly distributed in the coatings without agglomeration. High antibacterial ratio (>95%), against E. coli and S. albus was expressed by the silver-containing coatings (Ag/HA 0.8 and 1.6 wt %). The biocompatibility of the Ag/HA 0.8 surfaces was as good as that of pure HA surface, as revealed by culturing osteoblasts on them. The results indicated that Ag/HA 0.8 had the good balance between the biocompatibility and antibacterial properties of the coatings. Copyright © 2011 Wiley Periodicals, Inc.

An investigation of adhesive/adherend and fiber/matrix interactions. Part A: Surface characterization of titanium dioxide, titantium and titanium 6% Al to 4% V powders: Interaction with water, hydrogen chloride and polymers

NASA Technical Reports Server (NTRS)

Siriwardane, R. V.; Wightman, J. P.

1982-01-01

The titanium dioxide surface is discussed. Polymer adhesive are also discussed. Titanium powders are considered. Characterization techniques are also considered. Interactions with polymers, water vapor, and HCl are reported. Adsorbents are characterized.

Antimicrobial Agents Used in the Treatment of Peri-Implantitis Alter the Physicochemistry and Cytocompatibility of Titanium Surfaces.

PubMed

Kotsakis, Georgios A; Lan, Caixia; Barbosa, Joao; Lill, Krista; Chen, Ruoqiong; Rudney, Joel; Aparicio, Conrado

2016-07-01

Chemotherapeutic agents (ChAs) are considered an integral part of current treatment protocols for the decontamination of titanium implants with peri-implantitis, based on their antimicrobial effect. Despite the proven antimicrobial effect of ChAs on titanium-bound biofilms, previous studies have elucidated an unexpected disassociation between bacterial reduction and biologically acceptable treatment outcomes. In this study, the authors hypothesize that ChAs residues alter titanium physicochemistry and thus compromise cellular response to decontaminated surfaces. Grit-blasted acid-etched titanium disks were contaminated with multispecies microcosm biofilms grown from in vivo peri-implant plaque samples. To simulate implant decontamination, the contaminated disks were burnished with 0.12% chlorhexidine, 20% citric acid, 24% EDTA/1.5% NaOCl, or sterile saline and assessed surface physicochemical properties. Sterile untreated surfaces were the controls. The biologic effects of decontamination were assessed via cell proliferation and differentiation assays. Bacterial counts after decontamination confirmed that the ChAs were antimicrobial. X-ray photoelectron spectroscopy invariably detected elemental contaminants associated with each ChA molecule or salt that significantly altered wettability compared with controls. Notably, all surfaces with ChA residues showed some cytotoxic effect compared with controls (P <0.05). Increased cell counts were consistently found in the saline-treated group compared with chlorhexidine (P = 0.03). Interestingly, no association was found between antimicrobial effect and cell counts (P >0.05). ChA-specific residues left on the titanium surfaces altered titanium physical properties and adversely affected the osteoblastic response irrespective of their observed antimicrobial effect. Chlorhexidine may compromise the biocompatibility of titanium surfaces, and its use is not recommended to detoxify implants. Sterile saline, citric acid, and NaOCl-EDTA may be proposed for use in the treatment of peri-implantitis. Contrary to previous studies that recommended the selection of ChAs for the decontamination of titanium implants according to their antimicrobial effects, the present study demonstrated that the restoration of the biocompatibility of contaminated titanium surfaces is also contingent on the preservation of titanium material properties.

Friction and wear behavior of single-crystal silicon carbide in contact with titanium

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1977-01-01

Sliding friction experiments were conducted with single crystal silicon carbide in sliding contact with titanium. Results indicate that the friction coefficient is greater in vacuum than in argon and that this is due to the greater adhesion or adhesive transfer in vacuum. Thin films of silicon carbide transferred to titanium also adhered to silicon carbide both in argon at atmospheric pressure and in high vacuum. Cohesive bonds fractured on both the silicon carbide and titanium surfaces. The wear debris of silicon carbide created by fracture plowed the silicon carbide surface in a plastic manner. The friction characteristics of titanium in contact with silicon carbide were sensitive to the surface roughness of silicon carbide, and the friction coefficients were higher for a rough surface of silicon carbide than for a smooth one. The difference in friction results was due to plastic deformation (plowing of titanium).

Flexible anodized aluminum oxide membranes with customizable back contact materials

NASA Astrophysics Data System (ADS)

Nadimpally, B.; Jarro, C. A.; Mangu, R.; Rajaputra, S.; Singh, V. P.

2016-12-01

Anodized aluminum oxide (AAO) membranes were fabricated using flexible substrate/carrier material. This method facilitates the use of AAO templates with many different materials as substrates that are otherwise incompatible with most anodization techniques. Thin titanium (Ti) and tungsten (W) layers were employed as interlayer materials. Titanium enhances adhesion. Tungsten not only helps eliminate the barrier layer but also plays a critical role in enabling the use of flexible substrates. The resulting flexible templates provide new, exciting opportunities in photovoltaic and other device applications. CuInSe2 nanowires were electrochemically deposited into porous AAO templates with molybdenum (Mo) as the back contact material. The feasibility of using any material to form a contact with semiconductor nanowires has been demonstrated for the first time enabling new avenues in photovoltaic applications.

Conversion treatment of thin titanium layer deposited on carbon steel

NASA Astrophysics Data System (ADS)

Benarioua, Younes; Wendler, Bogdan; Chicot, Didier

2018-05-01

The present study has been conducted in order to obtain titanium carbide layer using a conversion treatment consisting of two main steps. In the first step a thin pure titanium layer was deposited on 120C4 carbon steel by PVD. In the second step, the carbon atoms from the substrate diffuse to the titanium coating due to a vacuum annealing treatment and the Ti coating transforms into titanium carbide. Depending on the annealing temperature a partial or complete conversion into TiC is obtained. The hardness of the layer can be expected to differ depending on the processing temperatures. By a systematic study of the hardness as a function of the applied load, we confirm the process of growth of the layer.

Tailoring of the titanium surface by immobilization of heparin/fibronectin complexes for improving blood compatibility and endothelialization: an in vitro study.

PubMed

Li, Guicai; Yang, Ping; Liao, Yuzhen; Huang, Nan

2011-04-11

To improve the blood compatibility and endothelialization simultaneously and to ensure the long-term effectiveness of the cardiovascular implants, we developed a surface modification method, enabling the coimmobilization of biomolecules to metal surfaces. In the present study, a heparin and fibronectin mixture (Hep/Fn) covalently immobilized on a titanium (Ti) substrate for biocompatibility was investigated. Different systems [N-(3-dimethylaminopropyl)-N'-ethylcarbodiimide and N-hydroxysuccinimide, electrostatic] were used for the formation of Hep/Fn layers. Atomic force microscopy (AFM) showed that the roughness of the silanized Ti surface decreased after the immobilization of Hep/Fn. Fourier transform infrared spectroscopy (FTIR), Toluidine Blue O (TBO) test, and immunochemistry assay showed that Hep/Fn mixture was successfully immobilized on Ti surface. Blood compatibility tests (hemolysis rate, APTT, platelet adhesion, fibrinogen conformational change) showed that the coimmobilized films of Hep/Fn mixture reduced blood hemolysis rate, prolonged blood coagulation time, reduced platelets activation and aggregation, and induced less fibrinogen conformational change compared with a bare Ti surface. Endothelial cell (EC) seeding showed more EC with better morphology on pH 4 samples than on pH 7 and EDC/NHS samples, which showed rounded and aggregated cells. Systematic evaluation showed that the pH 4 samples also had much better blood compatibility. All results suggest that the coimmobilized films of Hep/Fn can confer excellent antithrombotic properties and with good endothelialization. We envisage that this method will provide a potential and effective solution for the surface modification of cardiovascular implant materials.

Analyzing the Deposition of Titanium Dioxide Nanoparticles at Model Rough Mineral Surfaces Using a Quartz Crystal Microbalance with Dissipation Monitoring

NASA Astrophysics Data System (ADS)

Li, Y.; Kananizadeh, N.; Rodenhausen, K. B.; Schubert, M.; Bartelt-Hunt, S.

2015-12-01

Titanium dioxide nanoparticles (nTiO2) is the most extensively manufactured engineered materials. nTiO2 from sunscreens was found to enter sediments after released into a lake. nTiO2 may also enter the subsurface via irrigation using effluents from wastewater treatment plants. Interaction of nTiO2 with soils and sediments will largely influence their fate, transport, and ecotoxicity. Measuring the interaction between nTiO2 and natural substrates (e.g. such as sands) is particularly challenging due to highly heterogeneous and rough natural sand surfaces. In this study, an engineered controllable rough surface known as three dimensional nanostructured sculptured columnar thin films (SCTFs) has been used to mimic surface roughness. SCTFs were fabricated by glancing angle deposition (GLAD), a physical vapor deposition technique facilitated by electron beam evaporation. Interaction between nTiO2 and SCTF coated surfaces was investigated using a quartz crystal microbalance with dissipation monitoring (QCM-D). In parallel, a Generalized Ellipsometry (GE) was coupled with the QCM-D to measure the deposition of nTiO2. We found that the typical QCM-D modeling approach, e.g. viscoelastic model, would largely overestimate the mass of deposited nTiO2, because the frequency drops due to particle deposition or water entrapment in rough areas were not differentiated. Here, we demonstrate a new approach to model QCM-D data for nTiO2 deposition on rough surfaces, which couples the viscoelastic model with a model of flow on the non-uniform surface.

Controlled implant/soft tissue interaction by nanoscale surface modifications of 3D porous titanium implants.

PubMed

Rieger, Elisabeth; Dupret-Bories, Agnès; Salou, Laetitia; Metz-Boutigue, Marie-Helene; Layrolle, Pierre; Debry, Christian; Lavalle, Philippe; Vrana, Nihal Engin

2015-06-07

Porous titanium implants are widely employed in the orthopaedics field to ensure good bone fixation. Recently, the use of porous titanium implants has also been investigated in artificial larynx development in a clinical setting. Such uses necessitate a better understanding of the interaction of soft tissues with porous titanium structures. Moreover, surface treatments of titanium have been generally evaluated in planar structures, while the porous titanium implants have complex 3 dimensional (3D) architectures. In this study, the determining factors for soft tissue integration of 3D porous titanium implants were investigated as a function of surface treatments via quantification of the interaction of serum proteins and cells with single titanium microbeads (300-500 μm in diameter). Samples were either acid etched or nanostructured by anodization. When the samples are used in 3D configuration (porous titanium discs of 2 mm thickness) in vivo (in subcutis of rats for 2 weeks), a better integration was observed for both anodized and acid etched samples compared to the non-treated implants. If the implants were also pre-treated with rat serum before implantation, the integration was further facilitated. In order to understand the underlying reasons for this effect, human fibroblast cell culture tests under several conditions (directly on beads, beads in suspension, beads encapsulated in gelatin hydrogels) were conducted to mimic the different interactions of cells with Ti implants in vivo. Physical characterization showed that surface treatments increased hydrophilicity, protein adsorption and roughness. Surface treatments also resulted in improved adsorption of serum albumin which in turn facilitated the adsorption of other proteins such as apolipoprotein as quantified by protein sequencing. The cellular response to the beads showed considerable difference with respect to the cell culture configuration. When the titanium microbeads were entrapped in cell-laden gelatin hydrogels, significantly more cells migrated towards the acid etched beads. In conclusion, the nanoscale surface treatment of 3D porous titanium structures can modulate in vivo integration by the accumulative effect of the surface treatment on several physical factors such as protein adsorption, surface hydrophilicity and surface roughness. The improved protein adsorption capacity of the treated implants can be further exploited by a pre-treatment with autologous serum to render the implant surface more bioactive. Titanium microbeads are a good model system to observe these effects in a 3D microenvironment and provide a better representation of cellular responses in 3D.

