Metal chalcogenides are of interest as electrocatalysts, battery materials, and more. XPS is a valuable tool for studying changes to these materials before and after catalysis, making reference spectra for the pristine materials valuable. Here, we present XPS spectra for a family of nickel sulfoselenide (NiSSe) materials based on the Ni3X2 crystal structure, Ni3S2−xSex. XPS surveys and high-resolution spectra of Ni 2p, S 2p, S 2s, Se 3d, Se 3p, and Se 3s were recorded using Al Kα radiation.
Accession#: 01989, 01990, 01991, and 01992
Technique: XPS
Specimen: Nickel sulfoselenides
Instrument: Kratos Axis Supra
Major Elements in Spectra: Ni, S, Se
Minor Elements in Spectra: C, O
Published Spectra: 27
Spectral Category: Comparison
INTRODUCTION
Metal chalcogenides have become popular electrocatalyst and precatalyst materials, studied for reactions including the oxygen evolution reaction (OER), oxygen reduction reaction (ORR), and hydrogen evolution reaction (HER).1 Chalcogenide compounds based on first row transition metals like Fe, Co, and Ni are among the most popular due to the relative abundance, low cost, and high electrocatalytic activity of these metals.1–4 These metals have been paired with S, Se, and Te in electrocatalytic studies and demonstrated promising performance in all cases.2,4,5 Compositional modifications to these metal chalcogenides have most commonly revolved around the introduction of additional metals (e.g., NiCo2Se4)6 or anions like P or N,7 typically with the goal of further improving electrocatalytic performance or stability. More recently, reports have begun to describe the addition of a second chalcogen to various metal chalcogenides to affect similar changes.8–11
Composed of a mixture of metal, sulfur, and selenium, metal sulfoselenides have been recently studied as active electrocatalysts for the OER, ORR, and HER.9,10,12 Their performance has been attributed to the unique band structures resulting from the blending of both S2− and Se2− in a single material,12 the increased stability of selenide-rich metal chalcogenides under oxidative conditions,9 and the careful tuning of the electrocatalytic surface to improve turnover,9,12 among others. Because of the surface-specific nature of electrocatalytic interactions, techniques like x-ray photoelectron spectroscopy (XPS) are valuable in the characterization of these materials for electrocatalytic and other applications, both to characterize the as-synthesized precatalyst materials and to characterize changes to those materials after electrocatalytic testing.
Here, we present a study of the XPS spectra of a family of nickel sulfoselenide (NiSSe) materials based on the Ni3X2 (X = S, Se) crystal structure, Ni3S2−xSex (x = 0, 0.72, 1.43, 2). These materials have previously shown promise as OER, ORR, and bifunctional oxygen electrocatalysts for Zn-air batteries9,12 and may have additional applications in HER and other reactions. X-ray powder diffraction (XRD) spectroscopy has previously confirmed the presence of a single mixed chalcogen crystal phase in these NiSSe materials, and the results here provide Ni 2p, S 2p, S 2s, Se 3d, C 1s, and O 1s XPS spectra for these NiSSe materials with varying quantities of S and Se.
SPECIMEN DESCRIPTION (ACCESSION # 01989)
Specimen: Nickel sulfide
CAS Registry #: 12035-72-2
Specimen Characteristics: Homogeneous; powder; polycrystalline; semiconductor; inorganic compound; powder
Chemical Name: Nickel sulfide
Source: Prepared via hydrothermal synthesis as described in Ref. 9.
Composition: Ni3S2
Form: Polycrystalline powder
History and Significance: Prepared via hydrothermal synthesis. Crystal structure was confirmed with XRD and homogeneity was confirmed with scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDX).9
As Received Condition: As synthesized; stored at room temperature under Ar
Analyzed Region: Same as host material
Ex Situ Preparation/Mounting: The powder was packed densely on copper tape using a clean spatula so that no tape was visible through the sample. It was then tapped to remove any loose material.
In Situ Preparation: None
Charge Control: Charge neutralization was done using a coaxial electron filament with a filament current of 0.42 A, filament bias of 1 V, and charge balance of 2.5 V. The electrons converge on the center ∼2 mm diameter or so centered on the sample in a ring shape.
Temp. During Analysis: 300 K
Pressure During Analysis: 6.65 × 10−7 Pa
Pre-analysis Beam Exposure: 30 s
SPECIMEN DESCRIPTION (ACCESSION # 01990)
Specimen: Nickel selenide
CAS Registry #: 12137-13-2
Specimen Characteristics: Homogeneous; powder; polycrystalline; semiconductor; inorganic compound; powder
Chemical Name: Nickel selenide
Source: Prepared via hydrothermal synthesis as described in Ref. 9.
