scholarly journals The universal sample holders of microanalytical instruments of FIB, TEM, NanoSIMS, and STXM-NEXAFS for the coordinated analysis of extraterrestrial materials

2020 ◽  
Author(s):  
Motoo Ito ◽  
Naotaka Tomioka ◽  
Kentaro Uesugi ◽  
Masayuki Uesugi ◽  
Yu Kodama ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Isotopic Abundances ◽  
Sample Return Mission ◽  
Extraterrestrial Materials ◽  
Sample Damage

Abstract We developed universal sample holders (the Kochi grid, Kochi clamp, and Okazaki cell) and a transfer vessel (facility-to-facility transfer container (FFTC)) to analyze sensitive and fragile samples, such as extremely small extraterrestrial materials. The holders and container prevent degradation, contamination due to terrestrial atmosphere (water vapor and oxygen gas) and small particles, as well as mechanical sample damages. The FFTC can isolate the samples from the effects of the atmosphere for more than a week. The Kochi grid and clamp were made for a coordinate micro/nano-analysis that utilize a focused-ion beam apparatus, transmission electron microscope, and nanoscale secondary ion mass spectrometry. The Okazaki cell was made as an additional attachment for a scanning transmission X-ray microscope that uses near edge X-ray absorption fine structure. The coordinated analysis involving these holders was successfully carried out without any sample damage or loss, thereby enabling us to obtain sufficient quality of analytical datasets of textures, crystallography, elemental/isotopic abundances, and molecular functional groups for µm-sized minerals and organics in both an Antarctic micrometeorite and a carbonaceous chondrite. We will apply the coordinated analysis to acquire the complex characteristics in samples that obtain by the future spacecraft sample return mission.

scholarly journals The universal sample holders of microanalytical instruments of FIB, TEM, NanoSIMS, and STXM-NEXAFS for the coordinated analysis of extraterrestrial materials

2020 ◽  
Author(s):  
Motoo Ito ◽  
Naotaka Tomioka ◽  
Kentaro Uesugi ◽  
Masayuki Uesugi ◽  
Yu Kodama ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Isotopic Abundances ◽  
Sample Return Mission ◽  
Extraterrestrial Materials ◽  
Sample Damage

Abstract We developed universal sample holders (the Kochi grid, Kochi clamp, and Okazaki cell) and a transfer vessel (facility-to-facility transfer container (FFTC)) to analyze sensitive and fragile samples, such as extremely small extraterrestrial materials. The holders and container prevent degradation, contamination due to terrestrial atmosphere (water vapor and oxygen gas) and small particles, as well as mechanical sample damages. The FFTC can isolate the samples from the effects of the atmosphere for more than a week. The Kochi grid and clamp were made for a coordinate micro/nano-analysis that utilize a focused-ion beam apparatus, transmission electron microscope, and nanoscale secondary ion mass spectrometry. The Okazaki cell was made as an additional attachment for a scanning transmission X-ray microscope that uses near edge X-ray absorption fine structure. The coordinated analysis involving these holders was successfully carried out without any sample damage or loss, thereby enabling us to obtain sufficient quality of analytical datasets of textures, crystallography, elemental/isotopic abundances, and molecular functional groups for µm-sized minerals and organics in both an Antarctic micrometeorite and a carbonaceous chondrite. We will apply the coordinated analysis to acquire the complex characteristics in samples that obtain by the future spacecraft sample return mission.

scholarly journals The universal sample holders of microanalytical instruments of FIB, TEM, NanoSIMS, and STXM-NEXAFS for the coordinated analysis of extraterrestrial materials

2020 ◽  
Vol 72 (1) ◽  
Author(s):  
Motoo Ito ◽  
Naotaka Tomioka ◽  
Kentaro Uesugi ◽  
Masayuki Uesugi ◽  
Yu Kodama ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Isotopic Abundances ◽  
Sample Return Mission ◽  
Extraterrestrial Materials ◽  
Sample Damage