Engineered Chimeric Peptides as Antimicrobial Surface Coating Agents toward Infection-Free Implants

PubMed Central

Yazici, Hilal; O'Neill, Mary B.; Kacar, Turgay; Wilson, Brandon R.; Oren, E. Emre; Sarikaya, Mehmet; Tamerler, Candan

2016-01-01

Prevention of bacterial colonization and consequent biofilm formation remains a major challenge in implantable medical devices. Implant-associated infections are not only a major cause of implant failures but also their conventional treatment with antibiotics brings further complications due to the escalation in multidrug resistance to a variety of bacterial species. Owing to their unique properties, antimicrobial peptides (AMPs) have gained significant attention as effective agents to combat colonization of microorganisms. These peptides have been shown to exhibit a wide spectrum of activities with specificity to a target cell while having a low tendency for developing bacterial resistance. Engineering biomaterial surfaces that feature AMP properties, therefore, offer a promising approach to prevent implant infections. Here, we engineered a chimeric peptide with bifunctionality that both forms a robust solid-surface coating while presenting antimicrobial property. The individual domains of the chimeric peptides were evaluated for their solid-binding kinetics to titanium substrate as well as for their antimicrobial properties in solution. The antimicrobial efficacy of the chimeric peptide on the implant material was evaluated in vitro against infection by a variety of bacteria, including Streptococcus mutans, Staphylococcus. epidermidis, and Escherichia coli, which are commonly found in oral and orthopedic implant related surgeries. Our results demonstrate significant improvement in reducing bacterial colonization onto titanium surfaces below the detectable limit. Engineered chimeric peptides with freely displayed antimicrobial domains could be a potential solution for developing infection-free surfaces by engineering implant interfaces with highly reduced bacterial colonization property. PMID:26795060

Engineered Chimeric Peptides as Antimicrobial Surface Coating Agents toward Infection-Free Implants.

PubMed

Yazici, Hilal; O'Neill, Mary B; Kacar, Turgay; Wilson, Brandon R; Oren, E Emre; Sarikaya, Mehmet; Tamerler, Candan

2016-03-02

Prevention of bacterial colonization and consequent biofilm formation remains a major challenge in implantable medical devices. Implant-associated infections are not only a major cause of implant failures but also their conventional treatment with antibiotics brings further complications due to the escalation in multidrug resistance to a variety of bacterial species. Owing to their unique properties, antimicrobial peptides (AMPs) have gained significant attention as effective agents to combat colonization of microorganisms. These peptides have been shown to exhibit a wide spectrum of activities with specificity to a target cell while having a low tendency for developing bacterial resistance. Engineering biomaterial surfaces that feature AMP properties, therefore, offer a promising approach to prevent implant infections. Here, we engineered a chimeric peptide with bifunctionality that both forms a robust solid-surface coating while presenting antimicrobial property. The individual domains of the chimeric peptides were evaluated for their solid-binding kinetics to titanium substrate as well as for their antimicrobial properties in solution. The antimicrobial efficacy of the chimeric peptide on the implant material was evaluated in vitro against infection by a variety of bacteria, including Streptococcus mutans, Staphylococcus. epidermidis, and Escherichia coli, which are commonly found in oral and orthopedic implant related surgeries. Our results demonstrate significant improvement in reducing bacterial colonization onto titanium surfaces below the detectable limit. Engineered chimeric peptides with freely displayed antimicrobial domains could be a potential solution for developing infection-free surfaces by engineering implant interfaces with highly reduced bacterial colonization property.

DNA ELECTROPHORESIS AT SURFACES

DOE Office of Scientific and Technical Information (OSTI.GOV)

RAFAILOVICH, MIRIAM; SOKOLOV, JONATHAN; GERSAPPE, DILIP

2003-09-01

During this year we performed two major projects: I. We developed a detailed theoretical model which complements our experiments on surface DNA electrophoresis. We found that it was possible to enhance the separation of DNA chains by imposing a chemical nanoscale pattern on the surface. This approach utilized the surface interaction effect of the DNA chains with the substrate and is a refinement to our previous method in which DNA chains were separated on homogeneous flat surfaces. By introducing the nano-patterns on the surface, the conformational changes of DNA chains of different lengths can be amplified, which results in themore » different friction strengths with the substrate surface. Our results also show that, when compared to the DNA electrophoresis performed on homogeneous flat surfaces, nanopatterned surfaces offer a larger window in choosing different surface interactions to achieve separation. II. In collaboration with a large international manufacturer of skin care products we also embarked on a project involving photo toxicity of titanium dioxide nanoparticles, which are a key ingredient in sunscreen and cosmetic lotions. The results clearly implicated the nanoparticles in catalyzing damage to chromosomal DNA. We then used this knowledge to develop a polymer/anti-oxidant coating which prevented the photocatalytic reaction on DNA while still retaining the UV absorptive properties of the nanoparticles. The standard gel electrophoresis was not sufficient in determining the extent of the DNA damage. The conclusions of this study were based predominantly on analysis obtained with the surface electrophoresis method.« less

Bioactive potential of silica coatings and its effect on the adhesion of proteins to titanium implants.

PubMed

Romero-Gavilan, F; Araújo-Gomes, N; Sánchez-Pérez, A M; García-Arnáez, I; Elortza, F; Azkargorta, M; de Llano, J J Martín; Carda, C; Gurruchaga, M; Suay, J; Goñi, I

2018-02-01

There is an ever-increasing need to develop dental implants with ideal characteristics to achieve specific and desired biological response in the scope of improve the healing process post-implantation. Following that premise, enhancing and optimizing titanium implants through superficial treatments, like silica sol-gel hybrid coatings, are regarded as a route of future research in this area. These coatings change the physicochemical properties of the implant, ultimately affecting its biological characteristics. Sandblasted acid-etched titanium (SAE-Ti) and a silica hybrid sol-gel coating (35M35G30T) applied onto the Ti substrate were examined. The results of in vitro and in vivo tests and the analysis of the protein layer adsorbed to each surface were compared and discussed. In vitro analysis with MC3T3-E1 osteoblastic cells, showed that the sol-gel coating raised the osteogenic activity potential of the implants (the expression of osteogenic markers, the alkaline phosphatase (ALP) and IL-6 mRNAs, increased). In the in vivo experiments using as model rabbit tibiae, both types of surfaces promoted osseointegration. However, the coated implants demonstrated a clear increase in the inflammatory activity in comparison with SAE-Ti. Mass spectrometry (LC-MS/MS) analysis showed differences in the composition of protein layers formed on the two tested surfaces. Large quantities of apolipoproteins were found attached predominantly to SAE-Ti. The 35M35G30T coating adsorbed a significant quantity of complement proteins, which might be related to the material intrinsic bioactivity, following an associated, natural and controlled immune response. The correlation between the proteomic data and the in vitro and in vivo outcomes is discussed on this experimental work. Copyright © 2017 Elsevier B.V. All rights reserved.

Superhydrophilic TiO2 thin film by nanometer scale surface roughness and dangling bonds

NASA Astrophysics Data System (ADS)

Bharti, Bandna; Kumar, Santosh; Kumar, Rajesh

2016-02-01

A remarkable enhancement in the hydrophilic nature of titanium dioxide (TiO2) films is obtained by surface modification in DC-glow discharge plasma. Thin transparent TiO2 films were coated on glass substrate by sol-gel dip coating method, and exposed in DC-glow discharge plasma. The plasma exposed TiO2 film exhibited a significant change in its wetting property contact angle, which is a representative of wetting property, has reduced to considerable limits 3.02° and 1.85° from its initial value 54.40° and 48.82° for deionized water and ethylene glycol, respectively. It is elucidated that the hydrophilic property of plasma exposed TiO2 films dependent mainly upon nanometer scale surface roughness. Variation, from 4.6 nm to 19.8 nm, in the film surface roughness with exposure time was observed by atomic force microscopy (AFM). Analysis of variation in the values of contact angle and surface roughness with increasing plasma exposure time reveal that the surface roughness is the main factor which makes the modified TiO2 film superhydrophilic. However, a contribution of change in the surface states, to the hydrophilic property, is also observed for small values of the plasma exposure time. Based upon nanometer scale surface roughness and dangling bonds, a variation in the surface energy of TiO2 film from 49.38 to 88.92 mJ/m2 is also observed. X-ray photoelectron spectroscopy (XPS) results show change in the surface states of titanium and oxygen. The observed antifogging properties are the direct results of the development of the superhydrophilic wetting characteristics to TiO2 films.

[Follow-up examinations after removal of titanium plates coated with anodic titanium oxide ceramic].

PubMed

Velich, Norbert; Németh, Zsolt; Barabás, József; Szabó, György

2002-04-01

Transformation of the titanium metal surface with titanium oxides produced in various ways belongs among the most up-to-date procedures. The authors as pioneers in this field (e.g. Nobel Biocare TiUnite surface), have been utilizing for more than 15 years dental root implants and fixing elements (for mandibular osteosynthesis) coated with titanium oxide ceramics, produced by anodic oxidation and thermal treatment. The aim of this work was to assess the extent to which a titanium oxide ceramic coating influences the fate of plates applied for osteosynthesis within the human body. During a 5-year period (1995-1999), 108 of 1396 titanium oxide ceramic plates had to be removed for various reasons: loosening of the plate [47], osteomyelitis [25], a palpable swelling and tenderness [21] at the request of the patient for psychological reasons (13) or breaking of the plate [2]. When these 108 plates were removed, it was not possible to detect metallosis in even a single case; nor was there any tissue damage that could be attributed to the surface of the plates, whereas the literature data indicate that such damage is relatively frequent in the environment of traditional titanium fixing elements. The present investigation confirms the favourable properties of the titanium oxide ceramic surface.

a Study on Microstructure Characteristics of IN SITU Formed TiC Reinforced Composite Coatings

NASA Astrophysics Data System (ADS)

Liu, Peng; Guo, Wei; Luo, Hui

2012-04-01

In situ synthesized TiC reinforced composite coating was fabricated by laser cladding of Al-Ni-Cr-C powders on titanium alloys, which can greatly improve the surface performance of the substrate. In this study, the Al-Ni-Cr-C laser-cladded composite coatings have been researched by means of X-ray diffraction, scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA). There was a metallurgical combination between the Al-Ni-Cr-C laser-cladded coating and the Ti-6Al-4V substrate, and the micro-hardness of the Al-Ni-Cr-C laser-cladded coating was in the range of 1200-1450 HV0.2, which was 3-4 times higher than that of Ti-6Al-4V substrate. Furthermore, the reinforcement of theAl-Ni-Cr-C laser-cladded coating were mainly contributed to the action of the TiC, Ti3Al, Cr7C3, Al8Cr5 phases and the solution strengthening.

