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50 protocols using k alpha xps

1

X-ray Photoelectron Spectroscopy of Nanomaterial Powders

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The surface chemical analysis for powdered TD-NPs or conventional BPs was performed by XPS (K-Alpha XPS, Thermo Fisher Scientific, West Palm Beach, FL, USA) using Al-Kα X-ray source with a nominal spot size of 200 μm. The powdered samples were fixed on a sample holder using conductive carbon tape. Survey spectra were obtained at 200 eV pass energy and 1.0 eV energy step of the analyzer and recorded from 1350 to 0 eV. The individual high-resolution spectra for C1s, O1s, and N1s were recorded at 40 eV pass energy and 0.05 eV energy step. The obtained high-resolution spectra were fitted using Igor Pro software (version 8.04, Wavemetrics, Lake Oswego, OR, USA).
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2

Characterization of Polymer Properties

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1H NMR (500 MHz) and 13C NMR (125 MHz) were recorded on a Bruker spectrometer. Gel permeation chromatography (GPC) was performed on PL Aquagel−OH columns (Agilent Technologies) with Trisma buffer as detailed previously33 (link), with weight- and number-averaged molecular weights (Mw and Mn) and polydispersity index (PDI) of the polymers calculated referring to PEO standards. XPS was carried out on a Thermo Scientific K-Alpha XPS at 200 and 50 eV for survey and high-resolution scans, respectively20 (link). Survey scan spectra were obtained from five consecutive scans of a randomly chosen area of interest (spot size of 400 × 400 μm2), while high-resolution scan spectra were obtained from 10 consecutive scans. For scanning electron microscopy (SEM), the Ti6Al4V and Ti-pSBMA plates retrieved from the S. aureus culture were fixed with 2% EM-grade glutaraldehyde, sputter-coated with Au, and imaged on a Quanta 200 FEG MKII SEM20 (link).
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3

Characterizing Copolymer Composition via FTIR and XPS

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Fourier-transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were utilized to check comonomer incorporation in the synthesized gels. Attenuated total reflectance (ATR)-FTIR spectra were collected with a Varian 7000e FT-IR Spectrometer set to a resolution of 8 cm−1 co-added over 32 scans at a speed of 5 kHz. Elemental analysis was performed on each gel with a K-Alpha XPS (Thermo Scientific) using a spot size of 400 μm for a binding energy survey from −10 to 1,350 eV with a pass energy of 200 eV. The energy step size was held at 1 eV across 10 scans with a 10 ms dwell time. Two spots on opposite ends of each sample were captured to monitor intrabatch heterogeneity, and data represents the average and standard deviation from the two points for each gel between three gels synthesized identically. Linescans were drawn along the central z-axis of split T35.0 samples with a spot size of 30 μm. Six spots were planted equidistant from one another along the length of the scan, permitting three reflected points for each disk spanning from the thickness’s center. Parameters for surveys collected across the line scan were the same as those used for surface surveys.
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Characterization of Nanodiamonds and Wear Tracks

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The starting ND powders were characterized by transmission electron microscopy (TEM) using a JEOL 2500 TEM operating at 200 keV in order to assess the size of the ND particles. ND powders were dispersed into a methanol solution via ultrasonication and then a drop of the dispersion was deposited onto a lacy carbon TEM grid. An FEI Scios dual-beam focused ion beam – scanning electron microscope (FIB-SEM) was utilized to characterize the powders, consolidated microstructures, and wear track morphologies. WC particle sizes were analyzed using Image J software. Energy dispersive spectroscopy (EDS) analysis was conducted on an FEI Scios FIB-SEM equipped with an Oxford EDS system to characterize the elemental composition of phases present on wear tracks. Phases in the sintered samples and corresponding wear tracks were analyzed using a Scintag XDS2000 X-ray diffractometer. The operating voltage and current were 45 kV and 40 mA, respectively. Surface chemistry of the sintered samples and corresponding wear tracks was analyzed via X-ray photoelectron spectroscopy (XPS) using a Thermo Scientific K-alpha XPS. The density of sintered samples was measured using the Archimedes method, and relative densities were calculated based on the known densities of WC-Co and ND. WC particle sizes were measured using Image J software; averages presented are based on over 100 measurements.
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5

Multimodal Characterization of Samples

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X-ray photoelectron spectroscopy was recorded on a Thermo Scientific K-alpha XPS. UV–vis spectra were conducted on an Agilent Cary 60 spectrophotometer. Elemental concentration was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). H&E staining was observed on an inverted optical microscope (Nikon, Eclipse Ti–U, Japan).
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6

XPS Analysis of MnO2 Nanoflowers

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XPS analyses of MnO2 nanoflowers were carried out by a Thermo Scientific K‐Alpha XPS with Al K‐alpha monochromatic radiation (1486.3 eV). For XPS measurements, dried samples were exposed to 400 µm X‐ray spot size and 50.0 eV pass energy. The experimental pressure and the base pressure were kept below about 1 × 10−7 and 3 × 10−9 mbar, respectively. The C 1s peak at 285.0 eV was designated for the assessment.
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7

XPS Characterization of Materials

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XPS spectra were recorded using a Thermo Scientific K –alpha XPS with monochromatic Al Kα X-ray source (1486.7 eV) with a vacuum maintained at 5 × 10−9 torr. The XPS survey spectra were recorded at 200 eV pass energy, 1.0 eV/step. The high-resolution spectra of the individual elements were recorded by accumulating 20 scans at 50 eV pass energy and 0.1 eV/step. The sample measurements were performed at 400 μm spot. Data analysis and curve fitting were performed using origin software (origin lab corporation, Northampton, MA, USA).
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8

XPS Analysis of Drop-Cast Samples

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XPS scans were taken on a Thermo Scientific K-Alpha+ XPS in the constant analyzer energy mode with a 0.1 eV step size and averaged across 10 scans. Samples were drop-cast onto a silicon substrate in an identical manner to XRD experiments. All scans were corrected to the adventitious carbon binding energy (B.E.) peak at 284.8 eV. Peaks were fit with Pseudo-Voigt functions (typically 0.3–0.5, with a consistent shape across all peaks in a scan). For iron and sulfur, additional constraints were placed on the multiplet and the 2p1/2 peak position and area relative to the main 2p3/2 peak, in accordance with reference spectra.
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9

Depth-Profiling XPS Analysis of Surfaces

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XPS facilities were also provided by CNMS at ORNL. XPS analysis was conducted using a Thermo Scientific K-Alpha XPS with capabilities for sample through-thickness milling. A monochromatic Al Kα source with an energy of 1486.6 eV and Ar+ beam sputtering operated at an energy of 4.2 keV was used for XPS analysis. This type of analysis aids in measuring surface and interfacial elementals.
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10

XPS Catalyst Pellet Analysis

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XPS measurements were conducted on a K-Alpha+ XPS instrument from Thermo Fisher Scientific with an Al X-ray source. XPS samples were prepared by loading the pressed catalyst pellets into a custom-made stainless-steel holder.
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