Enhancing Biocompatibility and Corrosion Resistance of Ti-6Al-4V Alloy by Surface Modification Route

Titanium (Ti) and its alloys are widely used as candidate materials for biomedical implants. Despite their good biocompatibility and corrosion resistance, these materials suffer from corrosion after implantation in biological environments. The aim of this research work is to study the effect of two coatings on biocompatibility and corrosion behavior of Ti-6Al-4V biomedical implant material. Hydroxyapatite (HA) and hydroxyapatite/titanium dioxide (HA/TiO₂) coatings were thermal-sprayed on Ti-6Al-4V substrates. In the latter case, TiO₂ was used as a bond coat between the substrate and HA top coat. The corrosion behavior of coated and un-coated samples in Ringer’s solution was studied by potentiodynamic and linear polarization techniques. Before and after corrosion testing, XRD and SEM/EDS techniques were used for the analysis of phases formed and to investigate microstructure/compositional changes in the coated specimens. The cellular response was analyzed by the MTT (microculture tetrazolium) assay. The results showed that both the HA, as well as, the HA/TiO₂ coatings significantly increased the corrosion resistance of the substrate material. The HA coating was found to be more biocompatible as compared to the un-coated and HA/TiO₂-coated Ti-6Al-4V alloy.     

HVOF-Sprayed Nano TiO2-HA Coatings Exhibiting Enhanced Biocompatibility

Biomedical thermal spray coatings produced via high-velocity oxy-fuel (HVOF) from nanostructured titania (n-TiO₂) and 10 wt.% hydroxyapatite (HA) (n-TiO₂-10wt.%HA) powders have been engineered as possible future alternatives to HA coatings deposited via air plasma spray (APS). This approach was chosen due to (i) the stability of TiO₂ in the human body (i.e., no dissolution) and (ii) bond strength values on Ti-6Al-4V substrates more than two times higher than those of APS HA coatings. To explore the bioperformance of these novel materials and coatings, human mesenchymal stem cells (hMSCs) were cultured from 1 to 21 days on the surface of HVOF-sprayed n-TiO₂ and n-TiO₂-10 wt.%HA coatings. APS HA coatings and uncoated Ti-6Al-4V substrates were employed as controls. The profiles of the hMSCs were evaluated for (i) cellular proliferation, (ii) biochemical analysis of alkaline phosphatase (ALP) activity, (iii) cytoskeleton organization (fluorescent/confocal microscopy), and (iv) cell/substrate interaction via scanning electron microscopy (SEM). The biochemical analysis indicated that the hMSCs cultured on n-TiO₂-10 wt.%HA coatings exhibited superior levels of bioactivity than hMSCs cultured on APS HA and pure n-TiO₂ coatings. The cytoskeleton organization demonstrated a higher degree of cellular proliferation on the HVOF-sprayed n-TiO₂-10wt.%HA coatings when compared to the control coatings. These results are considered promising for engineering improved performance in the next generation of thermally sprayed biomedical coatings.     

Biocompatible nanostructured high-velocity oxyfuel sprayed titania coating: Deposition, characterization, and mechanical properties

Nanostructured titania (TiO₂) coatings were produced by high-velocity oxyfuel (HVOF) spraying. They were engineered as a possible candidate to replace hydroxyapatite (HA) coatings produced by thermal spray on implants. The HVOF sprayed nanostructured titania coatings exhibited mechanical properties, such as hardness and bond strength, much superior to those of HA thermal spray coatings. In addition to these characteristics, the surface of the nanostructured coatings exhibited regions with nanotextured features originating from the semimolten nanostructured feedstock particles. It is hypothesized that these regions may enhance osteoblast adhesion on the coating by creating a better interaction with adhesion proteins, such as fibronectin, which exhibit dimensions in the order of nanometers. Preliminary osteoblast cell culture demonstrated that this type of HVOF sprayed nanostructured titania coating supported osteoblast cell growth and did not negatively affect cell viability. This article was originally published inBuilding on 100 Years of Success, Proceedings of the 2006 International Thermal Spray Conference (Seattle, WA), May 15–18, 2006, B.R. Marple, M.M. Hyland, Y.-Ch. Lau, R.S. Lima, and J. Voyer, Ed., ASM International, Materials Park, OH, 2006.     