Silver Nanowire Top Electrodes in Flexible Perovskite Solar Cells using Titanium Metal as Substrate.

PubMed

Lee, Minoh; Ko, Yohan; Min, Byoung Koun; Jun, Yongseok

2016-01-08

Flexible perovskite solar cells (FPSCs) have various applications such as wearable electronic textiles and portable devices. In this work, we demonstrate FPSCs on a titanium metal substrate employing solution-processed silver nanowires (Ag NWs) as the top electrode. The Ag NW electrodes were deposited on top of the spiro-MeOTAD hole transport layer by a carefully controlled spray-coating method at moderate temperatures. The power conversion efficiency (PCE) reached 7.45 % under AM 1.5 100 mW cm(-2) illumination. Moreover, the efficiency for titanium-based FPSCs decreased only slightly (by 2.6 % of the initial value) after the devices were bent 100 times. With this and other advances, fully solution-based indium-free flexible photovoltaics, advantageous in terms of price and processing, have the potential to be scaled into commercial production. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of zirconium nitride physical vapor deposition coating on preosteoblast cell adhesion and proliferation onto titanium screws.

PubMed

Rizzi, Manuela; Gatti, Giorgio; Migliario, Mario; Marchese, Leonardo; Rocchetti, Vincenzo; Renò, Filippo

2014-11-01

Titanium has long been used to produce dental implants. Problems related to its manufacturing, casting, welding, and ceramic application for dental prostheses still limit its use, which highlights the need for technologic improvements. The aim of this in vitro study was to evaluate the biologic performance of titanium dental implants coated with zirconium nitride in a murine preosteoblast cellular model. The purpose of this study was to evaluate the chemical and morphologic characteristics of titanium implants coated with zirconium nitride by means of physical vapor deposition. Chemical and morphologic characterizations were performed by scanning electron microscopy and energy dispersive x-ray spectroscopy, and the bioactivity of the implants was evaluated by cell-counting experiments. Scanning electron microscopy and energy dispersive x-ray spectroscopy analysis found that physical vapor deposition was effective in covering titanium surfaces with zirconium nitride. Murine MC-3T3 preosteoblasts were seeded onto titanium-coated and zirconium nitride-coated screws to evaluate their adhesion and proliferation. These experiments found a significantly higher number of cells adhering and spreading onto zirconium nitride-coated surfaces (P<.05) after 24 hours; after 7 days, both titanium and zirconium nitride surfaces were completely covered with MC-3T3 cells. Analysis of these data indicates that the proposed zirconium nitride coating of titanium implants could make the surface of the titanium more bioactive than uncoated titanium surfaces. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Ductile and brittle transition behavior of titanium alloys in ultra-precision machining.

PubMed

Yip, W S; To, S

2018-03-02

Titanium alloys are extensively applied in biomedical industries due to their excellent material properties. However, they are recognized as difficult to cut materials due to their low thermal conductivity, which induces a complexity to their deformation mechanisms and restricts precise productions. This paper presents a new observation about the removal regime of titanium alloys. The experimental results, including the chip formation, thrust force signal and surface profile, showed that there was a critical cutting distance to achieve better surface integrity of machined surface. The machined areas with better surface roughness were located before the clear transition point, defining as the ductile to brittle transition. The machined area at the brittle region displayed the fracture deformation which showed cracks on the surface edge. The relationship between depth of cut and the ductile to brittle transaction behavior of titanium alloys in ultra-precision machining(UPM) was also revealed in this study, it showed that the ductile to brittle transaction behavior of titanium alloys occurred mainly at relatively small depth of cut. The study firstly defines the ductile to brittle transition behavior of titanium alloys in UPM, contributing the information of ductile machining as an optimal machining condition for precise productions of titanium alloys.

Dispersion toughened ceramic composites and method for making same

DOEpatents

Stinton, David P.; Lackey, Walter J.; Lauf, Robert J.

1986-01-01

Ceramic composites exhibiting increased fracture toughness are produced by the simultaneous codeposition of silicon carbide and titanium disilicide by chemical vapor deposition. A mixture of hydrogen, methyltrichlorosilane and titanium tetrachloride is introduced into a furnace containing a substrate such as graphite or silicon carbide. The thermal decomposition of the methyltrichlorosilane provides a silicon carbide matrix phase and the decomposition of the titanium tetrachloride provides a uniformly dispersed second phase of the intermetallic titanium disilicide within the matrix phase. The fracture toughness of the ceramic composite is in the range of about 6.5 to 7.0 MPa.sqroot.m which represents a significant increase over that of silicon carbide.

Dispersion toughened ceramic composites and method for making same

DOEpatents

Stinton, D.P.; Lackey, W.J.; Lauf, R.J.

1984-09-28

Ceramic composites exhibiting increased fracture toughness are produced by the simultaneous codeposition of silicon carbide and titanium disilicide by chemical vapor deposition. A mixture of hydrogen, methyltrichlorosilane and titanium tetrachloride is introduced into a furnace containing a substrate such as graphite or silicon carbide. The thermal decomposition of the methyltrichlorosilane provides a silicon carbide matrix phase and the decomposition of the titanium tetrachloride provides a uniformly dispersed second phase of the intermetallic titanium disilicide within the matrix phase. The fracture toughness of the ceramic composite is in the range of about 6.5 to 7.0 MPa..sqrt..m which represents a significant increase over that of silicon carbide.

In vitro bioactivity of a biocomposite fabricated from HA and Ti powders by powder metallurgy method.

PubMed

Ning, C Q; Zhou, Y

2002-07-01

Traditionally, hydroxyapatite was used as a coating material on titanium substrate by various techniques. In the present work, a biocomposite was successfully fabricated from hydroxyapatite and titanium powders by powder metallurgy method. Bioactivity of the composite in a simulated body fluid (SBF) was investigated. Main crystal phases of the as-fabricated composite are found to be Ti2O, CaTiO3, CaO, alpha-Ti and a TiP-like phase. When the composite is immersed in the simulated body fluid for a certain time, a poor-crystallized, calcium-deficient, carbonate-containing apatite film will form on the surface of the composite. The time required to induce apatite nucleation is within 2 h. In addition, the apatite is also incorporated with a little magnesium and chlorine element. It is found that Ti2O has the ability to induce the formation of bone-like apatite in the SBF. And a dissolve of the CaO phase could also provide favorable conditions for the apatite formation, by forming open pores on the surface of the composite and increasing the degree of supersaturation of the SBF with respect to the apatite.

The effect of hydrophilic titanium surface modification on macrophage inflammatory cytokine gene expression.

PubMed

Hamlet, Stephen; Alfarsi, Mohammed; George, Roy; Ivanovski, Saso

2012-05-01

Chemical modification of microrough titanium dental implants to produce a hydrophilic surface with increased wettability and improved surface energy has been demonstrated clinically to achieve superior bone wound healing and osseointegration compared to that achieved with a microrough titanium surface alone. As the recruitment of the necessary osseoinductive precursors involved in bone wound healing and osseointegration to the wound site is facilitated by the action of cytokines, this study sought to determine the in vitro effect of hydrophilic surface modification on the expression of pro-inflammatory cytokines from adherent macrophages. The surface topography and composition of the titanium surfaces was characterized by scanning electron microscopy and X-ray photoelectron spectroscopy. Macrophage attachment and proliferation was assessed using an MTT assay. The expression of 84 pro-inflammatory cytokines and chemokines by adherent RAW 264.7 cells, a murine leukaemic monocyte cell line, was assessed by PCR array after 24 h culture on either smooth polished, sand-blasted acid-etched (SLA) or hydrophilic-modified SLA (SLActive) titanium surfaces. Following 24 h culture on titanium, surface microroughness activated pro-inflammatory cytokine gene transcription in RAW 264.7 cells. Although there was no significant difference in the degree of cellular attachment or proliferation of RAW 264.7 cells to the different titanium surfaces, by 24 h the hydrophilic surface elicited a gene expression profile with significant down-regulation of the key pro-inflammatory cytokines Tnfα, IL-1α, IL-1β and the chemokine Ccl-2. Down-regulation of the expression of pro-inflammatory cytokine genes may thus modulate the inflammatory response and may facilitate the enhanced bone wound healing and osseointegration observed clinically using implants with a microrough hydrophilic surface. © 2011 John Wiley & Sons A/S.

Surface Modification of Dental Titanium Implant by Layer-by-Layer Electrostatic Self-Assembly

PubMed Central

Shi, Quan; Qian, Zhiyong; Liu, Donghua; Liu, Hongchen

2017-01-01

In vivo implants that are composed of titanium and titanium alloys as raw materials are widely used in the fields of biology and medicine. In the field of dental medicine, titanium is considered to be an ideal dental implant material. Good osseointegration and soft tissue closure are the foundation for the success of dental implants. Therefore, the enhancement of the osseointegration and antibacterial abilities of titanium and its alloys has been the focus of much research. With its many advantages, layer-by-layer (LbL) assembly is a self-assembly technique that is used to develop multilayer films based on complementary interactions between differently charged polyelectrolytes. The LbL approach provides new methods and applications for the surface modification of dental titanium implant. In this review, the application of the LbL technique to surface modification of titanium including promoting osteogenesis and osseointegration, promoting the formation and healing of soft tissues, improving the antibacterial properties of titanium implant, achieving local drug delivery and sustained release is summarized. PMID:28824462

Removal of titanium plates coated with anodic titanium oxide ceramic: retrospective study.

PubMed

Velich, Norbert; Németh, Zsolt; Suba, Csongor; Szabó, György

2002-09-01

Transformation of the surface of metallic titanium with titanium oxides prepared in various ways is a modern procedure. For more than 15 years, the authors have been utilizing fixing elements coated with titanium oxide ceramics, prepared by anodic oxidation and thermal treatment, for purposes of jawbone osteosynthesis. The aim of the authors' work was to assess the extent to which the titanium oxide ceramic coating influences the fate of the plates used for osteosynthesis within the human organism, in regard to the possible need for their removal. During a 5-year period, 108 of 1,396 plates coated with anodic titanium oxide had to be removed for various reasons: plate exposure (47), osteomyelitis (25), palpable swelling and tenderness (21), patient request for psychological reasons (13), or fracture of the plate (2). In none of these 108 cases was metallosis observed, which otherwise is reported relatively frequently in the vicinity of traditional titanium fixing elements, nor was any tissue damage connected with the surface of the plates. The results indicate the favorable properties of the titanium oxide ceramic surface.

