lithium ion battery (everything you need to know)

Applications note Lithium Ion Battery note LIB note Morphology Observation & Surface Analysis Instruments XRF / XPS / EPMA / AES / SEM / TEM / CP / FIB Chemical Analysis Instruments GC-MS / NMR Fabrication Systems Roll to Roll Electron Beam Deposition Systems RF Induction Thermal Plasma System for Nano Particle Synthesis 1 Morphology Observation & Surface Analysis Instruments Introduction P01 Lithium Ion Battery Basic Structure & Fabrication Pr ocess P02 1.Morphology Observation & Surface Analysis Instruments 1-1. Features to Consider for Instrument Selection P03 1-2. XRF: X-ray Fluorescence Spectr ometer P04 1-3. XPS: X-ray Photoelectron Spectr ometer P05 1-4. EPMA: Electron Pr obe Micro Analyzer P07 1-5. AES: Auger Electr on Spectrometer P09 1-6. SEM: Scanning Electron Micr oscope P11 1-7. TEM: T ransmission Electron Micr oscope P17 1-8. CP: Specimen Preparation Equipment: Air Isolation & Cooling CP , FIB P18 2.Chemical Analysis Instruments 2-1. GC-MS: Gas Chromatograph Mass Spectrometer P20 2-2. NMR: Nuclear Magnetic Resonance Spectrometer P21 3.Fabrication Systems 3-1. Roll to Roll Electron Beam Deposition Systems P23 3-2. RF Induction Thermal Plasma System for Nano Particle Synthesis P24 Conclusion Analysis Item and Applicable Instruments P25 INDEX 1 LIB note Introduction The appl i cati ons for l i th iu m ion ba t teri es (LIB ) co ver a w ide ra nge , from pow er sources for person al computers and mob i le dev ic es to aut omobi l es, an d there is a lw ay s a dema nd for ev en bet ter performance a nd saf et y . In order to en sure the performan ce and qu a l ity of LIB , ana l ys is an d eva l ua tion u si ng h i gh-per forman ce assessment sy stems is necessary . JEOL offers a ful l l ine-up of equ ipment t o support the devel opment of new L IB techno log ies and to i mpro ve produ ct qual i t y , in cl ud in g in struments for morphology observatio n and su r face an al ys is , chem ica l an al ys is sy stems to per form structura l an al ys is on a mo lec ul ar l ev el , as wel l as fabr ica tion systems to c reate h ig h-p er forma nce coa ti ngs and pow ders. Th is L IB note of fers sol ution s for researc hers and eng ineers who are l ooki ng for the best equ ipmen t for thei r app l ica tion . LIB note B LIB LIB B rang e, from pow er sources for pers ona l computers a demand f or ev en bet ter per forma nce a nd safety . an al ys is a nd ev al ua ti on us in g h igh-performanc e f equi pment to s uppor t the deve lopment of ne w LIB Lithium Ion Battery The basic structure of L IB consi st s of var ious \ue002\ue003\ue004\ue005\ue003\ue006\ue007\ue006\ue008 \ue009\ue00a\ue00b\ue00c\ue009\ue00b\ue009\ue00d\ue003\ue00e\ue006\ue00b\ue00f \ue006\ue00b\ue008\ue00d\ue007\ue00b\ue010\ue011\ue012 \ue013\ue007\ue00b\ue003\ue006\ue00b\ue008\ue00d\ue007\ue00b\ue014\ue007\ue015 \ue008\ue016 These component s ha ve a va riety of formats, \ue005\ue003\ue00e\ue017\ue007\ue013\ue009\ue00a\ue00b\ue009\ue00d\ue007\ue007\ue008 \ue009\ue00a\ue00b\ue018\ue012\ue00f\ue017\ue009 \ue00a\ue00b\ue00c\ue006\ue017\ue00b \ue008\ue00d\ue007\ue013\ue007\ue00b \ue00c\ue013\ue007\ue00b \ue017\ue00f\ue015\ue015\ue007\ue013\ue007\ue006\ue008\ue00b\ue00f\ue008\ue007\ue004\ue009\ue00b to assess for the vari ous ma teria l eva l uat ions. It