Effects of Zn Content on Crystal Structure, Cytocompatibility, Antibacterial Activity, and Chemical Stability in Zn-Modified Calcium Silicate Coatings

In our previous study, Zn-modified calcium silicate coatings possess not only excellent chemical stability but also well antibacterial activity. Still, effects of zinc content on these properties and cytocompatibility remain unclear. In this paper, two kinds of Zn-modified calcium silicate coatings (ZC0.3, ZC0.5) were fabricated on Ti-6Al-4V substrates via plasma spraying technology. X-ray diffraction results and transmission electron microscopy observations showed that the ZC0.5 coating was composed of pure hardystonite (Ca₂ZnSi₂O₇) phase, while, besides Ca₂ZnSi₂O₇ phase, the amorphous CaSiO₃ phase was also detected in the ZC0.3 coating. Chemical stability in Tris-HCl buffer solution and antibacterial activity of the Zn-modified calcium silicate coatings increased with an increase in zinc content. In vitro cytocompatibility evaluation demonstrated that the proliferation and alkaline phosphatase activity and collagen type I (COLI) secretion of osteoblast-like MC3T3-E1 cells on Zn-modified coatings were significantly enhanced compared to the Zn-free coating and Ti-6Al-4V control, and no cytotoxicity appeared on Zn-modified coatings. The better antibacterial activity and the enhanced capability to promote MC3T3-E1 cells differentiation of Zn-modified coatings should be attributed to the slow and constant Zn²⁺ releasing from the coatings.     

Nanostructured Si,Mg, CO<Subscript>3</Subscript><Superscript>2−</Superscript> Substituted Hydroxyapatite Coatings Deposited by Liquid Precursor Plasma Spraying: Synthesis and Characterization

In this study, a novel liquid precursor plasma spraying (LPPS) process was used to deposit Si, Mg, CO₃ ²⁻ substituted hydroxyapatite (HA) coatings (alone and cosubstituted) onto Ti-6Al-4V substrates. Salts of silicon, magnesium, and carbonate elements were directly added into the HA liquid precursor for subsequent plasma spraying. The phase composition, structure, and morphology of all HA coatings were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. The results indicated that the trace elements were successfully incorporated into the HA structure and nanostructured coatings were obtained for all doped HA formulations. The incorporation of trace elements into the HA structure reduced its crystallinity, especially when silicon, magnesium and carbonate ions entered simultaneously into the HA structure. FTIR spectra showed that the Si-HA and Mg-HA coatings had decreased intensities in both the O-H and P-O bands and that the CO₃ ²⁻-HA coating was mainly a B-type carbonate-substituted HA. The results showed that the LPPS process is an effective and simple method to synthesize trace element substituted biomimetic HA coatings with nanostructure.     

Development and growth of boron-modified and germanium-doped titanium-silicide diffusion coatings by the halide-activated,pack-cementation method

A halide-activated, cementation pack has been developed to codeposit either silicon and boron or else silicon and germanium in a single processing/reaction step to grow Ti-silicide diffusion coatings on commercially pure (CP) titanium, Ti-22Al-27Nb, and Ti-20Al-22Nb. Since boron is nearly insoluble in TiSi₂, a TiB₂ layer is localized at the surface of the B-modified silicide coatings. The thickness of the TiB₂ layer is controlled by the choice of boron activity and halide activator in the pack. Germanium is soluble in the Ti-silicide layers but inhomogeneously distributed in the Ge-doped silicide coating. The germanium content is controlled by choices of the Si-to-Ge ratio and the halide activator in the pack. The growth kinetics for the five-layered B-modified silicide coatings are generally similar to the undoped silicide coatings. The growth mechanism for the five-layered Ge-doped silicide coatings is generally different from the undoped silicides. The growth of dual-layer Ti-boride coatings was also studied.     

The nano-scratch behavior of biocompatible hydroxyapatite reinforced with aluminum oxide and carbon nanotubes

Hydroxyapatite (HA) reinforced with sub-micrometer Al₂O₃ and carbon nanotubes (CNTs) has been synthesized as a coating on the Ti-6Al-4V substrate via plasma spraying. The addition of Al₂O₃ and CNTs to HA has shown improvement in the hardness and elastic modulus by 65% and 50%, respectively, when compared to HA. Consequently, HA-Al₂O₃-CNT coatings have been nano-scratched to understand their wear performance. Reinforcement of HA by Al₂O₃ shows a decrease in the wear volume by more than 13 times, whereas HA-Al₂O₃-CNT coating demonstrated further wear volume reduction of five times compared to that of HA-Al₂O₃ coating.     

