Cary 100 spectrometer

Chemicals were weighed on analytical balances METTLER-TOLEDO, ME204T/02. ¹H NMR and ¹³C NMR measurements were performed on a Brüker AV-400 spectrometer at room temperature. The ESI mass spectra were measured on an LCT Premier XE mass spectrometer. Ultraviolet–visible spectroscopic measurements spectra were acquired on a Varian Cary 100 spectrometer (1 cm quartz cells). The fluorescence spectra were performed on a Lengguang Luminescence spectrophotometer F97PRO. The morphologies were detected by transmission electron microscopy (JEM2000EX). DLS was measured on MALVERN, ZETA SIZER, ModelZEN3600 at 303 K.

A calibration curve was constructed by measuring the absorbance between 200 and 900 nm of four solutions of dye N719 in KOH 1 M in MeOH, being the molar concentration of the dye in each case 1 × 10⁻⁶, 5 × 10⁻⁶, 5 × 10⁻⁵ and 1 × 10⁻⁴. Using the Lambert-Beer’s law, the absorption coefficient ε (M⁻¹cm⁻¹) can be calculated by taking the absorbance at 515 nm. In this case, a straight line with R2 = 0.997 was obtained by linear regression, estimating a value of 11331 ± 276 for ε. With this value and a known value of 1 cm for the light path, the molar volume concentration was calculated for each sample. The total number of moles for each film was calculated by multiplying the obtained concentration by the volume of solution employed (2 ml). Then, the surface concentration was calculated by dividing this value by the area of the sample (1.875 cm²). Finally, the normalized surface concentration is simply this value divided by the thickness of the layer.
A precision quartz cell from Hellma with a light path of 1 cm and a Cary 100 spectrometer from Varian were used for these experiments.
The UV-Visible spectra of dye-sesitized electrodes were measured using an integrating sphere (Mikropack, ISP-50–8-R-GT) in the range 350–700 nm

SEM micrographs were acquired in a Hitachi S4800 working at 2 kV. The samples were dispersed onto Holey carbon films on Cu or Ni grids from Agar scientific for TEM characterization. EDX maps were acquired with a FEI Tecnai Orisis TEM/STEM working at 200 kV and equipped with a Super-X EDX system. EDX data were post-processed with the open source Hyperspy software (www.hyperspy.org), in order to obtain more quantitative compositional maps of the multishell system. HAADF-STEM and HRTEM studies were carried out with both Osiris and FEI Tecnai F30 S-Twin STEM microscopes operating at 200 kV. HR-STEM images were acquired with a probe-corrected FEI TITAN3 80-300 microscope operating at 300 kV. The crystal structure was analyzed by XRD in a Siemens D5000 spectrometer operated in the θ–2θ configuration and using the Cu Kα (1.5418 Å) radiation as an excitation source. UV-Vis analysis of the samples was done in a Cary 100 spectrometer from Varian. Fluorescence spectra were recorded in a Jobin Yvon Fluorolog-3 spectrofluorometer using an excitation wavelength of 280 nm and scanning the emission spectra between 350 and 750 nm with a 2 nm monocromator step.

UV thermal melting experiments were monitored on a Varian Cary 100 spectrometer by recording changes in the UV absorption at either 260 nm or 295 nm using a 1 cm path length cuvette. Heating rate was adjusted to 1 °C/min with data intervals of 0.5 $°\mathrm{C}$ . T_m values were determined from dual baseline-corrected 1 to 0 normalized curves (1-native and 0-denatured forms) as temperatures at which half of the molecules were folded.