Composition: Ni3Se2
Form: Polycrystalline powder
History and Significance: Prepared via hydrothermal synthesis. Crystal structure was confirmed with XRD and homogeneity was confirmed with SEM/EDX.9
As Received Condition: As synthesized; stored at room temperature in Ar
Analyzed Region: Same as specimen
Ex Situ Preparation/Mounting: The powder was packed densely on copper tape using a clean spatula so that no tape was visible through the sample. It was then tapped to remove any loose material.
In Situ Preparation: None
Charge Control: Charge neutralization was done using a coaxial electron filament with a filament current of 0.42 A, filament bias of 1 V, and charge balance of 2.5 V. The electrons converge on the center ∼2 mm diameter or so centered on the sample in a ring shape.
Temp. During Analysis: 300 K
Pressure During Analysis: 6.65 × 10−7 Pa
Pre-analysis Beam Exposure: 30 s
SPECIMEN DESCRIPTION (ACCESSION # 01991)
Specimen: Nickel sulfoselenide
CAS Registry #: N/A
Specimen Characteristics: Homogeneous; powder; polycrystalline; semiconductor; inorganic compound; powder
Chemical Name: Nickel sulfoselenide
Source: Prepared via hydrothermal synthesis as described in Ref. 9.
Composition: Ni3S1.19Se0.72
Form: Polycrystalline powder
History and Significance: Prepared via hydrothermal synthesis. S and Se content was confirmed with x-ray fluorescence (XRF) spectroscopy, crystal structure was confirmed with XRD, and homogeneity was confirmed with SEM/EDX.9
As Received Condition: As synthesized; stored at room temperature in Ar
Analyzed Region: Same as specimen
Ex Situ Preparation/Mounting: The powder was packed densely on copper tape using a clean spatula so that no tape was visible through the sample. It was then tapped to remove any loose material.
In Situ Preparation: None
Charge Control: Charge neutralization was done using a coaxial electron filament with a filament current of 0.42 A, filament bias of 1 V, and charge balance of 2.5 V. The electrons converge on the center ∼2 mm diameter or so centered on the sample in a ring shape.
Temp. During Analysis: 300 K
Pressure During Analysis: 6.65 × 10−7 Pa
Pre-analysis Beam Exposure: 30 s
SPECIMEN DESCRIPTION (ACCESSION # 01992)
Specimen: Nickel sulfoselenide
CAS Registry #: N/A
Specimen Characteristics: Homogeneous; powder; polycrystalline; semiconductor; inorganic compound; powder
Chemical Name: Nickel sulfoselenide
Source: Prepared via hydrothermal synthesis as described in Ref. 9.
Composition: Ni3S0.4Se1.43
Form: Polycrystalline powder
History and Significance: Prepared via hydrothermal synthesis. S and Se content was confirmed with XRF, crystal structure was confirmed with XRD, and homogeneity was confirmed with SEM/EDX.9
As Received Condition: As synthesized; stored at room temperature in Ar
Analyzed Region: Same as specimen
Ex Situ Preparation/Mounting: The powder was packed densely on copper tape using a clean spatula so that no tape was visible through the sample. It was then tapped to remove any loose material.
In Situ Preparation: None
Charge Control: Charge neutralization was done using a coaxial electron filament with a filament current of 0.42 A, filament bias of 1 V, and charge balance of 2.5 V. The electrons converge on the center ∼2 mm diameter or so centered on the sample in a ring shape.
Temp. During Analysis: 300 K
Pressure During Analysis: 6.65 × 10−7 Pa
Pre-analysis Beam Exposure: 30 s
INSTRUMENT DESCRIPTION
Manufacturer and Model: Kratos Axis Supra
Analyzer Type: Spherical sector
Detector: Multichannel resistive plate
Number of Detector Elements: 128
INSTRUMENT PARAMETERS COMMON TO ALL SPECTRA
Spectrometer
Analyzer Mode: Constant pass energy
Throughput (T = EN): N = 0
Excitation Source Window: None
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Beam Size: 2000 × 1000 μm2
Signal Mode: Multichannel direct
Geometry
Incident Angle: 54.7°
Source-to-Analyzer Angle: 54.7°
Emission Angle: 0°
Specimen Azimuthal Angle: 45°
Acceptance Angle from Analyzer Axis: 17°
Analyzer Angular Acceptance Width: 34° × 34°
DATA ANALYSIS METHOD
Energy Scale Correction: Spectra corrected to C 1s at 285 eV.
