The current work shows the optimization of the preparation of nanosized titanium carbide in situ through mechanical alloying. Metallic titanium powders, along with two carbon sources, carbon nanotubes, and stearic acid, were used to reduce the particle size (around 11 nm) using an SPEX 800 high-energy mill. The combined use of 2 wt % of these carbon sources and n-heptane as a liquid process control agent proved crucial in generating nanoscale powder composites through a simple and scalable synthesis process within a 4 h timeframe. The uses of 20 wt % of both carbon sources were compared to determine the ability of carbon nanotubes to form carbides and the decomposition of process control agent during mechanical milling. The structure of the composites and starting materials were evaluated through X-ray diffraction and Raman spectroscopy, while the morphology features (average particle size and shape) were monitored via scanning electron microscopy and transmission electron microscopy.
The current work shows the optimization in the preparation of nanosized titanium carbide (TiC) in-situ through mechanical alloying (MA). Metallic titanium (Ti) powders, along with two carbon sources, carbon nanotubes (CNTs), and stearic acid (SA), were used to reduce the particle size using a high-energy Spex800 mill. The combined use of 2 wt % of these carbon sources and n-heptane as a liquid process control agent (PCA) proved crucial in generating nanoscale powder composites through a simple and scalable synthesis process within a 4-hour timeframe. The use of 20 wt % of both carbon sources was compared to determine the ability of CNTs to form carbides and the decomposition of PCAs during mechanical milling. The result reveals structures like nanoblocks and nanolumps with and important size reduction. The structure and morphology of the composites and starting materials were evaluated through x-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM).
The present work reports a comparative study on CuO and 3.0% Mn-doped CuO nanofibers (NFs) produced by the electrospinning method. State-of-the-art characterization techniques such as Electron Energy Loss Spectroscopy (EELS) and X-Ray photoelectron Spectroscopy (XPS) have been employed to determine the multivalent states and elucidate their electronic structure at the Cu-L3,2 (2p) edge. The CASTEP code has been used to model CuO (P1) and Mn-doped (C 2/c) with the GGA-PBE functional on the supercomputing system with the Xeon10 module (10 nuclei). Structural characterization was done by using a CM 200 Philips Transmission Electron Microscope (TEM) and the chemical state of surfaces with ESCALAB 250Xi XPS Thermoscientific TM. The NFs present an indirect energy bandgap, Eg = 2.03 eV and 2.85 eV, respectively. The results show that the Cu-L3,2 edge presents degenerate states associated with Cu 2p - O and Cu 3d - O hybridization, indicated as Cu3+.
The current work presents the influence of the magnesiothermic synthesis method on titanium carbide (TiC). In this method, powdered titanium precursors and two carbon sources—turbostratic carbon and carbon nanotubes—were employed in proportions of 10 wt.% and 20 wt.%. The refinement of the X-ray diffraction (XRD) patterns using the Rietveld method for TiC suggests suggested coexistence of two phases, cubic with Fm-3m space group and hexagonal with P3121 space group. In particular, for the sample with 20 wt.% of carbon sources, the XRD refinement revealed that the cubic phase accounted for 94% of the composition, in contrast to a secondary hexagonal phase, Ti6C3.75, which comprised 6%. The influence of carbon on the morphology (particle size and shape) and crystallite size was monitored through bright-field transmission electron microscopy (BF-TEM) imaging and XRD. In samples containing 20 wt.% carbon, a homogeneous morphology in both size (around 11 microns) and shape was observed, along with a reduction in crystallite size (from 22.7 to 17.8 nm). Raman band analysis further revealed vibrational modes indicating that carbon induced disorder in the TiC structure. The magnesiothermic synthesis method developed in this work offers a low-cost approach of interest in the aerospace and automotive industries. Additionally, the study provides significant insights for particles used as additives or reinforcing agents to enhance the mechanical properties of metal matrix composites (MMCs).