In situ composite coating of titania-hydroxyapatite on commercially pure titanium by microwave processing

Microwave (MW) processing has been studied as an alternative method of hydroxyapatite (HA) based composite coatings on commercially pure titanium (CPTi) to enhance the bioactivity for orthopaedic and dental implant applications. The coating was formed by processing CPTi metal packed in HA and at 800 W microwave power for 22 min. The composition of the coating was found to be TiO₂ (rutile) as major phase along with HA as minor phase. The MW absorption of non-stoichiometric TiO₂ layer, which was grown during the initial hybrid heating, resulted in sintering of apatite particles interfacing them. The non-stoichiometric nature of TiO₂ was evident from the observed mid-gap bands in ultraviolet-visible diffusive reflectance (UV-VIS-DR) spectrum. The lamellar α structure of the substrate suggests that the processing temperature was above β transus of CPTi (1155 K). The oxygen stabilized α phase whose thickness increased with microwave processing time, was likely to be the reason for the increase in Young's Modulus and hardness of the substrate. The coating induced apatite precipitation in bioactivity test. The osteoblast cell adhesion test demonstrated cell spreading which is considered favourable for cell proliferation and differentiation. Thus, in situ composite coating of titania and HA on CPTi was obtained by a simple one-step process.     

Wear Resistance Enhancement of Ti-6Al-4 V Alloy by Applying Zr-Modified Silicide Coatings

Zr-modified silicide coatings were prepared on Ti-6Al-4 V alloy by pack cementation process to enhance its wear resistance. The microstructure and wear properties of the substrate and the coatings were comparatively investigated using GCr15 and Al₂O₃ as the counterparts under different sliding loads. The obtained Zr-modified silicide coating had a multilayer structure, consisting of a thick (Ti,X)Si₂ (X represents Al, Zr and V elements) outer layer, a TiSi middle layer and a Ti₅Si₄ + Ti₅Si₃ inner layer. The micro-hardness of the coating was much higher than the substrate and displayed a decrease tendency from the coating surface to the interior. Sliding against either GCr15 or Al₂O₃ balls, the coatings showed superior anti-friction property to the Ti-6Al-4 V alloy, as confirmed by its much lower wear rate under each employed sliding condition.     

Compressive Strength Evaluation in Brazed ZrO<Subscript>2</Subscript>/Ti6Al4V Joints Using Finite Element Analysis

This study aims to synthesize and evaluate the compressive strength of the ZrO₂/Ti-6Al-4V joint brazed using an active metal filler Ag-Cu-Sn-Ti, and its application to dental implants assuring its reliability to resist the compressive failure in the actual oral environment. The brazing was performed at a temperature of 750 °C for 30 min in a vacuum furnace under 5 × 10^?6 Torr atmosphere. The microstructure of the brazed joint showed the presence of an Ag-rich matrix and a Cu-rich phase, and Cu-Ti intermetallic compounds were observed along the Ti-6Al-4V bonded interface. The compressive strength of the brazed ZrO₂/Ti-6Al-4V joint was measured by EN ISO 14801 standard test method. The measured compressive strength of the joint was ~1477 MPa—a value almost five times that of existing dental cements. Finite element analysis also confirmed the high von Mises stress values. The compressive strains in the samples were found concentrated near the Ti-6Al-4V position, matching with the position of the real fractured sample. These results suggest extremely significant compressive strength in ZrO₂/Ti-6Al-4V joints using the Ag-Cu-Sn-Ti filler. It is believed that a highly reliable dental implant can be processed and designed using the results of this study.     

