A PHI 5000 VersaProbe instrument (Physical Electronics, Chanhassen, MN, USA) was used for survey, scan and high resolution XPS. The powder was dried in oven at 100 °C for 24 h at atmospheric pressure before analysis and thereafter placed in the XPS pre-chamber overnight, in order to avoid anomalous outgassing during the XPS characterization, performed in UHV conditions (10−8 Pa). A monochromatic Al K-alpha X-ray source (1486.6 eV energy, 15 kV voltage and 1 mA anode current, and a power of 25.2 W were used for analysis. Different pass energy values were employed: 187.85 eV for survey spectra and 23.5 eV for high resolution peaks. Analyses were carried out with a take-off angle of 45° and with a 100 μm diameter X-ray spot size on a square area of 1400 × 1400 μm2, with the aim to have a good average and better statistics of powder behavior. A double beam (electron and argon ion gun) neutralization system, dedicated to reduce the charging effect on samples, was also employed during data acquisition. All binding energies (BE) were referenced to the C1s line at 284.8 eV. Spectra were analyzed and peak deconvolution was performed using Gauss–Lorentz curves by MultiPak software (version 9.6.0, Physical Electronics, Chanhassen, MN, USA).
Phi 5000 versaprobe instrument
Manufactured by Physical Electronics
Sourced in United States, Japan
The PHI 5000 VersaProbe is a versatile X-ray photoelectron spectroscopy (XPS) instrument designed for surface analysis. It provides high-performance capabilities for the characterization of a wide range of materials, including metals, semiconductors, polymers, and ceramics. The instrument utilizes a monochromatic X-ray source to generate photoelectrons, which are then analyzed to determine the elemental composition, chemical states, and depth profiles of the sample surface.
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Lab products found in correlation
Multipak software, by Physical Electronics (1 mentions)
Titan 80 300 s tem, by Thermo Fisher Scientific (1 mentions)
X pro x ray diffractometer, by Philips (1 mentions)
Emx 10 12 spectrometer, by Bruker (1 mentions)
Ims 6 f, by Cameca (1 mentions)
V 770, by Jasco (1 mentions)
Nanoscope 5 multimode 8, by Bruker (1 mentions)
Jem 2100f, by JEOL (1 mentions)
D8 advance, by Bruker (1 mentions)
4 protocols using phi 5000 versaprobe instrument
1
X-Ray Photoelectron Spectroscopy of Powder Samples
2
UPS Spectra Acquisition and Sample Preparation
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(UPS measurements were carried out using a Physical Electronics PHI 5000 VersaProbe instrument. A monochromatized photon beam of 21.2 eV (He I) was utilized to acquire the spectra. The spectrometer was calibrated with Ag foil to determine the Fermi energy reference and a sample bias of −5 V was applied to obtain the secondary electron (SE) emission edge. Prior to record the spectra, sputter cleaning was performed on the samples using a cluster Ar beam at an energy per atom of 2.5 keV to remove surface contamination.
3
Characterization of Faceted Nanomaterials
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The powder XRD analysis was carried out on a Philips X’Pro X-ray diffractometer using Cu Kα irradiation (λ = 1.54184 Å) operated at 40 kV and 40 mA at 25 °C. High-resolution TEM images were obtained on an FEI Titan 80/300 S/TEM with an acceleration voltage of 200 kV. Electron paramagnetic resonance (EPR) spectra were recorded on the samples with the same mass (50 mg) by a Bruker EMX-10/12 spectrometer at room temperature. The Brunauer–Emmett–Teller specific surface areas of the samples were measured by nitrogen adsorption at 77 K using a Micromeritics tristar ASAP 2020 instrument. The contents of C and N impurities of the samples were analyzed using a Heraeus CHN-0-Rapid analyzer. XPS spectra of both faceted samples were obtained on an Ulvac-PHI PHI 5000 VersaProbe instrument.
4
Thermal Evaporation of Bi2S3 and Te Films
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The Bi2S3 powder (99%) and Te (99.8%) were purchased from Sigma-Aldrich and used directly as evaporation sources. Bi2S3 and Te films were deposited using the same thermal evaporator via a standard procedure. The substrate temperature was maintained at RT, and the vacuum pressure before evaporation was ~3 × 10−6 Torr. The distance between the substrate and Bi2S3/Te-loaded tungsten boat was ~20 cm. The thickness of the Bi2S3/Te film was monitored during deposition. The as-deposited samples were then annealed at different temperatures for 30 min in a N2-filled glove box. The crystal structures of the films on glass were analyzed using XRD with Cu Kα radiation (Bruker D8 ADVANCE). AFM images were obtained using a Nanoscope V Multimode 8 (Bruker, Newark, DE, United States of America) on Si substrates. Optical absorption spectra were obtained using a UV–visible spectrophotometer (V-770, JASCO). Samples for HRTEM characterization were prepared using a focused ion beam (FIB). The images and FFT patterns were obtained using HRTEM (JEOL JEM 2100 F). XPS analysis was performed using a PHI 5000 VersaProbe instrument (Ulvac-PHI, Japan). The depth element distribution was measured by SIMS (IMS 6 F, CAMECA). The Hall measurements of the films were performed in an N2-filled glove box using the van der Pauw method with a 0.51 T magnet at RT.
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