A Small Spot, Inert Gas, Ion Milling Process as a Complementary Technique to Focused Ion Beam Specimen Preparation

Fischione, Paul; Williams, Robert E.A.; Genç, Arda; Fraser, Hamish L.; Dunin-Borkowski, Rafal E.; Luysberg, M.; Bonifacio, Cecile S.; Kovács, András

doi:10.1017/s1431927617000514

Cited by 24 publications

(11 citation statements)

References 43 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Several groups have demonstrated the effectiveness of low energy inert gas ion milling in removing the surface damaged layer or reducing the thickness of the damaged layer. This method can reduce surface roughness of the specimen, revealing the intrinsic material beneath while further reducing the specimen thickness, ultimately resulting in electron transparent areas (Barna et al, 1999; Giannuzzi, 2006; Jin et al, 2010; Mitome, 2012; Fischione et al, 2017). Low energy (<1 keV) inert gas (Ar) ion milling was performed to determine whether the nanoscale features are intrinsic structures or surface artifacts.…”

Section: Resultsmentioning

confidence: 99%

Ion Beam Induced Artifacts in Lead-Based Chalcogenides

et al. 2019

View full text Add to dashboard Cite

Metal chalcogenides have attracted great attention because of their broad applications. It has been well acknowledged that microstructure can alter the intrinsic properties and performance of metal chalcogenides. The structure–property–performance relationships can be investigated at atomic scale with scanning transmission and transmission electron microscopy (STEM and TEM). Nevertheless, careful specimen preparation is paramount for accurate analyses and interpretations. In this work, we compare the effects of a variety of well-established TEM specimen preparation methods on the observed microstructure of an ingot stoichiometric lead telluride (PbTe). Most importantly, from aberration corrected STEM and first principles calculations, we discovered that argon (Ar) ion milling can lead to surface irradiation damage in the form of Pb vacancy clusters and self-interstitial atom (SIA) clusters. The SIA clusters appear as orthogonal nanoscale features when characterized along the <001> crystal orientation of the rock salt structured PbTe. This obfuscates the interpretation of the intrinsic microstructure of metal chalcogenides, especially lead chalcogenides. We demonstrate that with sufficiently low energy (300 eV) Ar ion cleaning or appropriate high-temperature annealing, the surface damage layer can be properly cleaned and the orthogonal nanoscale features are significantly reduced. This reveals the materials’ intrinsic structure and can be used as the standard protocol for future TEM specimen preparation of lead-based chalcogenide materials.

show abstract

Section: Resultsmentioning

confidence: 99%

Ion Beam Induced Artifacts in Lead-Based Chalcogenides

et al. 2019

View full text Add to dashboard Cite

show abstract

“…The amorphization coincides with the heating of the outer sample surface in the course of the collision cascade (Volkert and Minor, 2007;Fischione et al, 2017) along with the occurrence of so-called "thermal spikes", which can easily reach a few thousand kelvin (Ovchinnikov et al, 2015). Because of the immediate vaporization of the affected volume within 10 −12 s (Ovchinnikov et al, 2015), the thermal effect on the bulk material is rather low.…”

Section: Introductionmentioning

confidence: 92%

Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

Macholdt

Förster

Müller

et al. 2019

Geosci. Instrum. Method. Data Syst.

View full text Add to dashboard Cite

Abstract. The spatial distribution of transition metal valence states is of broad interest in the microanalysis of geological and environmental samples. An example is rock varnish, a natural manganese (Mn)-rich rock coating, whose genesis mechanism remains a subject of scientific debate. We conducted scanning transmission X-ray microscopy with near-edge X-ray absorption fine-structure spectroscopy (STXM-NEXAFS) measurements of the abundance and spatial distribution of different Mn oxidation states within the nano- to micrometer thick varnish crusts. Such microanalytical measurements of thin and hard rock crusts require sample preparation with minimal contamination risk. Focused ion beam (FIB) slicing was used to obtain ∼100–1000 nm thin wedge-shaped slices of the samples for STXM, using standard parameters. However, while this preparation is suitable for investigating element distributions and structures in rock samples, we observed artifactual modifications of the Mn oxidation states at the surfaces of the FIB slices. Our results suggest that the preparation causes a reduction of Mn4+ to Mn2+. We draw attention to this issue, since FIB slicing, scanning electron microscopy (SEM) imaging, and other preparation and visualization techniques operating in the kilo-electron-volt range are well-established in geosciences, but researchers are often unaware of the potential for the reduction of Mn and possibly other elements in the samples.

show abstract

“…Nanomilling is an effective tool for final thinning and cleaning of TEM specimens following other preparations by low voltage Ga + FIB milling or mechanical polishing. Nanomilling uses a focused Ar beam to polish both sides of the TEM specimen [54,133]. The spot size of an Ar beam is as small as 1 µm-smaller than the size of TEM lamella-so there will be no milling or redeposition of the specimen grid material (e.g., copper or molybdenum) if correct milling procedures are used [134].…”

Section: Nanomillingmentioning

confidence: 99%

A Review of Grain Boundary and Heterointerface Characterization in Polycrystalline Oxides by (Scanning) Transmission Electron Microscopy

et al. 2021

View full text Add to dashboard Cite

Interfaces such as grain boundaries (GBs) and heterointerfaces (HIs) are known to play a crucial role in structure-property relationships of polycrystalline materials. While several methods have been used to characterize such interfaces, advanced transmission electron microscopy (TEM) and scanning TEM (STEM) techniques have proven to be uniquely powerful tools, enabling quantification of atomic structure, electronic structure, chemistry, order/disorder, and point defect distributions below the atomic scale. This review focuses on recent progress in characterization of polycrystalline oxide interfaces using S/TEM techniques including imaging, analytical spectroscopies such as energy dispersive X-ray spectroscopy (EDXS) and electron energy-loss spectroscopy (EELS) and scanning diffraction methods such as precession electron nano diffraction (PEND) and 4D-STEM. First, a brief introduction to interfaces, GBs, HIs, and relevant techniques is given. Then, experimental studies which directly correlate GB/HI S/TEM characterization with measured properties of polycrystalline oxides are presented to both strengthen our understanding of these interfaces, and to demonstrate the instrumental capabilities available in the S/TEM. Finally, existing challenges and future development opportunities are discussed. In summary, this article is prepared as a guide for scientists and engineers interested in learning about, and/or using advanced S/TEM techniques to characterize interfaces in polycrystalline materials, particularly ceramic oxides.

show abstract

A Small Spot, Inert Gas, Ion Milling Process as a Complementary Technique to Focused Ion Beam Specimen Preparation

Cited by 24 publications

References 43 publications

Ion Beam Induced Artifacts in Lead-Based Chalcogenides

Ion Beam Induced Artifacts in Lead-Based Chalcogenides

Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

A Review of Grain Boundary and Heterointerface Characterization in Polycrystalline Oxides by (Scanning) Transmission Electron Microscopy

Contact Info

Product

Resources

About