S 4300se

High purity titanium tetrachloride was supplied by Junsei Chemical Co., Yakuri Pure Chemicals Co., Wako Chemical Co., Aldrich chemical Co., and Fluka. All titanium tetrachloride reagents were of analytical reagent grade (99.9%). The hydrochloric acid was purchased by Samchun Chemical Co. The used hydrochloric acid solution was of analytical reagent grade (35 wt. % HCl). To prepare the diluent for titanium tetrachloride, various concentrated hydrochloric acid (HCl) solvent solutions were prepared by diluting the stock acid solution with DI water. A 35 wt. % HCl solution was diluted with various quantities of DI water, and then 100 mL of 1, 3, 5, 7, 9, and 11 M diluted hydrochloric acid solutions was prepared.
Fourier transform-infrared vacuum spectrometer (FT-IR, A Bruker VERTEX 80V) was used to analyse the impurities in titanium tetrachloride. Golden gate single reflection diamond attenuated total reflectance (ATR) was used to examine the liquid-state titanium tetrachloride samples. A Hitachi S-4300SE field emission-scanning electron microscope (FE-SEM), especially with energy dispersive spectroscopy (EDS), was used to analyse the solid-state samples. A PerkinElmer Optima 7300DV inductively coupled plasma optical emission spectrometer (ICP-OES) was used to investigate the quantities of impurities in titanium tetrachloride.

The microstructural characteristics of extracted collagen were observed with scanning electron microscopy (SEM) (S-4300SE, Hitachi, Tokyo, Japan) and an accelerating voltage of 5.0 Kv. The collagen powder was mounted on 5 mm × 12.5 mm dimensional aluminium cylinder stubs and sputter-coated using a fine auto coater (JFC 1600, Tokyo, Japan). The samples were observed at 500× magnification in a superficial layer, and analysis was done in triplicate [12 ].

A high-resolution image of the AI-AgNPs was produced by SEM (Hitachi, S-4300SE, Tokyo, Japan), which includes details about their size, shape, composition, electrical conductivity, topography, and other characteristics.

The evolved crystal structure was identified via X-ray diffraction (XRD, X’Pert PRO-MRD, PHILIPS, Netherlands). The grain structure and phase distribution were investigated via EBSD using field-emission scanning electron microscopy (FE-SEM, S-4300SE, HITACHI, Japan). Specimens were mechanically polished using SiC papers of up to 4000 grit size, and electropolished in a mixed solution of 92% acetic acid and 8% perchloric acid. Transmission electron microscopy (TEM) was performed using a JEOL JEM-2100F instrument operated at 200 kV. The TEM specimens were prepared via focused ion beam lift-out using a FEI Helios NanoLab 450 F1 instrument. The chemical composition of each phase was measured via atom probe tomography (APT, Cameca LEAP 4000X HR) using the pulsed laser mode at a specimen base temperature of ~50 K. The pulse frequency and energy were 200 kHz and 50 pJ, respectively. The acquired APT data were reconstructed and analysed using the commercial IVAS® software by Cameca. To reveal the deformation structures, TEM was conducted for the 1%-deformed tensile specimen.

These sheets were 2%-nital-etched, and basic microstructures (longitudinal-short-transverse (L-S) plane) were examined by using an optical microscope and a field emission scanning electron microscope (FE-SEM, model: S-4300SE, Hitachi, Tokyo, Japan). Since martensite-austenite constituents (MA) were not clearly defined in the nital-etching, the etching in a LePera solution^{40 (link)} was also used. Electron back-scattered diffraction (EBSD) analysis (step size; 0.15 μm) was conducted on specimens electro-polished in a 92%-CH₃COOH + 8%-HClO₄ solution at 32 V by using an FE-SEM (model; Quanta 3D FEG, FEI, USA).