To observe uranium-bearing loci by TEM, we fabricated electron-transparent ultrathin sections with a focused ion beam (FIB) sample preparation technique using a Hitachi FB-2100 instrument (Ibaraki, Japan) with a micro-sampling system. Before FIB fabrication, the thin section sample was coated by a carbon film and inserted into the FIB apparatus, then locally coated with the deposition of W (100–500 nm thick) for protection, trimmed using a Ga ion beam at an accelerating voltage of 30 kV and thinned down to a final thickness of 100–200 nm with a low energy beam of 10 kV as a final process. FIB-fabricated ultrathin sections were placed on a Cu specimen support with W deposition and observed by TEM. TEM examinations were performed at an accelerating voltage of 200 kV using a JEOL JEM-2010 UHR (LaB6 electron gun) with a nominal point resolution of ~0.2 nm. TEM-EDS was used for elemental analysis of U-bearing nanoparticles and Mg- and Fe-bearing aluminosilicate.
Fb 2100
Manufactured by Hitachi
Sourced in Japan
The FB-2100 is a laboratory equipment product manufactured by Hitachi. It is designed to perform specific tasks in a laboratory setting. The core function of the FB-2100 is to provide a solution for laboratory needs, but a detailed description while maintaining an unbiased and factual approach is not available.
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Lab products found in correlation
Jem 2010 uhr, by JEOL (2 mentions)
Tecnai osiris, by Thermo Fisher Scientific (2 mentions)
Sigma probe, by Thermo Fisher Scientific (2 mentions)
Jed 2200, by JEOL (1 mentions)
Jem 3100fef, by JEOL (1 mentions)
Noran system six, by Thermo Fisher Scientific (1 mentions)
Jem 2800, by JEOL (1 mentions)
Hd 2300a, by Hitachi (1 mentions)
X pert pro powder, by Malvern Panalytical (1 mentions)
Ki powder, by Merck Group (1 mentions)
Aunps, by Merck Group (1 mentions)
Su8230, by Hitachi (1 mentions)
Versastat 4, by Ametek (1 mentions)
Jem 2100f, by JEOL (1 mentions)
S 4800, by Hitachi (1 mentions)
V 650, by Jasco (1 mentions)
Xpert pro xrd system, by Malvern Panalytical (1 mentions)
Auriga laser, by Zeiss (1 mentions)
Super x system, by Thermo Fisher Scientific (1 mentions)
9 protocols using fb 2100
1
Uranium Nanoparticle Characterization by TEM
2
Microparticle Analysis by Advanced TEM
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Cross-sectional thin TEM specimens were prepared from radioactive microparticles using a focused ion beam (FIB) instrument with micro-sampling system (Hitachi FB-2100) as described in the supplementary information . Then specimens were initially examined using a TEM (JEOL JEM-2010UHR) operated at 200 kV with an EDS analyzer system (JEOL JED-2200). Elemental mapping in the microparticles and quantitative analyses were performed using a JEOL JEM-3100FEF operated at 300 kV in the STEM mode, with an EDS analyzer system (Thermo Fisher Scientific NORAN System SIX). Finally, elemental maps for nanoparticulates inside the microparticles were acquired using a JEOL JEM-2800 operated at 200 kV with double wide-area (0.95 sr.) silicon drift detectors (SDD) for EDS analyses.
3
Synthesis of a-Si Nanotips on Si Substrate
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To make an aqueous solution, KI powder (0.002 mol, Sigma-Aldrich, Seoul, Korea) and 10 mL of Au NPs (3 nM, particle size = 20 nm, Sigma-Aldrich, Seoul, Korea) dispersed in H2O were mixed in 80 mL of deionized water. Subsequently, 20 mL of 30% aqueous SMS (Gelest, Morrisville, PA, USA) was added to the mixed solution. In order to mix the solution properly, the aqueous solution was stirred magnetically at 85 °C on a hot plate. Then, samples were prepared by dropping aqueous solution onto the Si substrate. All samples were cooled down 4 °C or room temperature (RT), or maintained at 70 °C over 24 h until the solution droplets dried. The structural, compositional, and optical properties of the samples were investigated using scanning electron microscopy (SEM, SU-8230, Hitachi, Japan), energy-dispersive X-ray spectrometry (EDX, SU-8230, Hitachi, Japan), X-ray diffraction (XRD, X’pert Pro Powder, PANalytical, Netherlands), transmission electron microscopy (TEM, HD-2300A, Hitachi, Japan), and PL (SpectraPro 500i, Acton, USA). To further investigate the growth mechanism of the a-Si nanotips on the Si substrate, focused ion beam (FIB)-SEM (FB-2100, Hitachi, Japan) and atomic force microscopy (AFM, MOD-1M series, Nanofocus, Richmond, VA, USA) analyses were also performed.
4
Cross-Sectional FIB Thin Film Preparation
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Cross-sectional thin film was prepared using conventional FIB technique with Ga ion source (FB-2100, Hitachi). The samples were thinned to ~150 nm at acceleration voltage of 40 kV and then to ~100 nm at 10 kV. Prepared samples were placed on TEM grid with Mo mesh for observation.
