Microscopic and Quantitative Investigations on PST Ti-Al / Ti Reaction Diffusion Couples

Interdiffusion in multi-phase diffusion couples of polycrystalline Ti and polysynthetically twinned (PST) Ti-49.3 at.% Al, with the diffusion direction parallel to the lamellar planes, is investigated in the temperature range 973 – 1173 K. A reaction zone (RZ) of the α2-Ti3Al phase forms between the end materials and exhibits deeper penetration in the α2 lamellae than in the primary γ lamellae. The mass balance and the lamellar thickness across the RZ / PST interface are believed to be the major factors that lead to the different behaviors in the penetration depth of the RZ. Direct measurements of the RZ thickness reveal a parabolic growth of the RZ, indicating a diffusion-controlled growth macroscopically. Concentration profiles from the Ti, through the RZ, into the PST γ and α2 lamellae are measured by x-ray spectroscopy in a transmission electron microscope. Deviations from a diffusion-controlled composition profile indicate some extent of interface-controlled growth. Plateaus are seen in the concentration profiles in the RZ adjacent to the RZ/PST interface, extending through most of the deeply penetrated well region. The interfacial energy and strain energy are possible reasons for the plateaus. The interdiffusion coefficients are found to be largely independent of composition with a temperature dependence that obeys the Arrhenius relationship

Interdiffusion and Phase Behavior in Polysynthetically Twinned (PST) TiAl / Ti Diffusion Couples

Diffusion couples of pure Ti and polysynthetically twinned (PST) TiAl (49.3 at.% Al) were prepared by high vacuum hot-pressing, with the bonding interface perpendicular to the lamellar planes. Diffusion experiments were carried out by annealing the couples in the same furnace at 650, 700 and 850oC for various times. The cross-section of the couple was studied using scanning electron microscopy (SEM) and quantitative wavelength-dispersive x-ray spectroscopy (WDS). A reaction layer whose composition is close to that of the stoichiometric α2–Ti3Al phase formed along the PST TiAl / Ti bonding interface in PST TiAl side. Direct measurements of the thickness of the reaction zone were performed at different phase regions and various boundaries. By assuming the thickness of the reaction zone increases as (Dt)1/2, where D is the diffusion coefficient and t is the annealing time, the diffusion coefficients at these temperatures were calculated. Composition profiles in the reaction zone, along the lamellae and at the lamellar interfaces were obtained by WDS analyses

Characterizations of Lamellar Interfaces and Segregations in a PST-TiAl Intermetallic Alloy by an Analytical Scanning Transmission Electron Microscope

Polysynthetically-twinned titanium aluminide (PST-TiAl), a fully lamellar γ-TiAl+α2- Ti3Al dual-phase alloy, is under evaluation for applications in rotary components in aircraft and automobile industries due to its high specific strength, and a high strength-retention capability at elevated-temperatures. However, the low ductility at room- to mid-high temperatures of the material hinders its application. Additions of certain tertiary elements to the binary TiAl system appear to improve the ductility at room- to mid-high temperatures, thus a balance among strength, ductility, and fracture toughness can be expected. In this article, segregation of tertiary elements to the lamellar interfaces is investigated. Single crystals of a TiAl with 0.6% atomic percentage tertiary additions are grown by an optical float-zone method. Segregation to the lamellar interfaces and the microstructure of the interfaces are investigated. Structures of the lamellar interfaces are characterized, and microchemistry and distribution habits of these elements along the γ+α2 lamellar boundaries as well as the γ-γ lamellar and domain boundaries are analyzed

Tuning the resonant frequency of single-walled carbon nanotube bundle oscillators through electron-beam-induced cross-link formations

The authors investigate the effect of electron irradiation on the resonant frequency of single-walled carbon nanotube bundles. Electron beam irradiation was employed to induce the formation of intertube cross-linking. An increase in the resonant frequency was observed at low electron doses as the bending modulus was enhanced by cross-link formation. Higher doses induced amorphization and knock-on damage in the bundle, resulting in an overall reduction of the bending modulus. The effect of stiffness enhancement is more pronounced in larger diameter bundles due to the more compliant initial condition. At 45 nm diameter, an increase in bending modulus of 115% is observed

Filling Single Wall Carbon Nanotubes with Metal Chloride and Metal Nanowires and Imaging with Scanning Transmission Electron Microscopy

