Tm3030

A SEM with an attached EDX (Hitachi TM3030, Hitachi High-Technologies Corporation, Japan) was used to characterize the morphological structures and elemental information of the nano-TiO₂ coated yarn for each washing cycle. Before the analysis, the coated cotton yarn was sputtered with a thin layer of gold to avoid electrostatic charging during testing and to capture a good image of the nano-TiO₂ coated cotton yarn. The samples were tested using two different magnifications, which were 500× and 5000× magnification, respectively. Meanwhile, the morphological structures and band gap of nano-titania were characterized using SEM (Hitachi TM3030, Hitachi High-Technologies Corporation, Tokyo, Japan) and a UV-Vis spectroscopy (Model Cary 5000, Agilent, CA, USA), respectively.

The finished fabric was sputtered gold and observed under a desktop electron microscope (TM3030, Hitachi, Tokyo, Japan) at a voltage of 3 kV. Elemental analysis was performed by energy scattering spectroscopy (EDX, TM3030, Hitachi, Tokyo, Japan). Reference standards GB/T 12490-2014 and GB/T 3920-2008, the fabrics finished with microcapsules, were tested for washing resistance and friction resistance, respectively. For the washing resistance test, the fabric (100 mm × 40 mm) was washed for 0, 5, 10, 20 and 30 cycles and naturally dried indoors. One washing cycle lasted for 30 min, clean water was used and the water level was moderate; the temperature of the washing water was 30–40 °C. The wash resistance of the fabric was characterized by calculating the content and loss of essential oil on the fabric after washing. For the friction resistance test, the fabric (50 mm × 200 mm) was rubbed against the friction head with a lining cloth (50 mm × 50 mm) for 0, 10, 20, 30, 50 and 100 times under vertical pressure (9 ± 0.2 N), and the friction resistance of the fabric was characterized by calculating the content of essential oil on the fabric after friction.

The as-synthesized samples were identified by X-ray powder diffraction (XRD) with Cu-Kα radiation (Ultima IV, Rigaku, Japan). The synchrotron XRD (SXRD) patterns were collected using a Debye–Scherrer camera installed at the BL02B2 beamline in SPring-8, Japan. The wavelength was determined as 0.49968 Å using CeO₂ as a reference. The SXRD data were analyzed using the Rietveld refinement program RIETAN-FP.²⁰ Specific surface areas were determined by Brunauer–Emmett–Teller (BET) analysis of Kr gas adsorption data (BELSORP-max, MicrotracBEL, Japan). The morphologies of all the catalysts were confirmed by scanning electron microscopy (SEM) images (TM3030, Hitachi High-Tech, Japan). X-ray absorption near edge structure (XANES) spectra of Cr, Mn, and Fe K-edges were collected in the transmission mode at the BL14B2 beamline in SPring-8. The X-ray absorption spectra were normalized by spline functions between pre-edge and post-edge regions using Athena program of the IFEFFIT package.^{21 (link)}