Bone Response to Surface-Modified Titanium Implants: Studies on the Early Tissue Response to Implants with Different Surface Characteristics

PubMed Central

Larsson Wexell, C.; Thomsen, P.; Aronsson, B.-O.; Tengvall, P.; Rodahl, M.; Lausmaa, J.; Kasemo, B.; Ericson, L. E.

2013-01-01

In a series of experimental studies, the bone formation around systematically modified titanium implants is analyzed. In the present study, three different surface modifications were prepared and evaluated. Glow-discharge cleaning and oxidizing resulted in a highly stoichiometric TiO2 surface, while a glow-discharge treatment in nitrogen gas resulted in implants with essentially a surface of titanium nitride, covered with a very thin titanium oxide. Finally, hydrogen peroxide treatment of implants resulted in an almost stoichiometric TiO2, rich in hydroxyl groups on the surface. Machined commercially pure titanium implants served as controls. Scanning Auger Electron Spectroscopy, Scanning Electron Microscopy, and Atomic Force Microscopy revealed no significant differences in oxide thickness or surface roughness parameters, but differences in the surface chemical composition and apparent topography were observed. After surface preparation, the implants were inserted in cortical bone of rabbits and evaluated after 1, 3, and 6 weeks. Light microscopic evaluation of the tissue response showed that all implants were in contact with bone and had a large proportion of newly formed bone within the threads after 6 weeks. There were no morphological differences between the four groups. Our study shows that a high degree of bone contact and bone formation can be achieved with titanium implants of different surface composition and topography. PMID:24174936

Potentiodynamic Polarization Studies and Surface Chemical Composition of Bismuth Titanate (BixTiyOz) Films Produced through Radiofrequency Magnetron Sputtering

PubMed Central

Alfonso, José E.; Olaya, Jhon J.; Pinzón, Manuel J.; Marco, José F.

2013-01-01

The applications of Bismuth Titanate (BixTiyOz) materials have been focused on their electronic and optical properties, but with respect to the use of these compounds in applications like corrosion resistance, have been very few or nonexistent. For this reason, in the present investigation BixTiyOz thin films were deposited using RF magnetron sputtering onto silicon wafers, stainless steel 316L, and titanium alloy (Ti6Al4V) substrates, in order to carry out a study of the corrosion behavior of this compound. The structural properties of the coatings were studied through X-ray diffraction (XRD), the morphology was determined using Scanning Electron Microscopy (SEM), the corrosion resistance behavior of the coated and uncoated substrates was evaluated via the Potentiodynamic Polarization technique, and surface chemical composition was evaluated through X-ray photoelectron spectroscopy (XPS). The XRD results indicated that the films were amorphous. The SEM micrographs showed that the deposited films were homogeneous, but in some cases there were cracks. The potentiodynamic polarization technique showed that the corrosion current in the coated substrates decreased by an order of two magnitudes with respect to the uncoated substrates, but in both cases the corrosion mechanism was pitting due to the pores in the film. The XPS analysis shows that the deposited films contain both Bi3+ and Ti4+. PMID:28788338

Potentiodynamic Polarization Studies and Surface Chemical Composition of Bismuth Titanate (Bi x Ti y O z ) Films Produced through Radiofrequency Magnetron Sputtering.

PubMed

Alfonso, José E; Olaya, Jhon J; Pinzón, Manuel J; Marco, José F

2013-10-08

The applications of Bismuth Titanate (Bi x Ti y O z ) materials have been focused on their electronic and optical properties, but with respect to the use of these compounds in applications like corrosion resistance, have been very few or nonexistent. For this reason, in the present investigation Bi x Ti y O z thin films were deposited using RF magnetron sputtering onto silicon wafers, stainless steel 316L, and titanium alloy (Ti₆Al₄V) substrates, in order to carry out a study of the corrosion behavior of this compound. The structural properties of the coatings were studied through X-ray diffraction (XRD), the morphology was determined using Scanning Electron Microscopy (SEM), the corrosion resistance behavior of the coated and uncoated substrates was evaluated via the Potentiodynamic Polarization technique, and surface chemical composition was evaluated through X-ray photoelectron spectroscopy (XPS). The XRD results indicated that the films were amorphous. The SEM micrographs showed that the deposited films were homogeneous, but in some cases there were cracks. The potentiodynamic polarization technique showed that the corrosion current in the coated substrates decreased by an order of two magnitudes with respect to the uncoated substrates, but in both cases the corrosion mechanism was pitting due to the pores in the film. The XPS analysis shows that the deposited films contain both Bi 3+ and Ti 4+ .

Influence of mechanical instruments on the biocompatibility of titanium dental implants surfaces: a systematic review.

PubMed

Louropoulou, Anna; Slot, Dagmar E; Van der Weijden, Fridus

2015-07-01

The objective of this systematic review was to evaluate the effect of mechanical instruments on the biocompatibility of titanium dental implant surfaces. MEDLINE, Cochrane-CENTRAL and EMBASE databases were searched up to December 2013, to identify controlled studies on the ability of cells to adhere and colonize non-contaminated and contaminated, smooth and rough, titanium surfaces after instrumentation with different mechanical instruments. A comprehensive search identified 1893 unique potential papers. Eleven studies met the inclusion criteria and were selected for this review. All studies were in vitro studies. Most studies used titanium discs, strips and cylinders. The air abrasive was the treatment mostly evaluated. The available studies had a high heterogeneity which precluded any statistical analysis of the data. Therefore, the conclusions are not based on quantitative data. Instrumentation seems to have a selective influence on the attachment of different cells. In the presence of contamination, plastic curettes, metal curettes, rotating titanium brushes and an ultrasonic scaling system with a carbon tip and polishing fluid seem to fail to restore the biocompatibility of rough titanium surfaces. The air-powder abrasive system with sodium bicarbonate powder does not seem to affect the fibroblast-titanium surface interaction after treatment of smooth or rough surfaces, even in the presence of contamination. The available data suggest that treatment with an air-powder abrasive system with sodium bicarbonate powder does not seem to adversely affect the biocompatibility of titanium dental implant surfaces. However, the clinical impact of these findings requires further clarification. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

A feasibility study for in vitro evaluation of fixation between prosthesis and bone with bone marrow-derived mesenchymal stem cells.

PubMed

Morita, Yusuke; Yamasaki, Kenichi; Hattori, Koji

2010-10-01

It is difficult to quantitatively evaluate adhesive strength between an implant and the neighboring bone using animal experiments, because the degree of fixation of an implant depends on differences between individuals and the clearance between the material and the bone resulting from surgical technique. A system was designed in which rat bone marrow cells were used to quantitatively evaluate the adhesion between titanium alloy plates and bone plates in vitro. Three kinds of surface treatment were used: a sand-blasted surface, a titanium-sprayed surface and a titanium-sprayed surface coated with hydroxyapatite. Bone marrow cells obtained from rat femora were seeded on the titanium alloy plates, and the cells were cultured between the titanium alloy plates and the bone plates sliced from porcine ilium for 2 weeks. After cultivation, adhesive strength was measured using a tensile test, after which DNA amount and Alkaline phosphatase activity were measured. The seeded cells accelerated adhesion of the titanium alloy plate to the bone plate. Adhesive strength of the titanium-sprayed surface was lower than that of the sand-blasted surface because of lower initial contact area, although there was no difference in Alkaline phosphatase activity between two surface treatments. A hydroxyapatite coating enhanced adhesive strength between the titanium alloy palate and the bone plate, as well as enhancing osteogenic differentiation of bone marrow cells. It is believed that this novel experimental method can be used to simultaneously evaluate the osteogenic differentiation and the adhesive strength of an implant during in vitro cultivation. 2010 Elsevier Ltd. All rights reserved.

Surface treatment of a titanium implant using low temperature atmospheric pressure plasmas

NASA Astrophysics Data System (ADS)

Lee, Hyun-Young; Tang, Tianyu; Ok, Jung-Woo; Kim, Dong-Hyun; Lee, Ho-Jun; Lee, Hae June

2015-09-01

During the last two decades, atmospheric pressure plasmas(APP) are widely used in diverse fields of biomedical applications, reduction of pollutants, and surface treatment of materials. Applications of APP to titanium surface of dental implants is steadily increasing as it renders surfaces wettability and modifies the oxide layer of titanium that hinders the interaction with cells and proteins. In this study, we have treated the titanium surfaces of screw-shaped implant samples using a plasma jet which is composed of a ceramic coaxial tube of dielectrics, a stainless steel inner electrode, and a coper tube outer electrode. The plasma ignition occurred with Ar gas flow between two coaxial metal electrodes and a sinusoidal bias voltage of 3 kV with a frequency of 20 kHz. Titanium materials used in this study are screw-shaped implants of which diameter and length are 5 mm and 13 mm, respectively. Samples were mounted at a distance of 5 mm below the plasma source, and the plasma treatment time was set to 3 min. The wettability of titanium surface was measured by the moving speed of water on its surface, which is enhanced by plasma treatment. The surface roughness was also measured by atomic force microscopy. The optimal condition for wettability change is discussed.

Effect of Electric Field on the Wetting Behavior of Eutectic Gallium-Indium Alloys in Aqueous Environment

NASA Astrophysics Data System (ADS)

Yuan, Bo; He, Zhi-Zhu; Liu, Jing

2018-02-01

Room-temperature liquid metals have many intriguing properties that have not previously been fully understood. Among them, surface tension behaviors of such metals are especially critical in a group of newly emerging areas such as printed electronics, functional materials and soft machines, etc. This study is dedicated to clarifying the wettability of liquid metals on various substrate surfaces with varied roughness immersed in solutions when subject to an electric field. The contact angles of Ga75.5In24.5 in several typical liquids were comprehensively measured and interpreted, and were revealed to be affected by the components and concentration of the environmental solution. Meanwhile, the roughness of the substrates is also revealed to be an important parameter dominating the process. The dynamic wetting behaviors of liquid metal in aqueous environment under an electric field were quantified. The contact angle values of eutectic gallium-indium alloys (eGaIn) on titanium substrates with different roughness would lead to better electrowetting performances on rougher surfaces. In particular, using an electrical field to control the wetting status of liquid metal with the matching substrate have been illustrated, which would offer a practical way to flexibly control liquid metal-based functional devices working in an aqueous environment. Furthermore, Lippmann-Young's equation reveals the relationship between contact angle and applied voltage, explaining the excellent electrowetting property of eGaIn. The power law, R = αt β , was adopted to characterize the two-stage wetting process of eGaIn under different voltages. In the initial process, β ≈ 1/2 represents the complete wetting law, while the later one, β ≈ 1/10, meets with Tanner's law of a drop spontaneously spreading on a smooth surface.