Recommended Energy Scale Shift: Varies depending on sample. For Ni3S2, 2.14 eV; for Ni3Se2, −0.175 eV; for Ni3S1.19Se0.72, −0.024 eV; and for Ni3S0.4Se1.43, −0.435 eV.
Peak Shape and Background Method: Data were fit using a Shirley background and Gaussian–Lorentzian peak shapes.
Quantitation Method: Quantification was done using casaxps with sensitivity factors supplied by Kratos Analytical.
SPECTRAL FEATURES TABLE
Spectrum ID # . | Element/ Transition . | Peak Energy (eV) . | Peak Width FWHM (eV) . | Peak Area (eV counts/s) . | Sensitivity Factor . | Concentration (at. %) . | Peak Assignment . |
---|---|---|---|---|---|---|---|
01989-02 | Ni 2p3/2 | 852.5 | … | … | 2.676 | 31e | Ni–S |
01989-02 | Ni 2p3/2 | 855.8 | … | … | … | … | … |
01989-02 | Ni 2p3/2 | 861.5 | … | … | … | … | … |
01989-03a | S 2p3/2 | 162.1 | … | … | … | … | Ni–S |
01989-03a | S 2p1/2 | 163.3 | … | … | … | … | Ni–S |
01989-04 | S 2s | 226.6 | 2.5 | 324.2 | 0.391 | 8 | Ni–S |
01989-04 | S 2s | 229.2 | 2.5 | 102.0 | 0.391 | 3 | S(0) |
01989-05 | C 1s | 285.0 | 1.36 | 427.0 | 0.278 | 15 | Adventitious surface C |
01989-05 | C 1s | 286.2 | 1.60 | 189.9 | 0.278 | 7 | C–O from surface C |
01989-05 | C 1s | 288.7 | 1.68 | 93.9 | 0.278 | 3 | Carbonate from surface C |
01989-06 | O 1s | 531.2 | 1.66 | 1845.3 | 0.78 | 24 | –OH |
01989-06 | O 1s | 532.5 | 2 | 684.9 | 0.78 | 9 | C-O from surface C |
01990-02 | Ni 2p3/2 | 852.6 | … | … | … | … | Ni–Se |
01990-02 | Ni 2p3/2 | 855.7 | … | … | … | … | … |
01990-02 | Ni 2p3/2 | 861.1 | … | … | … | … | … |
01990-03b | Se 3d5/2 | 53.9 | 1.04 | 612.2 | 0.853 | … | Ni–Se |
01990-03b | Se 3d3/2 | 54.75 | 1.04 | 408.1 | 0.853 | … | Ni–Se |
01990-03b | Se 3d5/2 | 54.5 | 0.47 | 304.3 | 0.853 | … | Ni–Se |
01990-03b | Se 3d3/2 | 55.38 | 0.47 | 202.9 | 0.853 | … | Ni–Se |
01990-03b | Se 3d5/2 | 54.9 | 1.05 | 296.4 | 0.853 | Se(0) | |
01990-03b | Se 3d3/2 | 55.77 | 1.05 | 197.6 | 0.853 | Se(0) | |
01990-03 | Se 3d | 57 | … | … | … | Loss feature | |
01990-04c | Se 3p3/2 | 160.7 | … | … | … | … | Ni–Se |
01990-04c | Se 3p1/2 | 166.2 | … | … | … | … | Ni–Se |
01990-05 | Se 3s | 229.3 | … | … | … | … | Ni–Se |
01990-05 | Se 3s | 231.5 | … | … | … | … | Se(0) |
01990-06d | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01990-07 | O 1s | 529.1 | … | … | … | … | Ni oxide |
01990-07 | O 1s | 531.0 | … | … | … | … | –OH |
01990-07 | O 1s | 532.4 | … | … | … | … | C–O from surface C |
01991-02 | Ni 2p3/2 | 852.7 | … | … | … | … | Ni–X |
01991-02 | Ni 2p3/2 | 855.6 | … | … | … | … | … |
01991-02 | Ni 2p3/2 | 861.2 | … | … | … | … | … |
01991-03b | Se 3d5/2 | 53.9 | 0.99 | 292.5 | 0.853 | … | Ni–Se |
01991-03b | Se 3d3/2 | 54.72 | 0.99 | 195.0 | 0.853 | … | Ni–Se |
01991-03b | Se 3d5/2 | 54.6 | 0.57 | 120.2 | 0.853 | … | Ni–Se |
01991-03b | Se 3d3/2 | 55.44 | 0.57 | 80.1 | 0.853 | … | Ni–Se |
01991-03b | Se 3d5/2 | 55.1 | 1.07 | 79.0 | 0.853 | … | Se(0) |
01991-03b | Se 3d3/2 | 55.98 | 1.07 | 52.7 | 0.853 | … | Se(0) |