Infrared heat treatment of Ti-6Al-4V with electroplated Cu

The objective of this study is to investigate an innovative infrared (IR) technique to enhance adhesion of electroplated copper (Cu) on Ti-6Al-4V without dichromate dipping. The ultimate goal is to develop a Cu coating process on Ti-6Al-4V without hazardous hexavalent chromium (Cr) solution treatments. Cu coatings of around 50 μm were electroplated on Ti-6Al-4V specimens at a current density of 0.03 A/cm² in an acidic Cu solution. To improve adhesion of coatings, IR heat treatments were performed on the Cu-coated samples at different temperatures and durations: 860 °C for 600 s and 875 °C for 20–120 s. This process was accomplished in an attempt to replace the use of dichromate dipping before electroplating. For samples heat treated at 860 °C, no bonding existed, even after 600 s. It is believed that solid-state diffusion prevailed at 860 °C and that 600 s was not enough for sufficient diffusion to occur. Adhesion was poor when samples were heat treated at 875 °C for 20 s. Excellent adhesion was observed when the heat treatment holding time was increased to 40 s. For 90 s, the surface appearance of coatings partially changed from Cu-colored to a grayish color. There was no Cu left on the surface after a 120 s heat treatment. From optical microscopic observations on sample cross sections, an interlayer between the Cu and Ti-6Al-4V formed when heat treated at 875 °C for 40 s and longer. The interlayer thickness increased as the holding time increased, until depletion of Cu. The sheet resistivity of coated specimens was on the order of pure Cu for samples heat treated at 875 °C and less than 90 s. During the 875 °C heat treatment, the following occurred: solid-state diffusion of Cu in Ti-6Al-4V, formation of eutectic solutions, dissolution of Cu and Ti-6Al-4V into the liquid phase, and the formation of intermetallic compounds. The lowest eutectic temperature of 875 °C played a key role in this innovative process of Cu coating on Ti-6Al-4V. This paper was presented at the 2nd International Surface Engineering Congress sponsored by ASM International, on September 15–17, 2003, in Indianapolis, Indiana and appears on pp. 403–10 of the Proceedings.     

Structure stability and corrosion resistance of nano-TiO2 coatings on aluminum in seawater by a vacuum dip-coating method

A stable nano-TiO₂ coating was prepared by vacuum dip-coating TiO₂ sol-gel onto the anodized aluminum surface. The effect of vacuum dip-coating method and anodization pretreatment on compactness and stability of the coatings was proved. The structure and composition of the coatings were characterized by means of scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results indicate that the surface of coatings is uniform and compact, with high load capacity. The particles of TiO₂ anatase is filled into the Al₂O₃ nano-pores formed by anodization. The electrochemical measurements show that the nano-TiO₂ coatings significantly decrease the corrosion currents densities (i_corr), as simultaneously increased the values of polarization resistance (R_t) of aluminum. It indicates the nano-TiO₂ coatings exhibit excellent anticorrosion properties in sterile seawater at the room temperature.     

Influence of electrodeposition potential,TiO2 nanoparticles and chromium (III) inhibitor addition on the corrosion protection performance of organosilane coating on aluminium

In this work, the anticorrosion properties of phenyl trimethoxysilane (PTMS) films coated on aluminium 5000 series alloys were studied. PTMS films were deposited at various cathodic potentials. The optimum electrodeposition potential was found to be ?0.8?V vs. SCE. The coatings were also modified by different amounts of nano-TiO₂. In order to introduce corrosion inhibition and a self-repair property of the PTMS film, the addition of chromium (III) corrosion inhibitor in the presence of nano-TiO₂ was studied. The anticorrosion performance of coatings was investigated in a 3.5 wt.% NaCl solution. At optimum deposition potential, the ‘critical’ nano-TiO₂ and Cr(III) contents were both observed, under which the obtained PTMS coatings show the highest anticorrosion performance. The surface morphologies of PTMS coatings were examined by scanning electron microscopy. The results showed that the coatings deposited at ?0.8?V vs. SCE, from 20?ppm of nano-TiO₂ and 0.003 M Cr(III) inhibitor present uniform and compact morphologies.     

SiO_2含量对激光熔覆含La_2O_3生物陶瓷涂层性能的影响

采用激光熔覆技术,利用CaHPO_4·2H_2O,CaCO_3,La_2O_3,SiO_2粉末和Ti粉在医用钛合金Ti-6Al-4V表面制备掺杂的质量分数分别为0%,5%,10%,15%SiO2的含La2O3梯度生物陶瓷涂层,并研究了SiO_2含量对涂层性能的影响。利用金相显微镜、扫描电镜、能谱仪、X射线分析仪分别对涂层进行显微结构、表面元素、物相组成分析,利用MTT细胞活性检测法对涂层上种植的小鼠破骨前体细胞(RAW264.7)进行细胞活性分析。结果显示:掺杂10%~15%的SiO_2后,涂层的裂纹明显减少,且厚度变均匀。涂层在模拟体液(SBF)中浸泡2周后,羟基磷灰石(HA)在掺杂10%SiO_2涂层表面的沉积量最多,涂层表面的金属元素含量稀少,这表明含10%SiO_2涂层在SBF中具备更加优良的沉积HA的能力,同时有效的阻碍了基体中重金属离子的析出。MTT结果表明,掺杂SiO_2的涂层对破骨前体细胞的活性有更加明显的抑制作用。     

