EBSD data were collected at the Microscopy and Microanalysis Facility, John de Laeter Centre, Curtin University, using a Tescan MIRA3 SEM with Oxford Instruments Symmetry EBSD detector. Data were collected at 20 kV and ~1 nA beam current, with an analytical step size of 2 μm. EBSD data were collected using Oxford Aztec 4.1 acquisition software. Data were noise reduced using a wildspike and 5 nearest neighbor zero solution algorithm in Oxford Instruments Channel 5.12 software. Channel 5.12 was also used to create misorientation maps used to investigate the microstructural relationship between spinel core and rim. Relatively poor-indexing of the spinel represents the difficulty in polishing the analyzed grains after laser-ablation analysis.
Channel 5
Manufactured by Oxford Instruments
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Channel 5 is a software application used to control and analyze data from Oxford Instruments' scientific instruments. It provides a user interface for configuring, operating, and monitoring the instruments.
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Lab products found in correlation
Symmetry ebsd detector, by Oxford Instruments (1 mentions)
Tecnai g2 f30, by Thermo Fisher Scientific (1 mentions)
Jsm 6510, by JEOL (1 mentions)
Jsm 7200f, by JEOL (1 mentions)
Sigma field emission gun scanning electron microscope, by Zeiss (1 mentions)
Sigma fesem, by Zeiss (1 mentions)
Nordlysebsd detector, by Oxford Instruments (1 mentions)
Aztech, by Oxford Instruments (1 mentions)
6 protocols using channel 5
1
EBSD Analysis of Spinel Microstructure
2
EBSD Mapping of Periclase, Spinel, and Monticellite
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EBSD mapping was performed using a Tescan MIRA3 Field Emission SEM, with an Oxford Instruments AZtec acquisition system that has combined energy dispersive X-ray (EDX) and EBSD capability. The data were collected at 20 kV, a beam current of ~ 1 nA, and a working distance of 20 mm. The sample was tilted at 70° and EBSD data were collected in map form covering ~ 2500 µm2 and the step size used for data collection was 200 nm. Collected electron backscatter diffraction patterns were indexed by reference to crystallographic data for periclase, spinel, and monticellite. Post-processing of EBSD data to produce phase and orientation maps was undertaken in Oxford Instruments Channel 5.12 software. Following standard EBSD protocols, a wildspike and a 6 nearest neighbour noise reduction was undertaken on the data.
3
Microstructural Characterization of Specimens
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The microstructures of specimens were observed by a JSM-6510 scanning electron microscope (SEM, JEOL, Tokyo, Japan) with an accelerating voltage of 20 kV and a Tecnai G2 F30 transmission electron microscope (TEM, FEI, Amsterdam, The Netherlands). The SEM specimens were ground, polished and then etched by 3 mL HNO3 + 9 mL HCl + 12 mL H2O. The TEM specimens were ground to 50 μm, punched to Φ3 mm discs and ion-milled. To further analyze the textures and microstructures, the rolling surface as defined by rolling direction (RD) and transverse direction (TD) were studied by electron backscattered diffraction (EBSD). Specimens were electro-polished by an applied potential of 30 V with 5% perchloric acid + 95% alcohol at −25 °C for 60 s. EBSD measurements were carried out by using the JSM-7200F field emission scanning electron microscope (FESEM, JEOL, Tokyo, Japan) with EBSD detector. The step of EBSD was 0.5 µm, and the EBSD data were analyzed by using the Channel 5 software (Oxford Instruments, Oxford, UK). The low-angle grain boundaries (LAGBs) were defined as 2° ≤ θ ≤ 15°, while the high-angle grain boundaries (HAGBs) were defined as θ > 15°.
4
Microstructural Characterization of Materials
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Microstructural observations were initially made using a standard research-grade polarised optical microscope. Selected samples were analysed using a Zeiss Sigma Field-Emission Gun scanning electron microscope in the Otago Micro and Nanoscale Imaging (OMNI) facility at the University of Otago. Backscatter electron (BE) and secondary electron (SE) images were acquired using a 15 keV accelerating voltage and 6.6–8 mm working distance. Electron Backscatter Diffraction (EBSD) data were acquired using an HKL Synergy Integrated EDS/EBSD system (Oxford Instruments) with an accelerating voltage of 30 kV and an aperture of 300 μm. Post-acquisition EBSD data processing was performed in Channel 5 software (Oxford Instruments) and the MTEX toolbox for MATLAB. Energy-Dispersive X-Ray Spectroscopy (EDS) measurements of chemical composition were acquired with an acceleration voltage of 15 kV, a beam current of approximately 1 nA, a live count time of 60 s, and a working distance of 8.5 mm.
5
Correlating Cu Electrocatalyst Orientation
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EBSD measurements
were performed on the samples after SECCM analysis. A Zeiss SIGMA
FE-SEM instrument (Zeiss, Germany) with a Nordlys EBSD detector (Oxford
Instruments, U.K.) was used. EBSD images were collected at 20 keV
accelerating voltage, with the sample tilted at 70° to the detector.
Note that the penetration depth is typically ∼70 nm on Cu for
the acceleration voltage employed in this work.54 (link) Therefore, activity correlations in this work are with
the “bulk” orientation of the grains, which we consider
to be reasonable for the ex situ evaluation of the post-catalyst structure,
noting that Cu electrocatalysts are expected to be dynamic during
eCO2RR.22 (link),23 (link) The z—normal direction
IPF (IPFz) color maps were extracted from AZtech
software linked with the instrument controls (AZtech, Oxford Instruments,
UK). Following EBSD characterization, the AZtechICE software package
(Oxford Instruments, UK) and Tango program in CHANNEL 5 software (Oxford
Instruments HKL, Denmark) were used to interrogate the acquired EBSD
data to extract the grain boundary lines and average grain parameters
(e.g., the Euler angles for deriving the average
Miller indexes) of grains that were relevant for correlation with
SECCM data.
were performed on the samples after SECCM analysis. A Zeiss SIGMA
FE-SEM instrument (Zeiss, Germany) with a Nordlys EBSD detector (Oxford
Instruments, U.K.) was used. EBSD images were collected at 20 keV
accelerating voltage, with the sample tilted at 70° to the detector.
Note that the penetration depth is typically ∼70 nm on Cu for
the acceleration voltage employed in this work.54 (link) Therefore, activity correlations in this work are with
the “bulk” orientation of the grains, which we consider
to be reasonable for the ex situ evaluation of the post-catalyst structure,
noting that Cu electrocatalysts are expected to be dynamic during
eCO2RR.22 (link),23 (link) The z—normal direction
IPF (IPFz) color maps were extracted from AZtech
software linked with the instrument controls (AZtech, Oxford Instruments,
UK). Following EBSD characterization, the AZtechICE software package
(Oxford Instruments, UK) and Tango program in CHANNEL 5 software (Oxford
Instruments HKL, Denmark) were used to interrogate the acquired EBSD
data to extract the grain boundary lines and average grain parameters
(e.g., the Euler angles for deriving the average
Miller indexes) of grains that were relevant for correlation with
SECCM data.
6
Microstructure Characterization via EBSD
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The average size of all grains (crystallites) was determined in the microstructure of all specimens by means of EBSD, utilizing Oxford Instruments Channel 5 software. The average size was calculated as a diameter of a circle equivalent to an average area of crystallites. A crystallite was considered as an object circumscribed by boundaries with at least 7° misorientation angles. All of the crystallites, with the exception of the ones smaller than 1 µm, were analyzed (Figure 2 ).
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