01991-03 | Se 3d | 57 | … | … | … | … | Loss feature |
01991-04c | Se 3p3/2 | 160.6 | … | … | … | … | Ni–Se |
01991-04c | Se 3p1/2 | 166.1 | … | … | … | … | Ni–Se |
01991-04a | S 2p3/2 | 162.3 | … | … | … | … | Ni–S |
01991-04a | S 2p1/2 | 163.4 | … | … | … | … | Ni–S |
01991-05 | S 2s | 226.7 | … | … | … | … | Ni–S |
01991-05 | Se 3s | 229.4 | … | … | … | … | Ni–Se |
01991-06b | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01991-07 | O 1s | 531.1 | … | … | … | … | –OH |
01991-07 | O 1s | 532.6 | … | … | … | … | C–O from surface C |
01992-02 | Ni 2p3/2 | 852.8 | … | … | … | … | Ni–X |
01992-02 | Ni 2p3/2 | 855.8 | … | … | … | … | … |
01992-02 | Ni 2p3/2 | 861.2 | … | … | … | … | … |
01992-03 | Se 3d5/2 | 53.9 | 1.01 | 194.8 | 0.853 | … | Ni–Se |
01992-03 | Se 3d3/2 | 54.76 | 1.01 | 129.9 | 0.853 | … | Ni–Se |
01992-03 | Se 3d5/2 | 54.6 | 0.57 | 122.0 | 0.853 | … | Ni–Se |
01992-03 | Se 3d3/2 | 55.50 | 0.57 | 81.3 | 0.853 | … | Ni–Se |
01992-03a | Se 3d5/2 | 54.9 | 1.18 | 111.9 | 0.853 | Se(0) | |
01992-03a | Se 3d3/2 | 55.81 | 1.18 | 74.6 | 0.853 | Se(0) | |
01992-03 | Se 3d | 57 | … | … | … | … | Loss feature |
01992-04c | Se 3p3/2 | 160.6 | … | … | … | … | Ni–Se |
01992-04c | Se 3p1/2 | 166.1 | … | … | … | … | Ni–Se |
01992-04a | S 2p3/2 | 161.0 | … | … | … | … | Ni–S |
01992-04a | S 2p1/2 | 162.2 | … | … | … | … | Ni–S |
01992-05 | S 2s | 226.7 | … | … | … | … | Ni–S |
01992-05 | Se 3s | 229.5 | … | … | … | … | Ni–Se |
01992-06d | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01992-07 | O 1s | 531.1 | … | … | … | … | –OH |
01992-07 | O 1s | 532.7 | … | … | … | … | C–O from surface C |
Spectrum ID # . | Element/ Transition . | Peak Energy (eV) . | Peak Width FWHM (eV) . | Peak Area (eV counts/s) . | Sensitivity Factor . | Concentration (at. %) . | Peak Assignment . |
---|---|---|---|---|---|---|---|
01989-02 | Ni 2p3/2 | 852.5 | … | … | 2.676 | 31e | Ni–S |
01989-02 | Ni 2p3/2 | 855.8 | … | … | … | … | … |
01989-02 | Ni 2p3/2 | 861.5 | … | … | … | … | … |
01989-03a | S 2p3/2 | 162.1 | … | … | … | … | Ni–S |
01989-03a | S 2p1/2 | 163.3 | … | … | … | … | Ni–S |
01989-04 | S 2s | 226.6 | 2.5 | 324.2 | 0.391 | 8 | Ni–S |
01989-04 | S 2s | 229.2 | 2.5 | 102.0 | 0.391 | 3 | S(0) |
01989-05 | C 1s | 285.0 | 1.36 | 427.0 | 0.278 | 15 | Adventitious surface C |
01989-05 | C 1s | 286.2 | 1.60 | 189.9 | 0.278 | 7 | C–O from surface C |
01989-05 | C 1s | 288.7 | 1.68 | 93.9 | 0.278 | 3 | Carbonate from surface C |
01989-06 | O 1s | 531.2 | 1.66 | 1845.3 | 0.78 | 24 | –OH |
01989-06 | O 1s | 532.5 | 2 | 684.9 | 0.78 | 9 | C-O from surface C |
01990-02 | Ni 2p3/2 | 852.6 | … | … | … | … | Ni–Se |
01990-02 | Ni 2p3/2 | 855.7 | … | … | … | … | … |
01990-02 | Ni 2p3/2 | 861.1 | … | … | … | … | … |
01990-03b | Se 3d5/2 | 53.9 | 1.04 | 612.2 | 0.853 | … | Ni–Se |
01990-03b | Se 3d3/2 | 54.75 | 1.04 | 408.1 | 0.853 | … | Ni–Se |
01990-03b | Se 3d5/2 | 54.5 | 0.47 | 304.3 | 0.853 | … | Ni–Se |