Ti- 6Al-4V/hydroxyapatite composite coatings prepared by thermal spray techniques

The poor mechanical properties of hydroxyapatite (HA) can be enhanced by forming a composite with a bioinert and mechanically strong metal alloy such as Ti-6A1-4V. Biomedical composites composed of titanium alloys and HA can offer concomitant bioactive properties as well as good mechanical strength and toughness. This paper describes an attempt to improve coating mechanical properties by forming a composite composed of HA and Ti-6A1-4V. Several compositions (20, 33, and 80 wt % HA) were prepared. Subsequent examination of the plasma-sprayed coatings revealed alternating HA-rich and titanium-rich lamella microstructures. The HA-rich regions appeared porous as a result of poor interparticle adhesion, with the 80 wt% HA coatings having the highest porosity. Mechanical property analysis showed the 20 wt% HA coating to have the highest storage modulus (∼60 GPa). This coating also had the highest bond strength (≥20 MPa max). The coatings tended to exhibit increased bond strength at thicknesses less than or equal to 60 μm. The excellent bond strength of the Ti-6A1-4V/HA composite is caused by the superior interfacial bond between the Ti-6Al-4V-rich splats and the substrate. The encouraging development of this composite raises the possibility of its use as a bond coat for plasma-sprayed HA on titanium-alloy implants.     

Investigation into microstructural properties of fluorapatite Nd-YAG laser clad coatings with PVA and WG binders

Biomedical implants are generally coated with a thin layer of hydroxyapatite (HA) using a plasma spraying or pulsed laser deposition method. However, the bonding strength between the coating layer and the substrate is relatively low. Moreover, the high temperature of the deposition process causes a structural instability of the HA, and therefore degrades its bioactivity and reduces the service life of the coating layer following implantation. Accordingly, the present study replaces HA with fluorapatite (FA) as the coating material, and examines the effects of two different binders, namely polyvinyl alcohol (PVA) and water glass (WG), on the properties of FA coatings deposited on Ti-6Al-4V substrates using an Nd-YAG laser cladding process. Scanning electron microscopy (SEM) observations reveal that the FA coating has a coral- and dendrite-like structure when mixed with the PVA binder, but a pure dendrite-like structure when mixed with the WG binder. In addition, the Ca/P value of the WG-based FA coating is significantly higher than that of the PVA-based coating. Fluorapatite, Al₂O₃, CaTiO₃ and Ca₃(PO₄)₂ phases are observed in both coating layers. However, the XRD analysis results indicate that the microstructure of the WG sample is dominated by Ca₃(PO₄)₂ phase while that of the PVA sample is dominated by FA. After soaking in SBF, it was observed that the specimen produced with PVA binder or less laser output power possessed a better apatite induction ability.     

Effect of Cu2+ doping on photocatalytic performance of liquid flame sprayed TiO2 coatings

Cu²⁺ was added to liquid feedstock to deposit ion doping TiO₂ photocatalytic coatings through liquid flame spraying. The coating microstructure was characterized by x-ray diffraction (XRD), transmission electron microscopy, and x-ray photoelectron spectroscopy (XPS). The photocatalytic performance of coatings was examined by photodegradation of acetaldehyde. The XRD analysis shows that the crystalline structure of coatings is not significantly influenced by Cu²⁺ doping. The photocatalytic activity of the TiO₂ coatings is enhanced by Cu²⁺ doping. It is found that a high concentration of Cu²⁺ doping decreases the activity. The XPS analysis shows that the adsorbed oxygen concentration is increased with the increase of Cu²⁺ dopant concentration and decreases with a further increase of dopant concentration. The enhancement of photocatalytic activity can be attributed to the adsorption ability of oxygen and other reactants on the surface of doping TiO₂ coatings. This article was originally published inBuilding on 100 Years of Success, Proceedings of the 2006 International Thermal Spray Conference (Seattle, WA), May 15–18, 2006, B.R. Marple, M.M. Hyland, Y.-Ch. Lau, R.S. Lima, and J. Voyer, Ed., ASM International, Materials Park, OH, 2006.     

