Axis ultra x ray photoelectron spectrometer

Stock solutions were characterized in MilliQ water by placing a drop on copper grids (Cu, 3 mm, 250 mesh square, SPI-grids) and letting it dry for 1 h before analysing it with TEM (Valeta CM 100 Phillips, operating voltage 100 kV). FT-IR spectroscopy was performed on powder samples using a Nicolet Magna 750 IR spectrophotometer. X-ray photoelectron spectroscopy (XPS) was acquired in energy spectrum mode at 210 W, using a Kratos Axis Ultra X-ray photoelectron spectrometer. Samples were prepared as films drop-cast from solution onto a copper foil substrate.
Size of Au NP in Elendt M7 was determined by Dynamic Light Scattering using a Zetasizer Nano-ZS at 20 °C. A backscattering angle of 173° was used to determine the observed light. Each agglomeration experiment was run with three replicates using 30 measurement runs of 1 mL sample solution in 1 × 1 cm plastic cuvettes. Stokes–Einstein equation was used to calculate the hydrodynamic diameter of the Au NP using the cumulant method for fitting the autocorrelation function (Kretzschmar et al. 1998 (link)).

XPS experiments were performed using a Kratos axis ultra X-ray photoelectron spectrometer, which uses monochromated Al Kα radiation as the X-ray source and the total energy resolution is ~0.5 eV. All spectra were acquired at a normal takeoff angle at room temperature.

A JEOL JSM6301FXV scanning electron microscope (SEM) with a field emission electron source running a 5 KV was used for the microstructure characterization of the TiO₂ nanotubular arrays with and without the peptide coating. Chemical state analysis of the samples was carried out with X-ray photoelectron spectroscopy (XPS) using a Kratos AXIS Ultra X-ray photoelectron spectrometer. A monochromatic Al source, operating at 210 W with a pass energy of 20 eV and a step of 0.1 eV, was utilized. All XPS spectra were obtained using the C1s line at 284.6 eV.

Nanoparticles were characterized by UV–VIS spectroscopy for their extinction properties (Agilent Technologies: Cary 60, Malaysia), and by X-ray diffraction for their compositional information (X'Pert Pro XRD). They were further characterized with high-resolution transmission electron microscopy (HRTEM), scanning tunnelling electron microscopy (STEM), and energy-dispersive X-ray spectroscopy (EDS) using JEOL 2010 FEG STEM with Oxford EDS and JEOL Neo ARM 200CF TEM equipped with aberration correlation and Oxford Aztec EDS. X-ray photoelectron spectroscopy (XPS) measurements were taken using a Kratos AXIS ULTRA X-ray Photoelectron Spectrometer. XPS samples were prepared by drying the samples at 90 °C for 1 h and being collected in a powdered form. The samples were scanned, resulting in a full range scan as well as a high-resolution scan for Nitrogen, Oxygen, Titanium, and Nickel. Raw response data from the XPS were normalized via an assumption of summations between normal distributions and matched to existing libraries of binding energies. The Ni loadings on TiN were determined by inductively coupled plasma spectrometry-mass spectrometry (ICP-MS) using Agilent ICP-MS 7900. The samples for ICP-MS were prepared by drying the sample at 70 °C for 8 h under vacuum, the collected dry powder sample was then dispersed in 1% nitric acid solution at the concentration of 1 mg/L.

The inductively coupled plasma atomic emission spectroscopy (ICP-AES) measurements were detected by a Prodigy ICP from Teledyne Leeman Labs. X-ray photoelectron spectroscopy (XPS) measurements were performed on an Axis Ultra X-ray photoelectron spectrometer from Kratos Analytical with an exciting source of Al Kα = 1486.7 eV. The binding energies obtained in the XPS spectral analysis were corrected for specimen charging by referencing C 1 s to 284.8 eV, and Powder X-Ray Diffraction (XRD) was performed on a Philips X’Pert Pro Super diffractometer with Cu Kα radiation (λ = 1.54178 Å). Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) were carried out on a FEI TECNAI F20 field emission electron microscope at an acceleration voltage of 200 kV. The inductively coupled plasma mass spectrum (ICP-MS) was detected by an ELEMENTAL XR ICP-MS from Thermo Fisher.

The surface morphology and elemental analysis of the samples were examined using a field emission scanning electron microscope equipped with an energy-dispersive X-ray spectroscope (FE-SEM/EDX, Hitachi SU8030). TEM and HRTEM analyses were conducted using a transmission electron microscope (JEOL2100 Plus, Japan). The crystalline phases of photoanodes were characterized by X-ray diffraction (XRD; Bruker, D2 Phaser) using the Cu Kα1 radiation in a 2θ range of 20°–80°. The light absorption spectrum and photocatalytic activity were investigated with a UV-Vis spectrophotometer (JASCO V-630). X-ray photoelectron spectroscopy (XPS) data were measured with a Kratos Axis ULTRA X-ray photoelectron spectrometer. Furthermore, electrochemical impedance spectra were measured in an AC potential frequency range of 100 000–0.1 Hz with an amplitude of 10 mV. Z-view software was used to fit the Nyquist spectrum to obtain the equivalent circuit.