Abstract We developed universal sample holders [the Kochi grid, Kochi clamp, and Okazaki cell) and a transfer vessel (facility-to-facility transfer container (FFTC)] to analyze sensitive and fragile samples, such as extremely small extraterrestrial materials. The holders and container prevent degradation, contamination due to the terrestrial atmosphere (water vapor and oxygen gas) and small particles, as well as mechanical sample damage. The FFTC can isolate the samples from the effects of the atmosphere for more than a week. The Kochi grid and clamp were made for a coordinated micro/nano-analysis that utilizes a focused-ion beam apparatus, transmission electron microscope, and nanoscale secondary ion mass spectrometry. The Okazaki cell was developed as an additional attachment for a scanning transmission X-ray microscope that uses near-edge X-ray absorption fine structure (NEXAFS). These new apparatuses help to minimize possible alterations from the exposure of the samples to air. The coordinated analysis involving these holders was successfully carried out without any sample damage or loss, thereby enabling us to obtain sufficient analytical datasets of textures, crystallography, elemental/isotopic abundances, and molecular functional groups for µm-sized minerals and organics in both the Antarctic micrometeorite and a carbonaceous chondrite. We will apply the coordinated analysis to acquire the complex characteristics in samples obtained by the future spacecraft sample return mission.

scholarly journals The Universal Sample Holders of Microanalytical Instruments of FIB, TEM, NanoSIMS, and STXM-NEXAFS for the Coordinated Analysis of Extraterrestrial Materials

2020 ◽  
Author(s):  
Motoo Ito ◽  
Naotaka Tomioka ◽  
Kentaro Uesugi ◽  
Masayuki Uesugi ◽  
Yu Kodama ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Secondary Ion Mass Spectrometry ◽  
Ion Beam ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Isotopic Abundances ◽  
Sample Return Mission ◽  
Extraterrestrial Materials ◽  
Sample Damage

Abstract We developed universal sample holders (the Kochi grid, Kochi clamp, and Okazaki cell) and a transfer vessel (facility-to-facility transfer container (FFTC)) to analyze sensitive and fragile samples, such as extremely small extraterrestrial materials. The holders and container prevent degradation, contamination due to the terrestrial atmosphere (water vapor and oxygen gas) and small particles, as well as mechanical sample damage. The FFTC can isolate the samples from the effects of the atmosphere for more than a week. The Kochi grid and clamp were made for a coordinated micro/nano-analysis that utilizes a focused-ion beam apparatus, transmission electron microscope, and nanoscale secondary ion mass spectrometry. The Okazaki cell was developed as an additional attachment for a scanning transmission X-ray microscope that uses near-edge X-ray absorption fine structure (NEXAFS). These new apparatuses help to minimize possible alterations from the exposure of the samples to air. The coordinated analysis involving these holders was successfully carried out without any sample damage or loss, thereby enabling us to obtain sufficient analytical datasets of textures, crystallography, elemental/isotopic abundances, and molecular functional groups for µm-sized minerals and organics in both the Antarctic micrometeorite and a carbonaceous chondrite. We will apply the coordinated analysis to acquire the complex characteristics in samples obtained by the future spacecraft sample return mission.

3D Observation of Elemental Distribution of Si-Device using a Dedicated FIB/STEM System

2005 ◽  
Author(s):  
T. Yaguchi ◽  
M. Konno ◽  
T. Kamino ◽  
M. Ogasawara ◽  
K. Kaji ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Three Dimensional ◽  
Elemental Distribution ◽  
Multivariate Statistical ◽  
X Ray ◽  
Sample Rotation ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Elemental Maps

Abstract A technique for preparation of a pillar shaped sample and its multi-directional observation of the sample using a focused ion beam (FIB) / scanning transmission electron microscopy (STEM) system has been developed. The system employs an FIB/STEM compatible sample rotation holder with a specially designed rotation mechanism, which allows the sample to be rotated 360 degrees [1-3]. This technique was used for the three dimensional (3D) elemental mapping of a contact plug of a Si device in 90 nm technology. A specimen containing a contact plug was shaped to a pillar sample with a cross section of 200 nm x 200 nm and a 5 um length. Elemental analysis was performed with a 200 kV HD-2300 STEM equipped with the EDAX genesis Energy dispersive X-ray spectroscopy (EDX) system. Spectrum imaging combined with multivariate statistical analysis (MSA) [4, 5] was used to enhance the weak X-ray signals of the doped area, which contain a low concentration of As-K. The distributions of elements, especially the dopant As, were successfully enhanced by MSA. The elemental maps were .. reconstructed from the maps.