Double-chimera proteins to enhance recruitment of endothelial cells and their progenitor cells.

PubMed

Behjati, M; Kazemi, M; Hashemi, M; Zarkesh-Esfahanai, S H; Bahrami, E; Hashemi-Beni, B; Ahmadi, R

2013-08-20

Enhanced attraction of selective vascular reparative cells is of great importance in order to increase vascular patency after endovascular treatments. We aimed to evaluate efficient attachment of endothelial cells and their progenitors on surfaces coated with mixture of specific antibodies, L-selectin and VE-cadherin, with prohibited platelet attachment. The most efficient conditions for coating of L-selectin-Fc chimera and VE-cadherin-Fc chimera proteins were first determined by protein coating on ELISA plates. The whole processes were repeated on titanium substrates, which are commonly used to coat stents. Endothelial progenitor cells (EPCs) and human umbilical vein endothelial cells (HUVECs) were isolated and characterized by flow cytometry. Cell attachment, growth, proliferation, viability and surface cytotoxicity were evaluated using nuclear staining and MTT assay. Platelet and cell attachment were evaluated using scanning electron microscopy. Optimal concentration of each protein for surface coating was 50 ng/ml. The efficacy of protein coating was both heat and pH independent. Calcium ions had significant impact on simultaneous dual-protein coating (P<0.05). Coating stability data revealed more than one year stability for these coated proteins at 4°C. L-selectin and VE-cadherin (ratio of 50:50) coated surface showed highest EPC and HUVEC attachment, viability and proliferation compared to single protein coated and non-coated titanium surfaces (P<0.05). This double coated surface did not show any cytotoxic effect. Surfaces coated with L-selectin and VE-cadherin are friendly surface for EPC and endothelial cell attachment with less platelet attachment. These desirable factors make the L-selectin and VE-cadherin coated surfaces perfect candidate endovascular device. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Glow discharge plasma pretreatment enhances osteoclast differentiation and survival on titanium plates.

PubMed

Kawai, Hiroyuki; Shibata, Yo; Miyazaki, Takashi

2004-05-01

Despite the fact that several reports have demonstrated osteoclast activity on various bioactive ceramics, osteoclast functions on surface-modified titanium have not come under focus. This study aimed to examine whether the increasing surface energy of glow discharge plasma (GDP) involved in protein adhesion containing the RGD (Arg-Gly-Asp) sequence affects osteoclast responses on titanium plates. We examined osteoclast differentiation and survival rates on titanium plates with and without GDP. The amounts of osteoclasts on titanium plates were not increased by GDP after 1 week. However, osteoclast differentiation was greatly activated by GDP pretreatment, as tartrate-resistant acid phosphatase synthesis significantly increased on the titanium plates with GDP. Additionally, since the presence of osteoclasts was detected only on the titanium plates with GDP, even after 4h cultivation in a coculture test, the osteoclasts survival rate was increased by GDP pretreatment. As osteoclast responses were affected even on surface modified metallic materials, we concluded that novel approaches are needed not only for osteoclastic resorption on ceramic materials but also for osteoclast responses on surface-modified metallic materials.

Effect of doping on the photocatalytic, electronic and mechanical properties of sol-gel titanium dioxide films

NASA Astrophysics Data System (ADS)

Kurtoglu, Murat

Heterogeneous photocatalysis has been an active research area over the last decade as a promising solution for energy generation and environmental problems which has led to promising applications from air and water purification systems, self-cleaning and self-sterilizing surfaces to solar cells and hydrogen production from water dissociation reaction. Titanium dioxide (TiO2), an abundant material with a high photocatalytic efficiency and chemical stability, is undoubtedly the most widely studied and used among all photocatalytic materials. Although titanium dioxide has been used in powder form, its immobilized form (film) is necessary from practical application standpoint. However, there are several shortcomings of titanium dioxide films that need to be addressed to realize a wide range of successful applications: lack of visible light activity, poisoning of the catalytic performance by the substrate and the low surface area compared to powder forms. In addition, mechanical properties of such films have not been investigated thoroughly, which may be critical when abrasion and weathering resistance are necessary. To address each of these issues, a systematic experimental and theoretical investigation of doping titanium dioxide films with a variety of elements were conducted. Utilizing theoretical calculations to filter elements for experimental studies as well as interpretation of the experimental results, several dopant or dopant combinations were found to remedy some of the issues of photocatalytic titanium dioxide films. Doping with 32 metals, nitrogen and 11 metal-nitrogen combinations are investigated theoretically and the results are used as guideline for the experimental studies. Particular attention is given to certain metal dopants such as Cr, V, Mo, Ta and Ga not just because of their relatively modest cost but also their non-toxicity and wide availability of their compatible compounds for sol-gel synthesis. While metal-dopants improved the overall efficiency and mechanical properties of titanium dioxide films, visible light activity is only achieved with nitrogen and metal-nitrogen doping where some of the metal co-dopants significantly improved the overall photocatalytic efficiency compared to nitrogen-only doped films. In addition, majority of the experimental studies is accompanied by nanoindentation technique to study the effect of doping and calcination on the key mechanical properties of titanium dioxide films. It is shown that good mechanical properties---good photocatalytic activity combinations can be achieved by a choice of appropriate dopant---dopant combinations and coupled with appropriate calcination parameters. Results of the theoretical and experimental investigations led to the development of first commercial photocatalytic tableware glass items which can be utilized under indoor lighting conditions by carefully selecting metal-nitrogen couples for doping of titanium dioxide films.

Surface patterning by pulsed-laser-induced transfer of metals and compounds

NASA Astrophysics Data System (ADS)

Toth, Zsolt; Mogyorosi, Peter; Szoerenyi, Tamas

1990-08-01

Besults of a systematic study on Q-switched nthy laser induced rrrn2 area transfer of supported titanium and chranium thin films and Ge/Se multilayer structures are reported. The appearance of the prints is governed by film-support adhesion and source-target spacing. Best quality prints are produced by ablating well adhering ntal films in close proximity ( spacing < 15 pm) to the target to be patterned. Transfer fran stacked elenntaxy layers as a source offers a unique possibility of depositing acinpound films by mixing the constituents and transferring the material onto the target substrate in a single step.

Adhesion between a rutile surface and a polyimide: a coarse grained molecular dynamics study

NASA Astrophysics Data System (ADS)

Kumar, Arun; Sudarkodi, V.; Parandekar, Priya V.; Sinha, Nishant K.; Prakash, Om; Nair, Nisanth N.; Basu, Sumit

2018-04-01

Titanium, due to its high strength to weight ratio and polyimides, due to their excellent thermal stability are being increasingly used in aerospace applications. We investigate the bonding between a (110) rutile substrate and a popular commercial polyimide, PMR-15, starting from the known atomic structure of the rutile substrate and the architecture of the polymer. First, the long PMR-15 molecule is divided into four fragments and an all-atom non-bonded forcefield governing the interaction between PMR-15 and a rutile substrate is developed. To this end, parameters of Buckingham potential for interaction between each atom in the fragments and the rutile surface are fitted, so as to ensure that the sum of non-bonded and electrostatic interaction energy between the substrate and a large number of configurations of each fragment, calculated by the quantum mechanical route and obtained from the fitted potential, is closely matched. Further, two coarse grained models of PMR-15 are developed—one for interaction between two coarse grained PMR-15 molecules and another for that between a coarse grained PMR-15 and the rutile substrate. Molecular dynamics simulations with the coarse grained models yields a traction separation law—a very useful tool for conducting continuum level finite element simulations of rutile-PMR-15 joints—governing the normal separation of a PMR-15 block from a flat rutile substrate. Moreover, detailed information about the affinity of various fragments to the substrate are also obtained. In fact, though the separation energy between rutile and PMR-15 turns out to be rather low, our analysis—with merely the molecular architecture of the polyimide as the starting point—provides a scheme for in-silico prediction of adhesion energies for new polyimide formulations.

Effect of plastic-covered ultrasonic scalers on titanium implant surfaces.

PubMed

Mann, M; Parmar, D; Walmsley, A D; Lea, S C

2012-01-01

Maintaining oral health around titanium implants is essential. The formation of a biofilm on the titanium surface will influence the continuing success of the implant. These concerns have led to modified ultrasonic scaler instruments that look to reduce implant damage while maximising the cleaning effect. This study aimed to assess the effect of instrumentation, with traditional and modified ultrasonic scalers, on titanium implant surfaces and to correlate this with the oscillations of the instruments. Two ultrasonic insert designs (metallic TFI-10 and a plastic-tipped implant insert) were selected. Each scaler probe was scanned using a scanning laser vibrometer, under loaded and unloaded conditions, to determine their oscillation characteristics. Loads were applied against a titanium implant (100g and 200 g) for 10 s. The resulting implant surfaces were then scanned using laser profilometry and scanning electron microscopy (SEM). Insert probes oscillated with an elliptical motion with the maximum amplitude at the probe tip. Laser profilometry detected defects in the titanium surface only for the metallic scaler insert. Defect widths at 200 g high power were significantly larger than all other load/power conditions (P<0.02). Using SEM, it was observed that modifications to the implant surface had occurred following instrumentation with the plastic-tipped insert. Debris was also visible around the defects. Metal scalers produce defects in titanium implant surfaces and load and power are important factors in the damage caused. Plastic-coated scaler probes cause minimal damage to implant surfaces and have a polishing action but can leave plastic deposits behind on the implant surface. © 2011 John Wiley & Sons A/S.

In vitro adhesion of fibroblastic cells to titanium alloy discs treated with sodium hydroxide.

PubMed

Al Mustafa, Maisa; Agis, Hermann; Müller, Heinz-Dieter; Watzek, Georg; Gruber, Reinhard

2015-01-01

Adhesion of osteogenic cells on titanium surfaces is a prerequisite for osseointegration. Alkali treatment can increase the hydrophilicity of titanium implant surfaces, thereby supporting the adhesion of blood components. However, it is unclear if alkali treatment also supports the adhesion of cells with a fibroblastic morphology to titanium. Here, we have used a titanium alloy (Ti-6AL-4V) processed by alkali treatment to demonstrate the impact of hydrophilicity on the adhesion of primary human gingival fibroblast and bone cells. Also included were the osteosarcoma and fibroblastoma cell lines, MG63 and L929, respectively. Cell adhesion was determined by scanning electron microscopy. We also measured viability, proliferation, and protein synthesis of the adherent cells. Alkali treatment increased the adhesion of gingival fibroblasts, bone cells, and the two cell lines when seeded onto the titanium alloy surface for 1 h. At 3 h, no significant changes in cell adhesion were observed. Cells grown for 1 day on the titanium alloy surfaces processed by alkali treatment behave similarly to untreated controls with regard to viability, proliferation, and protein synthesis. Based on these preliminary In vitro findings, we conclude that alkali treatment can support the early adhesion of cells with fibroblastic characteristics to a titanium alloy surface. © 2013 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Consolidation of Surface Coatings by Friction Stir Techniques

DTIC Science & Technology

2010-09-01

alloy samples were plasma sprayed with a Titanium-Nickel-Chrome coating or a Titanium coating. Single and multiple pass experiments were performed...based coatings onto the Aluminum alloy surface. Results showed that the most successful results were accomplished using a flat, pinless tool, with...properties. Aluminum alloy samples were plasma sprayed with a Titanium-Nickel-Chrome coating or a Titanium coating. Single and multiple pass experiments

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching.