01990-03b | Se 3d3/2 | 55.38 | 0.47 | 202.9 | 0.853 | … | Ni–Se |
01990-03b | Se 3d5/2 | 54.9 | 1.05 | 296.4 | 0.853 | Se(0) | |
01990-03b | Se 3d3/2 | 55.77 | 1.05 | 197.6 | 0.853 | Se(0) | |
01990-03 | Se 3d | 57 | … | … | … | Loss feature | |
01990-04c | Se 3p3/2 | 160.7 | … | … | … | … | Ni–Se |
01990-04c | Se 3p1/2 | 166.2 | … | … | … | … | Ni–Se |
01990-05 | Se 3s | 229.3 | … | … | … | … | Ni–Se |
01990-05 | Se 3s | 231.5 | … | … | … | … | Se(0) |
01990-06d | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01990-07 | O 1s | 529.1 | … | … | … | … | Ni oxide |
01990-07 | O 1s | 531.0 | … | … | … | … | –OH |
01990-07 | O 1s | 532.4 | … | … | … | … | C–O from surface C |
01991-02 | Ni 2p3/2 | 852.7 | … | … | … | … | Ni–X |
01991-02 | Ni 2p3/2 | 855.6 | … | … | … | … | … |
01991-02 | Ni 2p3/2 | 861.2 | … | … | … | … | … |
01991-03b | Se 3d5/2 | 53.9 | 0.99 | 292.5 | 0.853 | … | Ni–Se |
01991-03b | Se 3d3/2 | 54.72 | 0.99 | 195.0 | 0.853 | … | Ni–Se |
01991-03b | Se 3d5/2 | 54.6 | 0.57 | 120.2 | 0.853 | … | Ni–Se |
01991-03b | Se 3d3/2 | 55.44 | 0.57 | 80.1 | 0.853 | … | Ni–Se |
01991-03b | Se 3d5/2 | 55.1 | 1.07 | 79.0 | 0.853 | … | Se(0) |
01991-03b | Se 3d3/2 | 55.98 | 1.07 | 52.7 | 0.853 | … | Se(0) |
01991-03 | Se 3d | 57 | … | … | … | … | Loss feature |
01991-04c | Se 3p3/2 | 160.6 | … | … | … | … | Ni–Se |
01991-04c | Se 3p1/2 | 166.1 | … | … | … | … | Ni–Se |
01991-04a | S 2p3/2 | 162.3 | … | … | … | … | Ni–S |
01991-04a | S 2p1/2 | 163.4 | … | … | … | … | Ni–S |
01991-05 | S 2s | 226.7 | … | … | … | … | Ni–S |
01991-05 | Se 3s | 229.4 | … | … | … | … | Ni–Se |
01991-06b | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01991-07 | O 1s | 531.1 | … | … | … | … | –OH |
01991-07 | O 1s | 532.6 | … | … | … | … | C–O from surface C |
01992-02 | Ni 2p3/2 | 852.8 | … | … | … | … | Ni–X |
01992-02 | Ni 2p3/2 | 855.8 | … | … | … | … | … |
01992-02 | Ni 2p3/2 | 861.2 | … | … | … | … | … |
01992-03 | Se 3d5/2 | 53.9 | 1.01 | 194.8 | 0.853 | … | Ni–Se |
01992-03 | Se 3d3/2 | 54.76 | 1.01 | 129.9 | 0.853 | … | Ni–Se |
01992-03 | Se 3d5/2 | 54.6 | 0.57 | 122.0 | 0.853 | … | Ni–Se |
01992-03 | Se 3d3/2 | 55.50 | 0.57 | 81.3 | 0.853 | … | Ni–Se |
01992-03a | Se 3d5/2 | 54.9 | 1.18 | 111.9 | 0.853 | Se(0) | |
01992-03a | Se 3d3/2 | 55.81 | 1.18 | 74.6 | 0.853 | Se(0) | |
01992-03 | Se 3d | 57 | … | … | … | … | Loss feature |
01992-04c | Se 3p3/2 | 160.6 | … | … | … | … | Ni–Se |
01992-04c | Se 3p1/2 | 166.1 | … | … | … | … | Ni–Se |
01992-04a | S 2p3/2 | 161.0 | … | … | … | … | Ni–S |
01992-04a | S 2p1/2 | 162.2 | … | … | … | … | Ni–S |
01992-05 | S 2s | 226.7 | … | … | … | … | Ni–S |
01992-05 | Se 3s | 229.5 | … | … | … | … | Ni–Se |
01992-06d | C 1s | 285.0 | … | … | … | … | Adventitious surface C |
01992-07 | O 1s | 531.1 | … | … | … | … | –OH |
01992-07 | O 1s | 532.7 | … | … | … | … | C–O from surface C |
Peak splitting used for S 2p was 1.16 eV.
