For iDPC image acquisition, the cross-sectional TEM specimens were thinned to less than ~30 μm first by using mechanical polishing and then by performing argon ion milling. The ion-beam milling was carried out using the Precision Ion Polishing System (Model 691, Gatan Inc.) with an accelerating voltage of 3.5 kV until a hole was made. Low voltage milling was performed with an accelerating voltage of 0.3 kV to remove the surface amorphous layer and to minimize damage.
Precision ion polishing system
Manufactured by Ametek
The Precision Ion Polishing System is a laboratory equipment designed to prepare high-quality, electron-transparent specimens for transmission electron microscopy (TEM) analysis. The system utilizes a focused ion beam to gently and precisely remove material from the sample surface, resulting in a thin, electron-transparent specimen suitable for high-resolution imaging and analysis.
Automatically generated - may contain errors
Lab products found in correlation
Helios nanolab dualbeam 650, by Thermo Fisher Scientific (1 mentions)
Jem 2010f, by JEOL (1 mentions)
Dimplegrinder, by Ametek (1 mentions)
Themis g2, by Thermo Fisher Scientific (1 mentions)
Titan 80 300 microscope, by Thermo Fisher Scientific (1 mentions)
Cm20 microscope, by Philips (1 mentions)
Jsm 6700f, by JEOL (1 mentions)
10 protocols using precision ion polishing system
1
Transmission Electron Microscopy Specimen Preparation
2
Characterization of Wear Subsurface Layers
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Cross-sectional structural characterization of the wear subsurface layers in these samples was carried out using an FEI Nova NanoSEM 430 system and a JEM-2010 TEM operated at a voltage of 200 kV. The cross-sectional TEM foils of the as-prepared GNG sample were made by electrodepositing a Cu coating (about 1.5 mm thick) on the GNG surface, cutting cross-sectional foils, mechanical polishing, and ion milling using the Gatan precision ion polishing system.
For the worn samples, cross-sectional TEM foils for the characterization of wear subsurface were prepared by cutting at the middle of the wear track parallel to the sliding direction using the standard lift-out method in a focused ion beam (FIB) system (FEI Helios NanoLab DualBeam 650). A thin layer of platinum was deposited on the worn surface for protection against the beam damage. For microstructure characterization at deep subsurface positions, cross-sectional samples were cut perpendicular to the sliding direction in the center of the wear tracks. TEM foils were accurately positioned and prepared using the FIB lift-out method. Similarly, a thin platinum layer was deposited on the sample surfaces for protection.
For the worn samples, cross-sectional TEM foils for the characterization of wear subsurface were prepared by cutting at the middle of the wear track parallel to the sliding direction using the standard lift-out method in a focused ion beam (FIB) system (FEI Helios NanoLab DualBeam 650). A thin layer of platinum was deposited on the worn surface for protection against the beam damage. For microstructure characterization at deep subsurface positions, cross-sectional samples were cut perpendicular to the sliding direction in the center of the wear tracks. TEM foils were accurately positioned and prepared using the FIB lift-out method. Similarly, a thin platinum layer was deposited on the sample surfaces for protection.
3
Cross-Sectional TEM Sample Preparation
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The TEM samples used for the analysis were prepared in cross-sectional geometry using standard procedure of mechanical grinding and dimpling. Afterwards they have been thinned by argon ion beam milling with an energy of 4 keV under an incident angle of 4° using a Gatan precision ion polishing system. The TEM data were collected in a JEM-2100F operated at 80 kV equipped with a field emission gun. Additional TEM images were taken with a JEM-3010 operated at 200 kV.
4
Microstructural Characterization of Metal Alloys
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The microstructure, phase composition and structure of the alloys were characterized by SEM equipped with EDS and electron back-scattered diffraction (EBSD) system, X-ray diffraction (XRD) and transmission electron microscope (TEM). All the specimens for SEM observation were polished with 3000 grit SiC abrasive papers and etched in a 3% HNO3/C2H5OH solution. For EBSD tests, the specimens with size of 4 × 4 × 3 mm3 were polished with 3000 grit SiC abrasive papers, and then electrolytic polishing was conducted at constant current with specimen as anode and stainless as cathode in the electrolyte solution (alcohol anhydrous and phosphate, with the volume ratio 3:5). XRD was carried out on Xpert-Pro diffractometer with Cu Kα radiation in the range from 20° to 80° with a step of 0.02°. The thin foil samples for TEM observation were prepared by polishing small plates to thickness of ~30 μm, and finally using Gatan Precision Ion Polishing System until a hole appeared.