Fabrication and Characterization of Suspension Plasma-Sprayed Fluoridated Hydroxyapatite Coatings for Biomedical Applications

Fluoridated hydroxyapatite (FHA) coatings were prepared on a Ti substrate using a suspension plasma spraying technique. The crystalline phases and chemical compositions of the coatings were characterized using x-ray diffraction, Fourier transform infrared spectroscopy, and x-ray photoelectron spectroscopy. The analysis confirmed that the coating consisted of an FHA phase. The corrosion behavior in simulated body fluid was studied using potentiodynamic polarization tests, and the results indicated that the FHA coating greatly enhanced the corrosion resistance of the Ti substrate. The chemical stability of the FHA coatings was assessed by evaluating the release of Ca²⁺ ions. The results indicated that the substitution of fluorine into the hydroxyapatite (HA) structure had a positive effect on the dissolution resistance of the HA. The antibacterial activity was investigated using a surface-plating method; the results revealed that the antibacterial activity of the FHA coating was greater than that of the pure HA coatings. During cell culture tests, the FHA coating did not exhibit cytotoxicity toward the osteoblast cell line, and the cell proliferation was comparable with that of the HA coatings. The antibacterial activity and cell culture results suggested that the plasma-sprayed FHA coating possesses good antibacterial qualities, but is biocompatible with osteoblasts. The promising features of the FHA coating render it suitable for orthopedic and dental applications.     

Fabrication of Nano-TiO2 Coating for Dye-Sensitized Solar Cell by Vacuum Cold Spraying at Room Temperature

Deposition of nanocrystalline TiO₂ coating at low temperature is becoming more attractive due to the possibility for continuous roll production of the coating for assembly lines of dye-sensitized solar cell (DSC) at a low cost. In this study, porous nano-TiO₂ coating was deposited by vacuum cold spraying (VCS) at room temperature on a conducting glass substrate using commercial P25 nanocrystalline TiO₂ powder. The microstructure of TiO₂ coating was characterized by field emission scanning electron microscopy (FESEM) and nitrogen adsorption test. A commercial dye (N719) was adsorbed on the surface of TiO₂ particles within the coating to assemble a DSC. The cell performance was evaluated by employing simulated solar light at an intensity of 100 mW/cm². The results showed that TiO₂ coating was deposited by the agglomerates of nano-TiO₂ powders. The Brunauer-Emmett-Teller (BET) test of the as-sprayed TiO₂ coating yielded a porosity of 49% and an average pore size of 17 nm. The assembled solar cell yielded a short-circuit current density of 7.3 mA/cm² and an energy conversion efficiency of 2.4%. The test results indicate that VCS was a promising method to deposit nanocrystalline TiO₂ coatings at low temperature applied to DSCs. This article is an invited paper selected from presentations at the 2007 International Thermal Spray Conference and has been expanded from the original presentation. It is simultaneously published in Global Coating Solutions, Proceedings of the 2007 International Thermal Spray Conference, Beijing, China, May 14-16, 2007, Basil R. Marple, Margaret M. Hyland, Yuk-Chiu Lau, Chang-Jiu Li, Rogerio S. Lima, and Ghislain Montavon, Ed., ASM International, Materials Park, OH, 2007.     

Phase equilibria in Ti3Al-Nb alloys at 1000 °C

Titanium aluminides are considered to be the future high-temperature structural materials for turbine applications. Major focus is on α₂Ti₃Al based and γTiAl based alloys. Niobium additions to Ti₃Al alloys is found to improve the room-temperature ductility. Thus phase equilibria in Ti-Al-Nb system is of practical significance with regard to their processing and high-temperature phase stability characteristics. In the present research, four alloys with compositions Ti-22Al-12Nb, Ti-21A1-16Nb, Ti-20Al-20Nb, and Ti-25Al-25Nb (all in atom percent) were equilibrated at 1000 °C for 225 hours and then quenched in water. The quenched alloys were characterized for phase relations by optical microscopy, X-ray diffraction (XRD), and electron probe microanalysis (EPMA). Based on the phase analysis, the ternary isotherm of the Ti-Al-Nb system at 1000 °C was constructed on the Ti₃Al-rich side. The orthorhombic Ti₂AlNb phase was observed in the sample with Ti-25Al-25Nb composition signifying the presence of this phase at 1000 °C.