Peak splitting used for Se 3d was 0.86 eV.
Peak splitting used for Se 3p was 5.5 eV.
Se LMM Auger electron overlaps region.
Comment to Spectral Features Table: Fitting Ni 2p peaks is challenging, so concentration given is total Ni concentration based on the area of Ni 2p3/2. Quantification was not done for Se containing samples due to overlap of Se LMM Auger electron region with C 1s region and overlap of Se and S regions.
ANALYZER CALIBRATION TABLE
Spectrum ID # . | Element/ Transition . | Peak Energy (eV) . | Peak Width FWHM (eV) . | Peak Area (eV counts/s) . | Sensitivity Factor . | Concentration (at. %) . | Peak Assignment . |
---|---|---|---|---|---|---|---|
… | Ag 3d5/2 | 368.21 | 0.56 | 2.09 × 105 | 5.99 | 100 | … |
… | Au 4f7/2 | 83.96 | 0.67 | 1.41 × 105 | 6.25 | 100 | … |
… | Cu 2p3/2 | 932.59 | 0.87 | 3.77 × 105 | 5.32 | 100 | … |
Spectrum ID # . | Element/ Transition . | Peak Energy (eV) . | Peak Width FWHM (eV) . | Peak Area (eV counts/s) . | Sensitivity Factor . | Concentration (at. %) . | Peak Assignment . |
---|---|---|---|---|---|---|---|
… | Ag 3d5/2 | 368.21 | 0.56 | 2.09 × 105 | 5.99 | 100 | … |
… | Au 4f7/2 | 83.96 | 0.67 | 1.41 × 105 | 6.25 | 100 | … |
… | Cu 2p3/2 | 932.59 | 0.87 | 3.77 × 105 | 5.32 | 100 | … |
GUIDE TO FIGURES
Spectrum (Accession) # . | Element/Transition . | Voltage Shifta . | Multiplier . | Baseline . | Comment # . |
---|---|---|---|---|---|
01989-01 | Survey | −2.14 | 1 | 0 | … |
01989-02 | Ni 2p3/2 | −2.14 | 1 | 0 | … |
01989-03 | S 2p | −2.14 | 1 | 0 | … |
01989-04 | S 2s | −2.14 | 1 | 0 | … |
01989-05 | C 1s | −2.14 | 1 | 0 | … |
01989-06 | O 1s | −2.14 | 1 | 0 | … |
01990-01 | Survey | +0.175 | 1 | 0 | … |
01990-02 | Ni 2p3/2 | +0.175 | 1 | 0 | … |
01990-03 | Se 3d | +0.175 | 1 | 0 | … |
01990-04 | Se 3p | +0.175 | 1 | 0 | … |
01990-05 | Se 3s | +0.175 | 1 | 0 | … |
01990-06 | C 1s/Se LMM | +0.175 | 1 | 0 | Se LMM Auger electron overlaps region |
01990-07 | O 1s | +0.175 | 1 | 0 | … |
01991-01 | Survey | −0.024 | 1 | 0 | … |
01991-02 | Ni 2p3/2 | −0.024 | 1 | 0 | … |
01991-03 | Se 3d | −0.024 | 1 | 0 | … |
01991-04 | S 2p/Se 3p | −0.024 | 1 | 0 | … |
01991-05 | S 2s/Se 3s | −0.024 | 1 | 0 | … |
01991-06 | C 1s/Se LMM | −0.024 | 1 | 0 | Se LMM Auger electron overlaps region |
01991-07 | O 1s | −0.024 | 1 | 0 | … |
01992-01 | Survey | −0.435 | 1 | 0 | … |
01992-02 | Ni 2p3/2 | −0.435 | 1 | 0 | … |
01992-03 | Se 3d | −0.435 | 1 | 0 | |
01992-04 | S 2p/Se 3p | −0.435 | 1 | 0 | … |
01992-05 | S 2s/Se 3s | −0.435 | 1 | 0 | … |
01992-06 | C 1s/Se LMM | −0.435 | 1 | 0 | Se LMM Auger electron overlaps region |
01992-07 | O 1s | −0.435 | 1 | 0 | … |
Spectrum (Accession) # . | Element/Transition . | Voltage Shifta . | Multiplier . | Baseline . | Comment # . |
---|---|---|---|---|---|
01989-01 | Survey | −2.14 | 1 | 0 | … |
01989-02 | Ni 2p3/2 | −2.14 | 1 | 0 | … |
01989-03 | S 2p | −2.14 | 1 | 0 | … |
01989-04 | S 2s | −2.14 | 1 | 0 | … |
01989-05 | C 1s | −2.14 | 1 | 0 | … |
01989-06 | O 1s | −2.14 | 1 | 0 | … |
01990-01 | Survey | +0.175 | 1 | 0 | … |
01990-02 | Ni 2p3/2 | +0.175 | 1 | 0 | … |
01990-03 | Se 3d | +0.175 | 1 | 0 | … |
01990-04 | Se 3p | +0.175 | 1 | 0 | … |
01990-05 | Se 3s | +0.175 | 1 | 0 | … |
01990-06 | C 1s/Se LMM | +0.175 | 1 | 0 | Se LMM Auger electron overlaps region |
01990-07 | O 1s | +0.175 | 1 | 0 | … |
01991-01 | Survey | −0.024 | 1 | 0 | … |
01991-02 | Ni 2p3/2 | −0.024 | 1 | 0 | … |
01991-03 | Se 3d | −0.024 | 1 | 0 | … |
01991-04 | S 2p/Se 3p | −0.024 | 1 | 0 | … |
01991-05 | S 2s/Se 3s | −0.024 | 1 | 0 | … |
01991-06 | C 1s/Se LMM | −0.024 | 1 | 0 | Se LMM Auger electron overlaps region |
01991-07 | O 1s | −0.024 | 1 | 0 | … |
01992-01 | Survey | −0.435 | 1 | 0 | … |
01992-02 | Ni 2p3/2 | −0.435 | 1 | 0 | … |
01992-03 | Se 3d | −0.435 | 1 | 0 | |
01992-04 | S 2p/Se 3p | −0.435 | 1 | 0 | … |
01992-05 | S 2s/Se 3s | −0.435 | 1 | 0 | … |
01992-06 | C 1s/Se LMM | −0.435 | 1 | 0 | Se LMM Auger electron overlaps region |
01992-07 | O 1s | −0.435 | 1 | 0 | … |
Voltage shift of the archived (as-measured) spectrum relative to the printed figure. The figure reflects the recommended energy scale correction due to a calibration correction, sample charging, flood gun, or other phenomenon.
Accession #: . | 01989-01 . |
---|---|
■ Specimen: | Nickel sulfide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01989-01 . |
---|---|
■ Specimen: | Nickel sulfide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01989-01 . |
---|---|
■ Specimen: | Nickel sulfide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01989-01 . |