Nanowires of magnetic metals (Ho, Gd) have been synthesized inside the hollow interior of single wall carbon nanotubes by the sealed-tube reaction. Amongst the d- and f-series metal chlorides investigated in this study, HoCl3 and GdCl3 fill the SWNTs to a significantly higher extent than FeCl2 and CoCl2. HoCl3 and GdCl3 nanowires have been transformed into the respective metal nanowires via the reduction of the chloride nanowires. The nanowires have been imaged using high-resolution transmission electron microscopy and scanning transmission electron microscopy (STEM). X-ray energy dispersive spectroscopy carried out in conjunction with STEM confirmed the presence of metal chloride and metal nanowires

Atomic Structure of a Grain Boundary in a Metallic Alloy: Combined Electron Microscope and Theoretical Study

A synergistic high-resolution electron microscopy (HREM) and theoretical analysis of the structure of a grain boundary in copper containing bismuth is presented. The calculation of the structure of the boundary were carried out using N-body empirical potentials constructed using results of ab initio full-potential linear-muffin-tin-orbital calculations. Excellent agreement between the calculated and observed structures is shown by comparing a through-focal series of observed and calculated images. It is shown for the first time that HREM combined with computer modeling employing realistic empirical potentials can decipher with a great accuracy the structure of boundaries containing multiple atomic species

Single Wall Carbon Nanotubes Filled with Metallocenes: a First Example of Non-Fullerene Peapods

We report the synthesis and analysis of metallocenes (ferrocene, chromocene, ruthenocene, vanadocene, tungstenocene-dihydride) encapsulated in single wall carbon nanotubes (SWNTs). In the case of ferrocene, efficient filling of the SWNTs was accomplished from both the liquid and the vapor phase. The other two metallocenes were filled from the vapor phase. High resolution transmission electron microscopy reveals single molecular chains of metallocenes inside SWNTs. Molecules move under the electron beam in the SWNTs indicating the absence of strong chemical bonds between each other and the SWNT wall. Their movement freezes after short illumination as a result of irradiation damage. Energy dispersive X-ray spectrometry confirms the presence of iron, chromium, ruthenium, vanadium and tungsten

Encapsulated Molecules in Carbon Nanotubes: Structure and Properties

We encapsulate a number of fullerenes inside single-walled carbon nanotubes (SWNTs) including La2@C80 and ErxSc3-xN@C80(x=0-3). The structural properties of these nanoscopic hybrid materials are described using high resolution transmission electron microscopy and electron diffraction. It is found that the encapsulated fullerenes selfassemble into long, one-dimensional chains. The thermal stability of these supramolecular assemblies are studied and large variations are found. The behavior is nominally consistent with the mass of the encapsulated metallofullerenes

Structure and properties of C\u3csub\u3e60\u3c/sub\u3e@SWNT

Our recent achievement of high-yield C60@SWNT synthesis facilitates characterization by various techniques, including selected area electron diffraction (SAD) and Raman spectroscopy. The obtained SAD patterns show that interior C60 molecules sit on a simple 1-D lattice having a parameter of 1.00 nm. Simulated SAD patterns and real-space measurements both support this determination and do not indicate a lattice with a more complex basis, e.g. a dimer basis. Empty and bulk-filled SWNTs (22%, 56%, and 90% yields), each subjected to identical processing steps, were examined by room temperature Raman spectroscopy. Systematic differences are seen between the spectra of filled and unfilled SWNTs, particularly with respect to the G- and RBM-bands of the nanotubes. We present a possible explanation for this behavior

Reproducible synthesis of C\u3csub\u3e60\u3c/sub\u3e@SWNT in 90% yields

In previous works, we have shown our discovery of C60@SWNT and first described the general mechanism of filling, which involves the vapor phase transport of C60 molecules to openings in the SWNTs\u27 walls. Here, we discuss the high-yield synthesis of C60@SWNT by refinements to our method. Yields are measured by a calibrated weight uptake technique, a methodology that is not subject to many of the potential pitfalls inherent to other techniques that have been applied. At certain processing conditions, yields exceeding 90% were obtained and corroborated by transmission electron microscopy. From our data, we determine the parameters most important for creating endohedral SWNT supramolecular assemblies by the vapor phase method. Our results pave the way for successful single-tube measurements and for high-yield filling with non-fullerenes