FIB Preparation of a NiO Wedge-Lamella and STEM X-Ray Microanalysis for the Determination of the Experimental k(O-Ni) Cliff-Lorimer Coefficient

2013 ◽  
Vol 19 (1) ◽  
pp. 79-84 ◽  
Author(s):  
Aldo Armigliato ◽  
Stefano Frabboni ◽  
Gian Carlo Gazzadi ◽  
Rodolfo Rosa
Keyword(s):  
Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Analytical Electron Microscopy ◽  
X Ray ◽  
Transmission Electron ◽  
The Monte Carlo Method ◽  
Scanning Transmission ◽  
Reliable Quantification ◽  
Experimental Values

AbstractA method for the fabrication of a wedge-shaped thin NiO lamella by focused ion beam is reported. The starting sample is an oxidized bulk single crystalline, ⟨100⟩ oriented, Ni commercial standard. The lamella is employed for the determination, by analytical electron microscopy at 200 kV of the experimental k(O-Ni) Cliff-Lorimer (G. Cliff & G.W. Lorimer, J Microsc103, 203–207, 1975) coefficient, according to the extrapolation method by Van Cappellen (E. Van Cappellen, Microsc Microstruct Microanal1, 1–22, 1990). The result thus obtained is compared to the theoretical k(O-Ni) values either implemented into the commercial software for X-ray microanalysis quantification of the scanning transmission electron microscopy/energy dispersive spectrometry equipment or calculated by the Monte Carlo method. Significant differences among the three values are found. This confirms that for a reliable quantification of binary alloys containing light elements, the choice of the Cliff-Lorimer coefficients is crucial and experimental values are recommended.

Physical Failure Analysis Techniques for Front-End-of-Line Defect Analysis

2016 ◽  
Author(s):  
Dirk Doyle ◽  
Lawrence Benedict ◽  
Fritz Christian Awitan
Keyword(s):  
Cross Section ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Gate Oxide ◽  
Top Down ◽  
New Techniques ◽  
First Case ◽  
Transmission Electron ◽  
Scanning Transmission

Abstract Novel techniques to expose substrate-level defects are presented in this paper. New techniques such as inter-layer dielectric (ILD) thinning, high keV imaging, and XeF2 poly etch overflow are introduced. We describe these techniques as applied to two different defects types at FEOL. In the first case, by using ILD thinning and high keV imaging, coupled with focused ion beam (FIB) cross section and scanning transmission electron microscopy (STEM,) we were able to judge where to sample for TEM from a top down perspective while simultaneously providing the top down images giving both perspectives on the same sample. In the second case we show retention of the poly Si short after removal of CoSi2 formation on poly. Removal of the CoSi2 exposes the poly Si such that we can utilize XeF2 to remove poly without damaging gate oxide to reveal pinhole defects in the gate oxide. Overall, using these techniques have led to 1) increased chances of successfully finding the defects, 2) better characterization of the defects by having a planar view perspective and 3) reduced time in localizing defects compared to performing cross section alone.

scholarly journals An Analysis of Li Ion Secondary Battery Materials by Using Focused Ion Beam Micro-sampling Technique and Cold Field Emission Scanning Transmission Electron Microscope

2010 ◽  
Vol 16 (S2) ◽  
pp. 214-215
Author(s):  
T Tanigaki ◽  
K Ito ◽  
K Nakamura ◽  
Y Nagakubo ◽  
J Azuma ◽  
...  
Keyword(s):  
Electron Microscope ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Sampling Technique ◽  
Scanning Transmission Electron Microscope ◽  
Battery Materials ◽  
Secondary Battery ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Li Ion

Extended abstract of a paper presented at Microscopy and Microanalysis 2010 in Portland, Oregon, USA, August 1 – August 5, 2010.

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

2019 ◽  
Vol 8 (1) ◽  
pp. 97-111
Author(s):  
Dorothea S. Macholdt ◽  
Jan-David Förster ◽  
Maren Müller ◽  
Bettina Weber ◽  
Michael Kappl ◽  
...  
Keyword(s):  
Spatial Distribution ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Oxidation States ◽  
X Ray ◽  
Scientific Debate ◽  
Rock Samples ◽  
Valence States ◽  
Scanning Transmission ◽  
Visualization Techniques

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.

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