PubMed

Nazarov, Denis V; Zemtsova, Elena G; Solokhin, Alexandr Yu; Valiev, Ruslan Z; Smirnov, Vladimir M

2017-01-13

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed.

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching

PubMed Central

Nazarov, Denis V.; Zemtsova, Elena G.; Solokhin, Alexandr Yu.; Valiev, Ruslan Z.; Smirnov, Vladimir M.

2017-01-01

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed. PMID:28336849

Surface Characterization of an Organized Titanium Dioxide Layer

NASA Astrophysics Data System (ADS)

Curtis, Travis

Soft lithographic printing techniques can be used to control the surface morphology of titanium dioxide layers on length scales of several hundred nanometers. Controlling surface morphology and volumetric organization of titanium dioxide electrodes can potentially be used in dye-sensitized solar cell devices. This thesis explores how layer-by-layer replication can lead to well defined, dimensionally controlled volumes and details how these control mechanisms influence surface characteristics of the semiconducting oxide.

Hydrogen leak detection using laser-induced breakdown spectroscopy.

PubMed

Ball, A J; Hohreiter, V; Hahn, D W

2005-03-01

Laser-induced breakdown spectroscopy (LIBS) is investigated as a technique for real-time monitoring of hydrogen gas. Two methodologies were examined: The use of a 100 mJ laser pulse to create a laser-induced breakdown directly in a sample gas stream, and the use of a 55 mJ laser pulse to create a laser-induced plasma on a solid substrate surface, with the expanding plasma sampling the gas stream. Various metals were analyzed as candidate substrate surfaces, including aluminum, copper, molybdenum, stainless steel, titanium, and tungsten. Stainless steel was selected, and a detailed analysis of hydrogen detection in binary mixtures of nitrogen and hydrogen at atmospheric pressure was performed. Both the gaseous plasma and the plasma initiated on the stainless steel surface generated comparable hydrogen emission signals, using the 656.28 Halpha emission line, and exhibited excellent signal linearity. The limit of detection is about 20 ppm (mass) as determined for both methodologies, with the solid-initiated plasma yielding a slightly better value. Overall, LIBS is concluded to be a viable candidate for hydrogen sensing, offering a combination of high sensitivity with a technique that is well suited to implementation in field environments.

Corrosive effects of fluoride on titanium under artificial biofilm.

PubMed

Fukushima, Azusa; Mayanagi, Gen; Sasaki, Keiichi; Takahashi, Nobuhiro

2018-01-01

This study aimed to investigate the effect of sodium fluoride (NaF) on titanium corrosion using a biofilm model, taking environmental pH into account. Streptococcus mutans cells were used as the artificial biofilm, and pH at the bacteria-titanium interface was monitored after the addition of 1% glucose with NaF (0, 225 or 900ppmF) at 37°C for 90min. In an immersion test, the titanium samples were immersed in the NaF solution (0, 225 or 900ppm F; pH 4.2 or 6.5) for 30 or 90min. Before and after pH monitoring or immersion test, the electrochemical properties of the titanium surface were measured using a potentiostat. The amount of titanium eluted into the biofilm or the immersion solution was measured using inductively coupled plasma mass spectrometry. The color difference (ΔE*ab) and gloss of the titanium surface were determined using a spectrophotometer. After incubation with biofilm, pH was maintained at around 6.5 in the presence of NaF. There was no significant change in titanium surface and elution, regardless of the concentration of NaF. After immersion in 900ppm NaF solution at pH 4.2, corrosive electrochemical change was induced on the surface, titanium elution and ΔE*ab were increased, and gloss was decreased. NaF induces titanium corrosion in acidic environment in vitro, while NaF does not induce titanium corrosion under the biofilm because fluoride inhibits bacterial acid production. Neutral pH fluoridated agents may still be used to protect the remaining teeth, even when titanium-based prostheses are worn. Copyright © 2017 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

The influence of surface area, porous structure, and surface state on the supercapacitor performance of titanium oxynitride: implications for a nanostructuring strategy.

PubMed

Lee, Eun Joo; Lee, Lanlee; Abbas, Muhammad Awais; Bang, Jin Ho

2017-08-09

A recent surge of interest in metal (oxy)nitride materials for energy storage devices has given rise to the rapid development of various nanostructuring strategies for these materials. In supercapacitor applications, early transition metal (oxy)nitrides have been extensively explored, among which titanium oxynitride stands out due to its great potential for charge storage. Despite recent advances in supercapacitors based on titanium oxynitride, many underlying factors governing their capacitive performance remain elusive. In this work, nanostructured titanium oxynitride is prepared by firing an organic-inorganic hybrid precursor under a hot ammonia atmosphere, and the influence of its physical characteristics on the supercapacitor performance is investigated. New insights into the effects of surface area, porous structure, and surface state of titanium oxynitride on the supercapacitor performance are revealed through which a comprehensive understanding about the capacitive behavior of titanium oxynitride is provided. In addition, the implications of these insights for a nanostructuring strategy striving for higher capacitance and improved stability are discussed.

Effects of UV Aging on the Cracking of Titanium Oxide Layer on Poly(ethylene terephthalate) Substrate: Preprint

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Chao; Gray, Matthew H.; Tirawat, Robert

Thin oxide and metal films deposited on polymer substrates is an emerging technology for advanced reflectors for concentrated solar power applications, due to their unique combination of light weight, flexibility and inexpensive manufacture. Thus far, there is little knowledge on the mechanical integrity or structural persistence of such multi-layer thin film systems under long-term environmental aging. In this paper, the cracking of a brittle titanium dioxide layer deposited onto elasto-plastic poly(ethylene terephthalate) (PET) substrate is studied through a combination of experiment and modeling. In-situ fragmentation tests have been conducted to monitor the onset and evolution of cracks both on pristinemore » and on samples aged with ultraviolet (UV) light. An analytical model is presented to simulate the cracking behavior and to predict the effects of UV aging. Based on preliminary experimental observation, the effect of aging is divided into three aspects and analyzed independently: mechanical property degradation of the polymer substrate; degradation of the interlayer between substrate and oxide coating; and internal stress-induced cracks on the oxide coating.« less

Electrophoretic Deposition of Hydroxyapatite Film Containing Re-Doped MoS₂ Nanoparticles.

PubMed

Shalom, Hila; Feldman, Yishay; Rosentsveig, Rita; Pinkas, Iddo; Kaplan-Ashiri, Ifat; Moshkovich, Alexey; Perfilyev, Vladislav; Rapoport, Lev; Tenne, Reshef

2018-02-26

Films combining hydroxyapatite (HA) with minute amounts (ca. 1 weight %) of (rhenium doped) fullerene-like MoS₂ (IF) nanoparticles were deposited onto porous titanium substrate through electrophoretic process (EPD). The films were analyzed by scanning electron microscopy (SEM), X-ray diffraction and Raman spectroscopy. The SEM analysis showed relatively uniform coatings of the HA + IF on the titanium substrate. Chemical composition analysis using energy dispersive X-ray spectroscopy (EDS) of the coatings revealed the presence of calcium phosphate minerals like hydroxyapatite, as a majority phase. Tribological tests were undertaken showing that the IF nanoparticles endow the HA film very low friction and wear characteristics. Such films could be of interest for various medical technologies. Means for improving the adhesion of the film to the underlying substrate and its fracture toughness, without compromising its biocompatibility are discussed at the end.

Adherence of sputtered titanium carbides

NASA Technical Reports Server (NTRS)

Brainard, W. A.; Wheeler, D. R.

1979-01-01

The study searches for interface treatment that would increase the adhesion of TiC coating to nickel- and titanium-base alloys. Rene 41 (19 wt percent Cr, 11 wt percent Mo, 3 wt percent Ti, balance Ni) and Ti-6Al-4V (6 wt percent Al, 4 wt percent V, balance Ti) are considered. Adhesion of the coatings is evaluated in pin-and disk friction tests. The coatings and interface regions are examined by X-ray photoelectron spectroscopy. Results suggest that sputtered refractory compound coatings adhere best when a mixed compound of coating and substrate metals is formed in the interfacial region. The most effective type of refractory compound interface appears to depend on both substrate and coating material. A combination of metallic interlayer deposition and mixed compound interface formation may be more effective for some substrate coating combinations than either alone.

Effect of Laser Power and Scan Speed on Melt Pool Characteristics of Commercially Pure Titanium (CP-Ti)

NASA Astrophysics Data System (ADS)

Kusuma, Chandrakanth; Ahmed, Sazzad H.; Mian, Ahsan; Srinivasan, Raghavan

2017-07-01

Selective laser melting (SLM) is an additive manufacturing technique that creates complex parts by selectively melting metal powder layer-by-layer using a laser. In SLM, the process parameters decide the quality of the fabricated component. In this study, single beads of commercially pure titanium (CP-Ti) were melted on a substrate of the same material using an in-house built SLM machine. Multiple combinations of laser power and scan speed were used for single bead fabrication, while the laser beam diameter and powder layer thickness were kept constant. This experimental study investigated the influence of laser power, scan speed, and laser energy density on the melt pool formation, surface morphology, geometry (width and height), and hardness of solidified beads. In addition, the observed unfavorable effect such as inconsistency in melt pool width formation is discussed. The results show that the quality, geometry, and hardness of solidified melt pool are significantly affected by laser power, scanning speed, and laser energy density.

Fabrication of a biomimetic ZeinPDA nanofibrous scaffold impregnated with BMP-2 peptide conjugated TiO2 nanoparticle for bone tissue engineering.

PubMed

Babitha, S; Annamalai, Meenakshi; Dykas, Michal Marcin; Saha, Surajit; Poddar, Kingshuk; Venugopal, Jayarama Reddy; Ramakrishna, Seeram; Venkatesan, Thirumalai; Korrapati, Purna Sai

2018-04-01

A biomimetic Zein polydopamine based nanofiber scaffold was fabricated to deliver bone morphogenic protein-2 (BMP-2) peptide conjugated titanium dioxide nanoparticles in a sustained manner for investigating its osteogenic differentiation potential. To prolong its retention time at the target site, BMP-2 peptide has been conjugated to titanium dioxide nanoparticles owing to its high surface to volume ratio. The effect of biochemical cues from BMP-2 peptide and nanotopographical stimulation of electrospun Zein polydopamine nanofiber were examined for its enhanced osteogenic expression of human fetal osteoblast cells. The sustained delivery of bioactive signals, improved cell adhesion, mineralization, and differentiation could be attributed to its highly interconnected nanofibrous matrix with unique material composition. Further, the expression of osteogenic markers revealed that the fabricated nanofibrous scaffold possess better cell-biomaterial interactions. These promising results demonstrate the potential of the composite nanofibrous scaffold as an effective biomaterial substrate for bone regeneration. Copyright © 2017 John Wiley & Sons, Ltd.