5
Characterization and Photocatalytic Evaluation of MoS2/g-C3N4 Heterojunction
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We differentiated the well-constructed morphologies of the photoanode film using field-emission scanning electron microscopy (FE-SEM; model S4800, Hitachi, Japan), focused ion beam (FIB; model FB-2100, Hitachi, Japan) and transmission electron microscopy (TEM; model JEM-2100F, JEOL, Japan). To observe the crystalline structure and its properties, X-ray diffraction (XRD) using a Cu Kα source (model D/Max-2500/PC; Rigaku/USA Inc., USA) analysis was carried out on the MoS2 and g-C3N4 phases. Fourier transform infrared spectroscopy (FT-IR; model iS10; Thermo Fisher Scientific, UK) and X-ray photoelectron spectroscopy (XPS) using an Al Kα source (Sigma Probe; Thermo Fisher Scientific, UK) were used to confirm the formation of g-C3N4. Then, UV-VIS spectroscopy (model V650; JASCO, Japan) was used to observe the optical absorbance of the films so that we could calculate their band gap energy. Photoluminescence (PL; SC-100; Dongwoo, Korea) was employed to monitor the recombination rate of the as-prepared films at 325 nm laser excitation. All photocatalytic performance tests of transient photocurrents, Mott–Schottky analysis and electrochemical impedance spectroscopy (EIS) were carried out using a potentiostat (VersaSTAT 4; Princeton Applied Research, USA). The photocatalytic degradation solutions were measured by UV-VIS spectroscopy.
6
MOCVD Growth of InGaN Heterojunction
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The investigated heterojunction was deposited on a 2-μm-thick high-resistance GaN (HR-GaN) template by using the metal organic chemical vapor deposition (MOCVD). Before InGaN deposition, a long-time growth interrupt in both nitrogen and ammonia ambient was introduced to polish the interface. The growth interrupt can improve the interface quality, which was confirmed in our previous study28 29 . Then a super-thin unintentionally doped GaN (UID-GaN) spacer layer with the thickness of 5 nm was grown with an ultra-flat morphology. To compensate the high-density n-type background concentration and serve as a source of the holes, slightly Mg-doping is performed for the strained InGaN layer26 . A 5-nm-thick p-type GaN cap layer was used to screen surface trap effects and enable the formation of ohmic contacts. The material properties were characterized by XRD (Panalytical Xpert PRO XRD system), TEM (JEM-2000EX operated at 200 kV). The TEM sample was prepared by FIB process (Hitachi FB-2100).
7
Fabrication of 2D Plasmonic Nanostructure
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The sample was a transparent quartz plate, which was polished to the optical quality and then coated with a silver film with a thickness of about 200 nm. The grating was fabricated by ion etching using a focused ion beam setup (FB-2100, Hitachi). The structure represents a 2D regular array of round holes, as shown in Fig. 1 b. The structure contains 40 periods along each axis and has overall sizes of . The respective periods were , while the hole diameter was about , so the duty cycles of the structure were 0.5. The use of a nontransparent silver coating allowed us to achieve the high level of the amplitude modulation of the intensity, as can be seen in the optical microscopy image presented in Fig. 1 c.
8
Cross-sectional Characterization of Multilayer Structures
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Cross-sectional scanning electron microscopic (SEM) images of the multilayer structure were obtained by ZEISS Auriga Laser (Carl Zeiss, Oberkochen, Germany) combined with a focused ion beam (FIB) with a Ga+ ion source. The FIB processing was performed for the carbon protection coating (deposited from carbon gas) and subsequent making of crevices to reveal the cross-sectional observation surface. Next, the microstructure was observed by SEM operated at 1 kV under a 54° gradient condition. Cross-sectional high-angle annular dark field scanning TEM (HAADF-STEM) images were obtained by Tecnai Osiris (FEI, Hillsboro, OR, USA). Before FIB processing with a Ga+ ion source (FB-2100, Hitachi, Tokyo, Japan), the substrates were coated with a chromium (Cr)-containing oil-based ink to protect the surface. Next, FIB processing was performed for the tungsten (W) protection coating (deposited from W(CO)6 gas) and subsequent preparation of the cross-sectional samples. Each sample was then mounted on a copper (Cu) FIB lift-out grid and thinned to approximately 100 nm. The prepared cross-sectional ultrathin samples were analyzed using HAADF-STEM operated at 200 kV.
9
Cross-sectional TEM Analysis of Dentin
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Cross-sectional ultra-thin samples were prepared from the LAB-processed substrates using a focused ion beam (FIB) technique with a Ga + ion source (FB-2100, Hitachi, Japan). As a pretreatment, the substrate was coated manually with a Cr-containing oil-based ink to protect the surface. The substrate was then coated with tungsten using W(CO)6 gas. A cross-sectional sample was prepared from the substrate, fixed on a molybdenum FIB lift-out grid, and thinned to approximately 100 nm.
The cross-sectional ultra-thin samples were analyzed using an analytical transmission electron microscopy (TEM; Tecnai Osiris, FEI, USA) system operating at 200 kV and equipped with an EDX spectrometer (Super-X system, FEI, USA) and a high-angle annular dark field (HAADF) scanning transmission electron microscopy (STEM) system with a probe diameter of less than 1 nm. For comparison, we used cross-sectional STEM-EDX data for an unprocessed (as-prepared) dentin substrate obtained in our previous study [36] . In the quantitative analysis by STEM-EDX, three different regions in each sample were analyzed to obtain the mean and the standard deviation (SD).
The cross-sectional ultra-thin samples were analyzed using an analytical transmission electron microscopy (TEM; Tecnai Osiris, FEI, USA) system operating at 200 kV and equipped with an EDX spectrometer (Super-X system, FEI, USA) and a high-angle annular dark field (HAADF) scanning transmission electron microscopy (STEM) system with a probe diameter of less than 1 nm. For comparison, we used cross-sectional STEM-EDX data for an unprocessed (as-prepared) dentin substrate obtained in our previous study [36] . In the quantitative analysis by STEM-EDX, three different regions in each sample were analyzed to obtain the mean and the standard deviation (SD).
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