---|---|
■ Specimen: | Nickel sulfide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: 01989-02
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01989-02
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01989-03
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01989-03
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01989-04
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01989-04
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01989-05
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: C 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01989-05
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: C 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01989-06
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01989-06
Specimen: Nickel sulfide
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: . | 01990-01 . |
---|---|
■ Specimen: | Nickel selenide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01990-01 . |
---|---|
■ Specimen: | Nickel selenide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01990-01 . |
---|---|
■ Specimen: | Nickel selenide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01990-01 . |
---|---|
■ Specimen: | Nickel selenide |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: 01990-02
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01990-02
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01990-03
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01990-03
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01990-04
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01990-04
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01990-05
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01990-05
Specimen: Nickel selenide
Technique: XPS
Spectral Region: Se 3s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01990-06
Specimen: Nickel selenide
Technique: XPS, XAES
Spectral Region: C 1s / Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01990-06
Specimen: Nickel selenide
Technique: XPS, XAES
Spectral Region: C 1s / Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01990-07
Specimen: Nickel selenide
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01990-07
Specimen: Nickel selenide
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: . | 01991-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S1.19Se0.72) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01991-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S1.19Se0.72) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01991-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S1.19Se0.72) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01991-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S1.19Se0.72) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: 01991-02
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Ni 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01991-02
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Ni 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01991-03
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01991-03
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01991-04
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3p and S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01991-04
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3p and S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01991-05
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3s and S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01991-05
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: Se 3s and S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01991-06
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS, XAES
Spectral Region: C 1s/Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01991-06
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS, XAES
Spectral Region: C 1s/Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01991-07
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01991-07
Specimen: Nickel sulfoselenide (Ni3S1.19Se0.72)
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: . | 01992-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S0.4Se1.43) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01992-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S0.4Se1.43) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01992-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S0.4Se1.43) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: . | 01992-01 . |
---|---|