Laser Surface Alloying of Copper, Manganese, and Magnesium with Pure Aluminum Substrate

NASA Astrophysics Data System (ADS)

Jiru, Woldetinsay G.; Sankar, M. Ravi; Dixit, Uday S.

2016-03-01

Laser surface alloying is one of the recent technologies used in the manufacturing sector for improving the surface properties of the metals. Light weight materials like aluminum alloys, titanium alloys, and magnesium alloys are used in the locomotive, aerospace, and structural applications. In the present work, an experimental study was conducted to improve the surface hardness of commercially pure aluminum plate. CO2 laser is used to melt pre-placed powders of pure copper, manganese, and magnesium. Microstructure of alloyed surface was analyzed using optical microscope. The best surface alloying was obtained at the optimum values of laser parameters, viz., laser power, scan speed, and laser beam diameter. In the alloyed region, microhardness increased from 30 HV0.5 to 430 HV0.5, while it was 60 HV0.5 in the heat-affected region. Tensile tests revealed some reduction in the strength and total elongation due to alloying. On the other hand, corrosion resistance improved.

The Effects of Different Wavelength UV Photofunctionalization on Micro-Arc Oxidized Titanium

PubMed Central

Zhou, Lei; Guo, Zehong; Rong, Mingdeng; Liu, Xiangning; Lai, Chunhua; Ding, Xianglong

2013-01-01

Many challenges exist in improving early osseointegration, one of the most critical factors in the long-term clinical success of dental implants. Recently, ultraviolet (UV) light-mediated photofunctionalization of titanium as a new potential surface treatment has aroused great interest. This study examines the bioactivity of titanium surfaces treated with UV light of different wavelengths and the underlying associated mechanism. Micro-arc oxidation (MAO) titanium samples were pretreated with UVA light (peak wavelength of 360 nm) or UVC light (peak wavelength of 250 nm) for up to 24 h. UVC treatment promoted the attachment, spread, proliferation and differentiation of MG-63 osteoblast-like cells on the titanium surface, as well as the capacity for apatite formation in simulated body fluid (SBF). These biological influences were not observed after UVA treatment, apart from a weaker effect on apatite formation. The enhanced bioactivity was substantially correlated with the amount of Ti-OH groups, which play an important role in improving the hydrophilicity, along with the removal of hydrocarbons on the titanium surface. Our results showed that both UVA and UVC irradiation altered the chemical properties of the titanium surface without sacrificing its excellent physical characteristics, suggesting that this technology has extensive potential applications and merits further investigation. PMID:23861853

Decreased fibrous encapsulation and enhanced osseointegration in vitro by decorin-modified titanium surface.

PubMed

He, Ronghan; Lu, Yunxiang; Ren, Jianhua; Wang, Zhe; Huang, Junqi; Zhu, Lei; Wang, Kun

2017-07-01

Orthopedic implants, using materials such as titanium, are extensively used in clinical surgeries. Despite its popularity, titanium is still inadequate to reliable osseointegration due to aseptic loosing. Fibrous encapsulation on the titanium implant interface prevents osseointegration and leads to the loosing of orthopedic implant. In this study, decorin was loaded on titanium surface by polydopamine film to examine fibrous encapsulation inhibition and bone growth acceleration. The coating of decorin was evaluated by X-ray photoelectron spectroscopy (XPS) and fluorescence microscopy. Quantitative analysis showed increased decorin coating on titanium surface when decorin in the loading solution increases. To test the effect of decorin modification, fibroblast and osteoblast cultures were utilized in vitro. The results showed that the functions of fibroblasts (proliferation, migration and collagen synthesis) were significantly attenuated on the decorin-modified surfaces and this anti-fibrous effect could be due to fibrotic gene suppression by decorin. In contrast, osteoblastic activities, such as calcium deposition and alkaline phosphatase (ALP) activity, were enhanced by the modified decorin. These results suggest that decorin coating on titanium surface inhibited proliferation and function of fibroblasts and improved that of osteoblasts. Therefore, this study is potentially useful for enhancing orthopedic implant. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimum surface roughness prediction for titanium alloy by adopting response surface methodology

NASA Astrophysics Data System (ADS)

Yang, Aimin; Han, Yang; Pan, Yuhang; Xing, Hongwei; Li, Jinze

Titanium alloy has been widely applied in industrial engineering products due to its advantages of great corrosion resistance and high specific strength. This paper investigated the processing parameters for finish turning of titanium alloy TC11. Firstly, a three-factor central composite design of experiment, considering the cutting speed, feed rate and depth of cut, are conducted in titanium alloy TC11 and the corresponding surface roughness are obtained. Then a mathematic model is constructed by the response surface methodology to fit the relationship between the process parameters and the surface roughness. The prediction accuracy was verified by the one-way ANOVA. Finally, the contour line of the surface roughness under different combination of process parameters are obtained and used for the optimum surface roughness prediction. Verification experimental results demonstrated that material removal rate (MRR) at the obtained optimum can be significantly improved without sacrificing the surface roughness.

In vitro osteoinduction of human mesenchymal stem cells in biomimetic surface modified titanium alloy implants.

PubMed

Santander, Sonia; Alcaine, Clara; Lyahyai, Jaber; Pérez, Maria Angeles; Rodellar, Clementina; Doblaré, Manuel; Ochoa, Ignacio

2012-01-01

Interaction between cells and implant surface is crucial for clinical success. This interaction and the associated surface treatment are essential for achieving a fast osseointegration process. Several studies of different topographical or chemical surface modifications have been proposed previously in literature. The Biomimetic Advanced Surface (BAS) topography is a combination of a shot blasting and anodizing procedure. Macroroughness, microporosity of titanium oxide and Calcium/Phosphate ion deposition is obtained. Human mesenchymal stem cells (hMCSs) response in vitro to this treatment has been evaluated. The results obtained show an improved adhesion capacity and a higher proliferation rate when hMSCs are cultured on treated surfaces. This biomimetic modification of the titanium surface induces the expression of osteblastic differentiation markers (RUNX2 and Osteopontin) in the absence of any externally provided differentiation factor. As a main conclusion, our biomimetic surface modification could lead to a substantial improvement in osteoinduction in titanium alloy implants.

Surface modified stainless steels for PEM fuel cell bipolar plates

DOEpatents

Brady, Michael P [Oak Ridge, TN; Wang, Heli [Littleton, CO; Turner, John A [Littleton, CO

2007-07-24

A nitridation treated stainless steel article (such as a bipolar plate for a proton exchange membrane fuel cell) having lower interfacial contact electrical resistance and better corrosion resistance than an untreated stainless steel article is disclosed. The treated stainless steel article has a surface layer including nitrogen-modified chromium-base oxide and precipitates of chromium nitride formed during nitridation wherein oxygen is present in the surface layer at a greater concentration than nitrogen. The surface layer may further include precipitates of titanium nitride and/or aluminum oxide. The surface layer in the treated article is chemically heterogeneous surface rather than a uniform or semi-uniform surface layer exclusively rich in chromium, titanium or aluminum. The precipitates of titanium nitride and/or aluminum oxide are formed by the nitriding treatment wherein titanium and/or aluminum in the stainless steel are segregated to the surface layer in forms that exhibit a low contact resistance and good corrosion resistance.

Oxidation Resistant Ti-Al-Fe Diffusion Barrier for FeCrAlY Coatings on Titanium Aluminides

NASA Technical Reports Server (NTRS)

Brady, Michael P. (Inventor); Smialke, James L. (Inventor); Brindley, William J. (Inventor)

1996-01-01

A diffusion barrier to help protect titanium aluminide alloys, including the coated alloys of the TiAl gamma + Ti3Al (alpha2) class, from oxidative attack and interstitial embrittlement at temperatures up to at least 1000 C is disclosed. The coating may comprise FeCrAlX alloys. The diffusion barrier comprises titanium, aluminum, and iron in the following approximate atomic percent: Ti-(50-55)Al-(9-20)Fe. This alloy is also suitable as an oxidative or structural coating for such substrates.

Titanium nitride formation by a dual-stage femtosecond laser process

NASA Astrophysics Data System (ADS)

Hammouti, S.; Holybee, B.; Zhu, W.; Allain, J. P.; Jurczyk, B.; Ruzic, D. N.

2018-06-01

Formation of TiN by femtosecond laser processing in controlled gas atmosphere is reported. A dual-stage process was designed and aimed to first remove and restructure the native oxide layer of titanium surface through laser irradiation under an argon-controlled atmosphere, and then to maximize titanium nitride formation through an irradiation under a nitrogen reactive environment. An extensive XPS study was performed to identify and quantify laser-induced titanium surface chemistry modifications after a single-stage laser process (Ar and N2 individually), and a dual-stage laser process. The importance of each step that composes the dual-stage laser process was demonstrated and leads to the dual-stage laser process for the formation of TiO, Ti2O3 and TiN. In this study, the largest nitride formation occurs for the dual stage process with laser conditions at 4 W/1.3 J cm-2 under argon and 5 W/1.6 J cm-2 under nitrogen, yielding a total TiN composition of 8.9%. Characterization of both single-stage and dual-stage laser process-induced surface morphologies has been performed as well, leading to the observation of a wide range of hierarchical surface structures such as high-frequency ripples, grooves, protuberances and pillow-like patterns. Finally, water wettability was assessed by means of contact angle measurements on untreated titanium surface, and titanium surfaces resulting from either single-stage laser process or dual-stage laser process. Dual-stage laser process allows a transition of titanium surface, from phobic (93°) to philic (35°), making accessible both hydrophilic and chemically functionalized hierarchical surfaces.

Novel antioxidant capability of titanium induced by UV light treatment.

PubMed

Ueno, Takeshi; Ikeda, Takayuki; Tsukimura, Naoki; Ishijima, Manabu; Minamikawa, Hajime; Sugita, Yoshihiko; Yamada, Masahiro; Wakabayashi, Noriyuki; Ogawa, Takahiro

2016-11-01

The intracellular production of reactive oxygen species (ROS) is a representative form of cellular oxidative stress and plays an important role in triggering adverse cellular events, such as the inflammatory reaction and delayed or compromised differentiation. Osteoblastic reaction to titanium with particular focus on ROS production remains unknown. Ultraviolet (UV) light treatment improves the physicochemical properties of titanium, specifically the induction of super hydrophilicity and removal of hydrocarbon, and eventually enhances its osteoconductivity. We hypothesized that there is a favorable regulatory change of ROS production within osteoblasts in contact with UV-treated titanium. Osteoblasts were cultured on titanium disks with or without UV-pretreatment. The intracellular production of ROS was higher on acid-etch-created rough titanium surfaces than on machine-prepared smooth ones. The ROS production was reduced by 40-50% by UV pretreatment of titanium regardless of the surface roughness. Oxidative DNA damage, as detected by 8-OHdG expression, was alleviated by 50% on UV-treated titanium surfaces. The expression of inflammatory cytokines was consistently lower in osteoblasts cultured on UV-treated titanium. ROS scavenger, glutathione, remained more without being depleted in osteoblasts on UV-treated titanium. Bio-burden test further showed that culturing osteoblasts on UV-treated titanium can significantly reduce the ROS production even with the presence of hydrogen peroxide, an oxidative stress inducer. These data suggest that the intracellular production of ROS and relevant inflammatory reaction, which unavoidably occurs in osteoblasts in contact with titanium, can be significantly reduced by UV pretreatment of titanium, implying a novel antioxidant capability of the particular titanium. Copyright © 2016 Elsevier Ltd. All rights reserved.

