Jxa 8230

The crystalline structure of the alloy powders was analyzed using X-ray diffraction (XRD, PANalytical EMPYREAN, PANalytical B.V., Almero, Netherlands) with Cu-Kα radiation at 40 kV and 40 mA. The morphology of the powders was observed using a cold field emission scanning electron microscope (FESEM, JSM-6701F, JEOL Ltd. Tokyo, Japan). Magnetic properties were tested using a Physical Property Measurement System (PPMS-9, Quantum Design, San Diego, CA, USA) equipped with a 9 T vibrating sample magnetometer. Thermal stability analysis was recorded on a simultaneous thermal analyzer (TGA/DSC STA449F5, Netzsch, Selb, Germany) from room temperature to 800 °C at a 10 °C/min heating ramp with continuous nitrogen flow. Micro-area element distribution analysis was analyzed by using an electron probe micro-analyzer (EMPA, JXA-8230, JEOL Ltd. Tokyo, Japan). The test conditions were a voltage of 15.0 kV, test current of 5.078 × 10⁻⁷ A, and micro-area magnification of 50,000×.

The microstructure and element distribution at the interface were characterized by electron probe microanalysis (EPMA, JEOL JXA-8230) equipped with an X-ray spectroscopy detector. The power generation performance of Fe/BTS ATMTD was evaluated at a temperature difference from 10 to 40 K, using a self-made measuring equipment that was presented in our previous report [33 (link),34 (link)].

Concentrations of some divalent cation species were sclerochronologically quantified from the core to the edge of each otolith, because the vateritic phase is characterized by both lower strontium (Sr) and higher magnesium (Mg) concentrations than the aragonitic phase [5 (link)]. Prior to the analysis, the upper surface of the specimens was coated with platinum-palladium for 60 s in an ion-beam sputter coater (Hitachi E-1030) to enhance electrical conductivity. Chemical composition of the otoliths was obtained using a JEOL JXA-8230 electron probe microanalyser (EPMA) at the Atmosphere and Ocean Research Institute, University of Tokyo (see [37 (link)]). The wavelength-dispersive spectrometry (WDS) method was used to measure Ca, Mg and Sr concentrations with the electron beam of 5 µm in diameter with 5 µm intervals. Exposure times were set at 10 s for peaks and 5 s for background measurements with an accelerating voltage of 15 kV and a beam current of 12 nA. Wollastonite (CaSiO₃), magnesium oxide (MgO), and strontium titanate (SrTiO₃) were used as standard materials for the ZAF correction. Otoliths collected from all 18 individuals (n = 36) were subjected to the EPMA analysis.

Samples were first crushed into gravel-size chips. Clean chips were then pulverized in a corundum mill. Major element compositions of whole rocks were determined using a Thermo Scientific ARL 9900 X-ray fluorescence spectrometer (XRF) at the State Key Laboratory for Mineral Deposits Research, Nanjing University, China. Measurements of bulk rock trace element concentrations were completed at the Department of Geology, Northwest University, China. Trace elements were determined using an ELANG100DRC inductively coupled plasma mass spectrometer (ICP-MS) after the acid digestion (HF + HNO₃) conducted in Teflon bombs. Trace elemental analyses of the USGS rock standards (BHVO-2, BCR-2, and AGV-2) are reported for comparison. Major element analysis and BSE imaging of minerals were carried out by EPMA (JEOL JXA-8230) equipped with four wavelength-dispersive spectrometers at the State Key Laboratory of Marine Geology, Tongji University. Details of methods are provided in the Supplementary Materials.

Major element determinations were made on a JEOL Superprobe (JXA-8230) housed at Victoria University of Wellington, using the ZAF correction method. Analyses were performed with 15 kV accelerating voltage, 8 nA beam current, and an electron beam defocused to between 20 to 10 μm. Standardization was achieved by means of mineral and glass standards. A rhyolitic glass standard (VG-568) was routinely used to monitor calibration in all analytical runs, and used to evaluate any day-to-day differences in the calibration. The large number of samples precluded conducting all analyses in a single batch. All analyses are normalized to 100 wt.% anhydrous, with H₂O by difference being given, and total Fe is reported as FeO. Glass shard major element analyses are presented in SI Table 2.

Phase purity and crystal structure were investigated by powder XRD (Bruker D8 Advance, Germany). Chemical uniformities and compositions of the samples were characterized by an EPMA (JXA-8230, JEOL, Japan). The chemical compositions were averaged from 10 arbitrarily selected points. The microstructures of the samples with different compositions were examined by a field-emission SEM (MERLIN Compact FE-SEM, Carl Zeiss, Germany) and a high-resolution transmission electron microscope (JEOL2010, Japan).

All materials and solvents were purchased from Merck, Sigma-Aldrich, and Fluka and were employed as received without further purification. Fourier transform infrared (FT-IR) was performed in the range 400 to 4000 cm⁻¹ (PerkinElmer) using the KBr disc technique. Morphologies of the synthesized nanomaterials were analyzed using a Quantum 2000 field emission scanning electron microscope (FESEM). ¹H- and ¹³C-NMR spectra were recorded on a 300 MHz Bruker AVANCE III spectrometer using TMS as the internal reference. A Photonix UV-visible array spectrophotometer was used to record UV-visible spectra. Elemental analyses were carried out using a Thermo Finnigan (Flash-1112EA) microanalyzer. Energy dispersive X-ray spectroscopy (EDS, Bruker QUANTAX 200) was run with an electron probe microanalyser (JEOL JXA-8230) equipped with an energy dispersive spectrometer. Melting points were determined in open capillary tubes on Stuart BI Branstead Electrothermal IA9200 apparatus. X-ray diffraction (XRD) patterns were acquired at a scanning rate of 3° min⁻¹ using a Philips PW1730 diffractometer at 40 keV and 30 mA for monochromatized Cu Kα radiation in the 2θ domain from 10° to 80°. Thermogravimetric analyses were performed with a TGA 92 Setaram with a heating rate of 10 °C per minute.