5
TEM Sample Preparation Protocol
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The
sample was cut into blocks and mounted face to face in a brass
ring with epoxy glue. The TEM specimen was ground to a thickness of
100 μm and dimpled down to 15 μm at the disc center (Dimple
grinder, Gatan, Inc., Warrendale, PA). The TEM specimen was finally
ion-milled (PIPS, Precision Ion Polishing System, Gatan, Inc., Warrendale,
PA) using 3 kV Ar+ ions at an incidence angle of 8°
until perforation. Detailed structural investigations of the sample
were performed using a 200 kV transmission electron microscope with
field emission electron gun (JEM-2010F, Jeol Ltd., Tokyo, Japan).
sample was cut into blocks and mounted face to face in a brass
ring with epoxy glue. The TEM specimen was ground to a thickness of
100 μm and dimpled down to 15 μm at the disc center (Dimple
grinder, Gatan, Inc., Warrendale, PA). The TEM specimen was finally
ion-milled (PIPS, Precision Ion Polishing System, Gatan, Inc., Warrendale,
PA) using 3 kV Ar+ ions at an incidence angle of 8°
until perforation. Detailed structural investigations of the sample
were performed using a 200 kV transmission electron microscope with
field emission electron gun (JEM-2010F, Jeol Ltd., Tokyo, Japan).
6
Preparation of STEM Specimen via Ion Milling
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The cross-sectional STEM specimen was prepared by conventional mechanical polishing followed by argon ion milling. The argon ion milling was carried out using the Precision Ion Polishing System (model 691; Gatan Inc.). The accelerating voltage was first set at 3.5 kV with angles ± 6° until a hole was made and then lowered to 1.0 kV with angles ± 3° until the hole was enlarged to the interface, and finally lowered to 0.1 kV for 2 min to remove the surface amorphous layer without damage. The specimen was baked at 160°C for 16 h to further remove the surface contamination layer before EELS experiments.
7
Atomic-Scale Imaging of Materials
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The sample for STEM was obtained by focused ion beam milling via the Precision Ion Polishing System (Model 691, Gatan Inc.). High-angle annular dark-field (HAADF) images were collected at 300 kV by using an aberration-corrected FEI Titan Themis G2 with spatial resolutions up to 60 pm.
8
Atomic-Resolution STEM Imaging of Polar Structures
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The planar view TEM sample was mechanically polished using Allied High Tech MultiPrep at 0.5° wedge angle, then ion-milled initially at 4 keV, and finished with 200 eV for final cleaning using a Gatan Precision ion polishing system. To image the local microstructure and detect the polarization distribution of the planar view TEM sample, atomic-resolution STEM images were acquired on a spherical aberration (Cs)–corrected FEI Titan 80-300 microscope operated at 300 kV with a point-to-point resolution of 50 pm at the National Center for Electron Microscopy, Lawrence Berkeley National Laboratory. Pairs of orthogonal scan images were used to correct the nonlinear drift distortions of the microscope in STEM mode. Using an established displacement vector-mapping algorithm (13 (link), 22 (link)), the local noncentrosymmetry of atomic columns in the ABO3 lattice was probed to determine the polar structures.
9
Thin Foil Preparation for TEM
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The thin foil for TEM observations was cut at 45° from the compression axis and prepared by slow mechanical polishing and dimpling down to a few microns. Subsequently the thin foil was glued on molybdenum grid and thinned down to electron transparency in a Precision Ion Polishing System (PIPS from Gatan). TEM observations were performed on a Phillips CM20 microscope operating at 200 kV.
10
Electron Microscopy Sample Preparation
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Electron Microscopy) observations were carried out on a JEOL JSM6700F. Samples for crosssectional TEM analysis were prepared following the standard method: the samples were first mechanically polished down to about 10 micron thickness, then the final thinning to electron transparency was achieved by ion milling at low angle (7°) and low voltage (5 kV) using a Precision Ion Polishing System (PIPS from Gatan). The TEM samples were investigated using a Tecnai F20 fitted with a Cs corrector (CEOS) which point resolution is 0.12 nm.
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