Bone response adjacent to calcium phosphate electrostatic spray deposition coated implants: an experimental study in goats.

PubMed

Manders, Peter J D; Wolke, Joop G C; Jansen, John A

2006-10-01

A new technique to deposit calcium phosphate (CaP) coatings onto titanium substrates has been developed recently. This electrostatic spray deposition (ESD) technique seems to be very promising. It appears to have clinical advantages such as an inexpensive and simple set-up, high deposition efficiency and the possibility to synthesize layers with a defined surface morphology. The aim of this study was to examine biological properties and osteoconductivity of ESD CaP coatings when inserted into the femoral condyle of a goat. Twenty-four implants with two gaps, i.e. 1 or 2 mm, were inserted into the femoral condyles of six goats. The implants were coated on one side with either a commercially available plasma-sprayed hydroxyapatite (HAPS) coating or an ESD carbonate apatite (CAESD) coating. The other side of the implant was always left uncoated (Ti). Twelve weeks after implantation the animals were sacrificed and the characteristics of bone ingrowth and bone contact were evaluated. At 3 months, histological and quantitative histomorphometrical measurements demonstrated more bone ingrowth and bone contact for coated sites as compared with uncoated sites. Statistical testing revealed that for both the 1 and 2 mm gaps HAPS (plasma-sprayed hydroxyapatite) as well as CAESD (ESD carbonate apatite) -coated surfaces always had a significantly higher (P<0.05) amount of bone contact than uncoated Ti surfaces. On HAPS surfaces always significantly more bone was present than on CAESD surfaces. Further statistical testing revealed a significant difference in bone ingrowth between the HAPS as well as CAESD and Ti 1+2 mm gap specimens (P<0.05). Further, HAPS 1 mm gaps showed more bone ingrowth than CAESD 1 mm gaps. No significant difference existed between HAPS and CAESD 2 mm gaps. On the basis of our observations, we conclude that the used ESD technique is a promising new method to deposit CaP coatings onto titanium substrates. On the other hand, plasma-spray HA-coated implants have a still more favourable effect on the bone response.

Present status of titanium removable dentures--a review of the literature.

PubMed

Ohkubo, C; Hanatani, S; Hosoi, T

2008-09-01

Although porcelain and zirconium oxide might be used for fixed partial dental prostheses instead of conventional dental metals in the near future, removable partial denture (RPD) frameworks will probably continue to be cast with biocompatible metals. Commercially pure (CP) titanium has appropriate mechanical properties, it is lightweight (low density) compared with conventional dental alloys, and has outstanding biocompatibility that prevents metal allergic reactions. This literature review describes the laboratory conditions needed for fabricating titanium frameworks and the present status of titanium removable prostheses. The use of titanium for the production of cast RPD frameworks has gradually increased. There are no reports about metallic allergy apparently caused by CP titanium dentures. The laboratory drawbacks still remain, such as the lengthy burn-out, inferior castability and machinability, reaction layer formed on the cast surface, difficulty of polishing, and high initial costs. However, the clinical problems, such as discoloration of the titanium surfaces, unpleasant metal taste, decrease of clasp retention, tendency for plaque to adhere to the surface, detachment of the denture base resin, and severe wear of titanium teeth, have gradually been resolved. Titanium RPD frameworks have never been reported to fail catastrophically. Thus, titanium is recommended as protection against metal allergy, particularly for large-sized prostheses such as RPDs or complete dentures.

Synthesis of embedded titanium dioxide nanoparticles by oxygen ion implantation in titanium films

NASA Astrophysics Data System (ADS)

Rukade, Deepti. A.; Desai, C. A.; Kulkarni, Nilesh; Tribedi, L. C.; Bhattacharyya, Varsha

2013-02-01

Thin films of titanium of 100nm thickness are deposited on fused silica substrates. These films are implanted by oxygen ions with implantation energy of 60keV obtained from ECR based highly charged ion accelerator. The implanted films are later annealed in a tube furnace to establish nanophase formation. The post implanted annealed films are characterized by UV-Visible Spectroscopy and Glancing Angle X-ray Diffraction technique (GAXRD). The phase formed and particle size is determined by GAXRD. Nanoparticle formation is confirmed by the UV-VIS spectroscopic analysis that shows quantum size effects in the form of a blue shift in the band-gap energy of titanium-oxide.

Hydrocarbon Deposition Attenuates Osteoblast Activity on Titanium

PubMed Central

Hayashi, R.; Ueno, T.; Migita, S.; Tsutsumi, Y.; Doi, H.; Ogawa, T.; Hanawa, T.; Wakabayashi, N.

2014-01-01

Although the reported percentage of bone-implant contact is far lower than 100%, the cause of such low levels of bone formation has rarely been investigated. This study tested the negative biological effect of hydrocarbon deposition onto titanium surfaces, which has been reported to be inevitable. Osteogenic MC3T3-E1 cells were cultured on titanium disks on which the carbon concentration was experimentally regulated to achieve carbon/titanium (C/Ti) ratios of 0.3, 0.7, and 1.0. Initial cellular activities such as cell attachment and cell spreading were concentration-dependently suppressed by the amount of carbon on the titanium surface. The osteoblastic functions of alkaline phosphatase activity and calcium mineralization were also reduced by more than 40% on the C/Ti (1.0) surface. These results indicate that osteoblast activity is influenced by the degree of hydrocarbon contamination on titanium implants and suggest that hydrocarbon decomposition before implant placement may increase the biocompatibility of titanium. PMID:24868012

Investigation of thermal spray coatings on austenitic stainless steel substrate to enhance corrosion protection

NASA Astrophysics Data System (ADS)

Rogers, Daniel M.

The research is aimed to evaluate thermal spray coatings to address material issues in supercritical and ultra-supercritical Rankine cycles. The primary purpose of the research is to test, evaluate, and eventually implement a coating to improve corrosion resistance and increase efficiency of coal fired power plants. The research is performed as part of a comprehensive project to evaluate the ability of titanium, titanium carbide, or titanium diboride powders to provide fireside corrosion resistance in supercritical and ultra-supercritical steam boilers, specifically, coal driven boilers in Illinois that must utilize high sulfur and high chlorine content coal. [1] The powder coatings that were tested are nano-sized titanium carbide (TiC) and titanium di-boride (TiB2) powders that were synthesized by a patented process at Southern Illinois University. The powders were then sent to Gas Technology Institute in Chicago to coat steel coupons by HVOF (High Velocity Oxy-Fuel) thermal spray technique. The powders were coated on an austenitic 304H stainless steel substrate which is commonly found in high temperature boilers, pipelines, and heat exchangers. The samples then went through various tests for various lengths of time under subcritical, supercritical, and ultra-supercritical conditions. The samples were examined using a scanning electron microscope and x-ray diffraction techniques to study microstructural changes and then determined which coating performed best.

Local induction of calcium phosphate formation on TiO2 coatings on titanium via surface treatment with a CO2 laser.

PubMed

Moritz, N; Jokinen, M; Peltola, T; Areva, S; Yli-Urpo, A

2003-04-01

Sol-gel-derived TiO(2) coatings are known to promote bonelike hydroxyapatite formation on their surfaces in vitro and in vivo. Hydroxyapatite integrates into bone tissue. In some clinical applications, the surface of an implant is simultaneously interfaced with soft and hard tissues, so it should match the properties of both. A new method is introduced for treating the coatings locally in a controlled manner. The local densification of sol-gel-derived titania coatings on titanium substrates with a CO(2) laser was studied in terms of the in vitro calcium phosphate-inducting properties. CO(2)-laser-treated multilayer coatings were compared with furnace-fired coatings prepared with the same recipe and previously shown to be bioactive. Additionally, local areas of furnace-fired multilayer coatings (previously shown to be bioactive in vitro) were further laser-treated to achieve various properties in the same implant. Topological surface properties were examined with atomic force microscopy. The formation of hydroxyapatite was studied with Fourier transform infrared and scanning electron microscopy energy-dispersive X-ray analysis. The results show that calcium phosphate formation can be adjusted locally by laser treatment. Calcium phosphate is a bonelike hydroxyapatite. The local treatment of sol-gel-derived coatings with a CO(2) laser is a promising technique for creating implants with various properties to interface different tissues and a possible way of coating implants that do not tolerate furnace firing. Copyright 2003 Wiley Periodicals, Inc.

Evaluation of modified titanium surfaces physical and chemical characteristics

NASA Astrophysics Data System (ADS)

Lukaszewska-Kuska, Magdalena; Leda, Bartosz; Gajdus, Przemyslaw; Hedzelek, Wieslaw

2017-11-01

Development of dental implantology is focused, among other things, on devising active surface of the implant, conditioning acceleration of the implant's integration with the bone. Increased roughness, characteristic for group of implants with developed surface, altered topography and chemically modified implant's surface determines increased implants stability. In this study four different titanium surfaces modifications: turned (TS); aluminium oxide-blasted (Al2O3); resorbable material blasted (RBM); sandblast and then etched with a mixture of acids (SAE), were evaluated in terms of surfaces topography and chemical composition prior to in vivo analysis. Topography analysis revealed two groups: one with smooth, anisotropic, undeveloped TS surface and the second group with remaining surfaces presenting rough, isotropic, developed surfaces with added during blasting procedure aluminium for Al2O3 and calcium and phosphorus for RBM. Physical and chemical modifications of titanium surface change its microstructure (typical for SAE) and increase its roughness (highest for Al2O3-blasted and RBM surfaces). The introduced modifications develop titanium surface - 10 times for SAE surfaces, 16 times for Al2O3-blasted surfaces, and 20 times for RBM surfaces.

Prospects of using titanium nickelide implants with modified surface in dental implantology.

PubMed

Razdorsky, V V

2008-06-01

Corrosion resistance and biocompatibility of 60 specimens of titanium nickelide with modified surfaces implanted into spongy bone were studied in rabbit experiments. Specimens modified by molybdenum ions exhibited high inertness and favorable tissue reaction. No accumulation of nickel and titanium ions in animal organs was detected.