REELS Reflection Electron Energy Loss Spectroscopy 1 JAMP-9510F Field Emission Auger Microprobe Lithium Analysis Using Reflection EELS A Joint Project with The National Institute of Advanced Industrial Science and Technology On April 1, 2016, JEOL Ltd. (Gon’emon Kurihara, President) and the National Institute of Advanced Industrial Science and Technology, a national research and development organization (Ryoji Nakahachi, Director) officially announced a new joint project; Lithium Analysis using reflection EELS (Electron Energy Loss Spectroscopy). Reflection EELS is an analytical technique to measure kinetic energy change of electrons resulting from inelastic scattering when a beam of electrons is projected at a few keV onto the sample surface. Detailed analysis of the energy loss peaks of electrons provides chemical and structural information on the sample surface (approximately 10 nm deep). The objective of the joint project is to develop a scanning electron microscope designed for lithium analysis, which supports high energy resolution spectrometry using a hemispherical detector, as well as analytical techniques applicable to evaluation of lithium cell materials. At the initial stage, JEOL will contribute to the joint project in the fields of microscopy and metrology utilizing expertise in preliminary sample preparation and Auger spectrometry for lithium analysis. 3 Field Emission Auger Microprobe TFEG-SEM For High Resolution Imaging High Current, High Stability Field Emission Electron Gun Ar Ion Gun For Surface Processing (Cleaning & Depth Profiling) and Charge Neutralization Hemispherical Auger Electron Detector (HSA) For Surface Analysis E/T Secondary Electron Detector 5-Axis Mechanically Eucentric Specimen Stage (X, Y, Z, Tilt, Rotate) to maintain a clean surface Ultra High Vacuum Specimen Chamber (5×10-8 Pa or better) to maintain a clean surface θ φ HSA (Electron Analyzer) Sample Some incident or back scattered electrons can excite electron shells of atoms at the sample surface. Those electrons are observed in an Auger spectrum as energy loss peaks. We can analyze the energy positions of loss peaks to investigate the atomic chemical state of atoms much like TEM EELS but with much less sample prep Secondary Electron peak Loss peaks Auger elecron peaks Secondary Electron 0 Auger can provide an EELS spectra of the top surface 8000 Counts (arb. unit) 7000 6000 [Reference Data] TEM EELS spectrum of SiO2 [REELSspectrum (SiO2)] 1kV, 60nA, M1(Ep=10eV) Si L2,3 5000 4000 3000 2000 1000 0 80 90 100 110 120 Energy (eV) Ec Electron energy (eV) 130 140 Back Scatter Electron Back Scatter Electron peak (BSE) Incident Electrons Intensity of Electrons N(E) Reflection Electron Energy Loss Spectroscopy (REELS) Ep Probe Electron Energy Li spectra ~Li metal and Li oxyde (Li2O)~ [Core loss peak of Li (metal)] [Core loss peak of Li (Li2O)] 500 3000 2 kV, 80 nA, CAE (Ep=10 eV) 2 kV, 80 nA, CAE (Ep=10 eV) 2500 Intensity (Arb. unit) Intensity (Arb. unit) 400 300 200 100 1000 0 50 55 60 65 Loss energy (eV) 1 1500 500 0 45 2000 70 75 45 50 55 60 65 Loss energy (eV) 70 75 Li spectra ~Li (LiF) and Li (LiCl)~ Core loss peaks of Li (LiF) and Li (LiCl) Auger peaks of Li (LiF) and Li (LiCl) 2000 30000 LiCl LiF Li 1s : 62.4 eV 1000 Li 1s : 60.8eV 20000 N(E)/N(E) Intensity (sounts) 25000 LiCl LiF 15000 0 -1000 10000 Li KLL(LiCl) : 41eV -2000 5000 Li KLL(LiF) : 34eV 0 40 -3000 50 60 70 Loss Energy(eV) 2 80 90 20 30 40 50 60 70 Electron Energy (eV) 80 90 100
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