Nrs 4100

UV-visible near-infrared spectroscopy was performed using a JASCO V-770 spectrophotometer (Tokyo, Japan). Field-emission scanning electron microscopy (FE-SEM) images were taken using a Hitachi S-4500. (Tokyo, Japan) Transmission electron microscopy (TEM) images were taken using a Hitachi HF-2000 (Tokyo, Japan). Atomic force microscopy (AFM) measurements were performed with a Hitachi SPI-3800N-SPA400 (Tokyo, Japan). The Raman scattering spectra were measured using a micro-Raman spectrometer (JASCO NRS-4100, Tokyo, Japan). A 785 nm continuous-wave (CW) laser (Sun Instruments, Tokyo, Japan) was used as the excitation light source. The modification of the probe molecule, indocyanine green (ICG), onto the sample substrate was achieved by casting a 50 μL solution of 1 × 10⁻⁶ M ICG onto the sample substrate and allowing it to dry. The laser was directed onto the sample surface through a 20× working distance objective lens. Dynamic light scattering measurements were performed using a Zetasizer Nano ZS (Malvern Panalytical, Great Malvern, UK).

The Ba₇Nb₄MoO₂₀·0.15 H₂O samples were prepared by the solid-state reaction method. High-purity (>99.9%) BaCO₃, Nb₂O₅ and MoO₃ were mixed as ethanol slurries and ground as dry powders using an agate mortar and pestle. The obtained powders were calcined at 900 °C for 12 h for decarbonation. The materials thus obtained were crushed and ground into fine powders in an agate mortar for 1 h as dried powders and ethanol slurries. The resultant powders were uniaxially pressed at 150 MPa and then sintered in air at 1100 °C for 24 h. The sintered pellets were crushed and ground into fine powders for X-ray powder diffraction (XRD), inductively coupled plasma atomic emission spectroscopy (ICP-AES, Shimadzu ICPS-8100 spectrometer), and TG-MS measurements. The ICP-AES results indicated that the cation molar ratio of Ba₇Nb₄MoO₂₀·0.15 H₂O was Ba: Nb: Mo = 6.89(12): 4.078(18): 1.034(10), which is consistent with the nominal composition. TG-MS analyses of Ba₇Nb₄MoO₂₀·0.15 H₂O were performed using RIGAKU Thermo Mass Photo under He flows at a heating rate of 20 K min^–1 up to 900 °C. The Raman spectrum of Ba₇Nb₄MoO₂₀·0.15 H₂O was collected using an NRS-4100 (JASCO Co.) instrument with an excitation wavelength of 532 nm.

The XRD patterns of the R/S/rac‐MBA_MoS₂ nanostructures were obtained using a MiniFlex600 + D/teX Ultra (Rigaku) diffractometer at 40 kV and 15 mA with a Cu‐K_α radiation source (λ = 1.54056 Å). Raman spectroscopy was performed on an NRS‐4100 (JASCO) spectrometer with a 20.1 mW laser (λ = 532 nm) from 100–1000 cm^–1. XPS measurements for Mo 3d, S 2p, N 1s and valence band region were recorded on a JPS‐9010TRX (JEOL) spectrometer with an Al‐K_α X‐ray at 12 kV and 25 mA. The peaks were resolved using the Shirley background and Voigt functions to identify the corresponding bonds. SEM and field‐emission (FE)‐TEM were performed using LSM‐7001F (JEOL) and JEM‐2100F(G5) (JEOL) microscopes, respectively. FE‐TEM was performed at an accelerating voltage of 200 kV using samples prepared on a carbon‐reinforced collodion film 250 square‐mesh copper grid (COL‐C10, Oken Shoji).

Raman measurements were carried out with a JASCO NRS-4100 confocal microscope with a 532 nm laser. Using a 100x oil objective, the laser beam was focused on the center of the MaSp2 samples through the coverslip side, as shown in Fig. 3a. Spectra were recorded in a wavenumber range from 500 to 2000 cm⁻¹. To detect the minor shift in wavenumber, the grating was set as 1800 grooves mm⁻¹ with a slit size of 10 × 8000 μm, providing a resolution as high as 0.8 cm⁻¹. The beam intensity of 16.9 mW and exposure time of 300 s were optimized to obtain a sufficient signal-to-noise ratio. Under the protection of the buffer medium surrounding the MaSp2 samples, no local heating effect was induced by the set laser power. Consistent results were obtained by repeating the measurement at least five times under the same conditions to ensure data reliability. As a control, MaSp2 was gently mixed with 0.5 M CPB (pH 7 or 5) in a customized chamber made from vinyl adhesive tape on a glass slide. To create a similar background as inside the microfluidic channel, native dragline silk from Trichonephila clavata and manually stretched MaSp2 fibers were immersed in 1 M CPB (pH 5) for Raman experiments.