S 5200

For material characterization, nitrogen sorption measurements were carried out using BELSORP-mini II-VS (MicrotracBEL Corp. Osaka, Japan). Before the measurement, samples were pre-treated at 200 °C under vacuum for 2 h. The specific surface area was calculated by a BET method using the adsorption area. The Barrett Joyner Hallenda (BJH) method was also applied to estimate the pore size distribution.
Thermogravimetric (TG) analyses were conducted using Thermo Plus Evo2 (Rigaku, Tokyo, Japan). Measurements were carried out in the air from room temperature to 400 °C via raising the temperature by 4 °C/min.
SEM observations were performed using S-5200 (Hitachi High-Tech, Tokyo, Japan), with the accelerating voltage of 30 kV. Studies with X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) were also conducted using Kratos Axis Ultra (Shimadzu, Kyoto, Japan) and RINT-UltimaIII/PSA (Rigaku), respectively.

TiO₂, Cu_xO, and TiO₂–Cu_xO samples were characterized under different final conditions. The pristine TiO₂ and TiO₂–Cu_xO samples were annealed at 500 °C, and the pristine Cu_xO samples were as deposited. Scanning electron microscopy (SEM; S-5200, Hitachi High Technologies, Tokyo, Japan) was performed to examine the surface morphology of the nanoparticulate thin films. Transmission electron microscopy with energy dispersive X-ray spectroscopy (TEM-EDS; JEM-2010, JEOL, Tokyo, Japan) was conducted to observe the nanoparticle’s morphology and the elements within the film.
The crystallinity was confirmed using X-ray diffraction (XRD; MiniFlex 600, Rigaku, Tokyo, Japan) over the 2θ range of 20–60°, with Cu Kα (λ = 0.154 nm) radiation, an accelerating voltage of 40 kV, and a current of 15 mA. The chemical states were determined using X-ray photoelectron spectroscopy (XPS; ESCA-3400, Shimadzu Corp., Kyoto, Japan). Additionally, the reflectance was measured by UV–vis diffuse reflectance spectroscopy (UV-Vis DRS, V-650, Jasco, Tokyo, Japan). Zeta potential measurements (ZEN3690, Malvern Instruments Ltd., Malvern, UK) were also conducted.

The cranial half of the descending thoracic aorta was opened longitudinally, washed with PBS⁻, fixed in 1% glutaraldehyde, washed with PBS⁻, and dehydrated in an ethanol series (30%, 50%, 70%, 90%, 99.5%, and 100%). The FE-SEM (Hitachi High-Technologies S-5200) was operated at 3 kV, and the entire area of the carbon-coated tissue was observed. The surface of the normal aortic endothelium exhibited less frequent horizontal waves and more frequent vertical waves (Figure 1(Aa)), and the number of crests in such vertical waves was counted in each of the seven fields/mouse (each field corresponds to the entire area of the image taken at 300 × magnification, 1 crest/field corresponding to ~7.5 crests/mm²). The detached area in the aortic endothelium with sizes in the longer axis of a few tens of microns was designated “detachment” (Figure 1(Ab)) and that of the order of 100 µm was designated “large detachment” (Figure 1(Ac)). Each mouse was considered positive if one or more such areas existed in the aorta, and such positivity in the group was evaluated independent of the number of such areas in each mouse (this was also the case for leukocyte rolling).

The colored TiO₂ hybrid particulates were characterized with Fourier transform infrared spectroscopy (FTIR), high resolution scanning electron microscopy (HR-SEM), X-ray diffractometer (XRD), and ultraviolet–visible (UV–Vis) spectrophotometry. UV–Vis (Perkin Elmer Lambda 25, MA, United States) was used to determine the reflectivity properties from the absorption spectra of TiO₂ hybrid particulates. UV–Vis measurements were carried out in a quartz cuvette ell at room temperature (25 °C) with a spectral range from 190 nm to 1100 nm. The distance between the lamp and sample was set to 121 mm with double beam light sources (pre-aligned Deuterium and Tungsten) and a linear absorbance up to 3.2 A. Samples for FTIR spectroscopy were prepared on a quartz plate. FTIR spectra were obtained using Spectrum Two (Perkin Elmer Spectrum Two, MA, United States) in an attenuated total reflection mode with a resolution of 4 cm^–1. HR-SEM (Hitachi S-5200, Tokyo, Japan) was used to characterize the changes in particle sizes and dispersions of TiO₂ after encapsulation. XRD (Bruker D8, MA, United States) measurements were performed inside a vacuum chamber to avoid scattering by air. Measurements were carried out using Cu-Kα radiation (λ = 1.5418 Å) for the 2θ range of 10° to 50° with a step size of 0.02°.

The chemical compositions and morphology of the samples were examined by X-ray diffraction (XRD; Cu-Kα λ = 1.541 Å, 2θ = 10~80°), Raman spectroscope (Raman spectrometer Labram ARAMIS, HR800, Jobin Yvon LabRam, Japan ), field-emission scanning electron microscopy (FE-SEM; Hitachi S-5200, Japan), and high-resolution electron scanning microscopy (HRTEM, JEM2100, JEOL, Japan). An electrochemical workstation (CHI 660D) was employed to test the electrochemical performances of the composites by using 1 M KOH solution as electrolyte at room temperature.