■ Specimen: | Nickel sulfoselenide (Ni3S0.4Se1.43) |
■ Technique: | XPS |
■ Spectral Region: | Survey |
Instrument: | Kratos Axis Supra |
Excitation Source: | Al Kα monochromatic |
Source Energy: | 1486.6 eV |
Source Strength: | 150.00 W |
Source Size: | 2000 × 1000 μm2 |
Analyzer Type: | Spherical sector analyzer |
Incident Angle: | 54.7° |
Emission Angle: | 0° |
Analyzer Pass Energy: | 160 eV |
Instrument Resolution: | 2.4 eV |
Total Signal Accumulation Time: | 131 s |
Total Elapsed Time: | 131 s |
Number of Scans: | 1 |
Accession #: 01992-02
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01992-02
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Ni 2p3/2
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1800 s
Total Elapsed Time: 1800 s
Number of Scans: 18
Accession #: 01992-03
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01992-03
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3d
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1224 s
Total Elapsed Time: 1224 s
Number of Scans: 18
Accession #: 01992-04
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3p and S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01992-04
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3p and S 2p
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 1656 s
Total Elapsed Time: 1656 s
Number of Scans: 18
Accession #: 01992-05
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3s and S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01992-05
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: Se 3s and S 2s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 2160 s
Total Elapsed Time: 2160 s
Number of Scans: 18
Accession #: 01992-06
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: C 1s/Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01992-06
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: C 1s/Se LMM
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Comments: Se Auger electron significantly overlaps region.
Accession #: 01992-07
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
Accession #: 01992-07
Specimen: Nickel sulfoselenide (Ni3S0.4Se1.43)
Technique: XPS
Spectral Region: O 1s
Instrument: Kratos Axis Supra
Excitation Source: Al Kα monochromatic
Source Energy: 1486.6 eV
Source Strength: 150.00 W
Source Size: 2000 × 1000 μm2
Analyzer Type: Spherical sector
Incident Angle: 54.7°
Emission Angle: 0°
Analyzer Pass Energy: 20 eV
Instrument Resolution: 0.3 eV
Total Signal Accumulation Time: 276 s
Total Elapsed Time: 276 s
Number of Scans: 6
ACKNOWLEDGMENTS
This work was supported by the Laboratory Directed Research and Development program at Sandia National Laboratories and based upon work supported by the U.S. Department of Energy, Office of Electricity (OE), Energy Storage Division. The views expressed in this article do not necessarily represent the views of the U.S. Department of Energy or the United States Government. Sandia National Laboratories is a multi-mission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC (NTESS), a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration (DOE/NNSA) under Contract No. DE-NA0003525. This written work is authored by an employee of NTESS. The employee, not NTESS, owns the right, title, and interest in and to the written work and is responsible for its contents. Any subjective views or opinions that might be expressed in the written work do not necessarily represent the views of the U.S. Government. The publisher acknowledges that the U.S. Government retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce the published form of this written work or allow others to do so, for U.S. Government purposes. The DOE will provide public access to results of federally sponsored research in accordance with the DOE Public Access Plan. The authors thank John Williard for his assistance in collecting and processing SEM and EDX data and Jonathon Duay for his assistance in collecting and processing the XRF data.
AUTHOR DECLARATIONS
Conflict of Interest
The authors have no conflicts to disclose.
Author Contributions
Melissa L. Meyerson: Investigation (equal); Methodology (equal); Writing – original draft (lead). Samantha G. Rosenberg: Investigation (equal); Methodology (equal); Writing – review & editing (equal). Bryan R. Wygant: Funding acquisition (lead); Methodology (equal); Resources (lead); Writing – original draft (equal).
DATA AVAILABILITY
The data that support the findings of this study are available within the article and its supplementary material.