i s al so nece ssary to make assessments af ter asse mbl y , and a f ter repeatin g the ch arge/ disc ha rge operat ions . \ue019\ue00d\ue007\ue00b \ue010\ue011\ue012\ue013\ue007\ue00b \ue01a\ue007\ue014 \ue003\ue00e\ue00b \ue009\ue00d\ue003 \ue00e\ue009\ue00b \ue007\ue01b\ue00c\ue004\ue005 \ue014\ue007\ue009\ue00b \ue003\ue015\ue00b \ue008\ue00d\ue007\ue00b \ue007\ue01c\ue012\ue00f\ue005\ue004\ue007\ue006\ue008\ue00b that i s su itable for m ateri al s assessment at the R& D lev el , and the equi pment useful f or maki ng the eva lu ati ons for eac h step of the fabricati on process. JE OL offers an a l y ti c i nstru men t sol u tio ns f or ea ch p roces s Positive electrode materials Negative electrode materials Separator Electrolyte Lithium Ion Battery Basic Structure & Fabrication Process LIB note 2 Cathode/ Anode materials Separator Electrolyte Cathode/ Anode materials Cathode/ Anode materials Winding, Extrusion, Drawing (cathode, anode, current collector , separator , electrolyte) Check battery performance Check deterioration process R&D Quality Control Fabrication Preparation of raw materials Coating / Press Cell assembly Aging Charging cycle test Gas Chromatography \u2013 Mass Spectrometer / GC-MS T ransmission Electron Microscope / TEM Auger Electron Spectr ometer / AES Nuclear Magnetic Resonance Spectrometer / NMR X-ray Fluorescence Spectrometer / XRF X-ray Photoelectron Spectrometer / XPS Scanning Electron Microscope / SEM Electron Pr obe Micro Analyzer / EPMA Electron Spin Resonance Spectrometer / ESR B 1 Morphology Observation & Surface Analysis Instruments Instrument Micro scale Nano s cale Features 1-1 Features to Consider for Instrument Selection The tables be lo w show the c ri teri a for se lectin g in strumen t s for m ateri a l assessmen t purposes. T ab le 1 l i sts the \ue015\ue007\ue00c\ue008\ue012 \ue013\ue007\ue009\ue00b\ue003\ue015\ue00b\ue007\ue00c\ue002 \ue00d\ue00b\ue00f\ue006 \ue009\ue008\ue013\ue012\ue004\ue007\ue006\ue008\ue00a\ue00b\ue00c\ue006\ue017\ue00b\ue019 \ue00c\ue01a \ue014\ue007\ue00b\ue01d\ue00b\ue009\ue00d\ue003 \ue00e\ue009\ue00b\ue00c\ue00b\ue002\ue003\ue004\ue005\ue00c \ue013 \ue00f\ue009\ue003\ue006\ue00b\ue003 \ue015\ue00b\ue008\ue00d\ue007\ue00b\ue009\ue005\ue007\ue002\ue00f\ue010 \ue002\ue00b\ue002\ue00d\ue00c \ue013\ue00c \ue002\ue008\ue007\ue013\ue00f\ue009\ue008\ue00f \ue002\ue009\ue00b\ue003\ue015\ue00b\ue007\ue00c\ue002 \ue00d\ue00b\ue017\ue007\ue01e\ue00f \ue002\ue007 \ue016 Fea tu res of i nstr umen ts to suppo r t the dev e lopm ent o f LI i on ba tteri es 1 Suitable f or rapid specimen a verage composition anal ysis just a few minute s to obt ain a result, including sampling and mea surem ent). Me asure ment s are pos sible for bot h vaccum and atm osphe re. Fluid samples as well as s olid samples c an be use d. Can be u sed fo r scre ening of transition m et als, such as Fe, Co, and Ni: for cath ode mate rials. Li is obs er vable, An id eal sys tem fo r chemical b onding st ate analysis of the sample sur face. Ch emical st ate analysis of th e elec tro de inter f ace is pos sible \ue012\ue009\ue00f\ue006\ue011\ue00b\ue01f\ue007\ue005\ue008 \ue00d\ue00b\ue021\ue013 \ue003\ue010\ue014\ue007\ue016\ue00b \ue022\ue00f\ue00b \ue00f\ue009\ue00b \ue003\ue01a\ue009 \ue007\ue013 \ue01e\ue00c\ue01a\ue014\ue007\ue016\ue00b \ue01f\ue007\ue005\ue008 \ue00d\ue00b \ue005\ue013\ue003\ue010\ue014\ue00f\ue006\ue011\ue00b \ue00c\ue006\ue017\ue00b chemic al bonding st ate analysis as well as sur face analysis for micro ar ea is po ssible. Secon dary e lectro n im ag es and back scat t ere d elec tron image s make it possible to o bse r ve the sur face mor p h olo g y . High res olution mo rpholo gy o bse r vations of t he sur face, including struc tural analysis of materials at a nano -level with low accelerat ing voltages. Available at tachme nts include EDS and W DS, enabling element analysis. EDS Energy dispersive X-ray spectrometer EELS Electron Energy Loss spectrometer WDS W avelength Dispersive X-ray spectrometer \ue002\ue003\ue004\ue005\ue006\ue007\ue004\ue008\ue009\ue00a\ue00b\ue003 Function to perform analysis while etching the surface with Ar ion Multi- channel WDS allows micro are a element analysis with a high ene rg y resolution . Secon dary e lectron im ag es an d ba cksca ttered e lectron im ages make it possible to o bse rve t he sur face mo rph olog y . Fea tu res of i nstr umen ts to suppo r t the dev e lopm ent o f LI i on ba tteri es 2 *1 epend on the system *2 When the optional analyzing crystal for Be is installed *3 Differs depending on the specimen and conditions *4 V aries according to the conditions of use For details, refer to the catalogs and data sheets for each instrument Instrument Environment Excitation Main detected Sample Resolution Analysis Detectable Energy Detection * 3 source signals formats guideline depth element range resolution concentration limit XRF V acuum X-ray Fluorescent Bulk 1 12 mm 1 mm* 3 Na to U About 150 eV Several ppm Normal atmosphere X-ray Fluids (analysis area) (Mn K ) or more XPS V acuum X-ray Photoelectron Bulk 30 µm to a few mm 6 nm Li to U About 0.1 eV About 0.1 % (analysis area) or more Secondary electron T ens of 10 ppm EPMA V acuum Electron Backscattered electron Bulk 0.1 1 µm* 1 1 µm Be to U* 2 About 10 eV or more beam Characteristic X-ray AES V acuum Electron Auger electron Bulk 3 nm (Secondary electron) 6 nm Li to U About 0.1 eV About 0.1 % beam Secondary electron 8 nm (Auger electron) or more Secondary electron B to U About 130 eV About 0.1 % or more SEM V acuum Electron Backscattered electron Bulk 1.2 nm * 1 1 µm B to U About 10 eV T ens of 10 ppm or more beam Characteristic X-ray B to U About 130 eV About 0.1 % or more TEM V acuum Electr on T ransmission electron \ue002\ue003\ue004\ue005\ue006\ue007\ue008\ue009 0.1 nm * 1 100 nm H to U 1.0 eV (Schottky) * 4 About 0.1 % or more beam Characteristic X-ray (sample thickness) 0.50 eV (Cold-FEG) * 4 3 LIB note XRF X-ray Fl uoresce nce Spe ct romete r XPS X-ra y Photoelectron Spec trometer EPM A Electr on Probe Micro Analyzer AES Au ger E l ectron Spectro meter SEM Scanning Electr on Microscop e TEM T ransmi ssion El ec tron Microsc ope Of f er s st ruc tu ral analysis at at omic re solutio n , element analysis with EDS, and \ue002\ue00d\ue007\ue004\ue00f\ue002\ue00c\ue014\ue00b \ue009 \ue008\ue00c\ue008\ue007\ue00b \ue00c\ue006\ue00c\ue014\ue023\ue009\ue00f\ue009\ue00b \ue012\ue009\ue00f\ue006\ue011\ue00b \ue024\ue024\ue022\ue025\ue00b \ue027\ue00c\ue00b \ue008\ue00d\ue00f\ue006\ue00b \ue010\ue014\ue004\ue00b \ue009\ue005\ue007 \ue002\ue00f\ue004\ue007\ue006\ue00b \ue00f\ue009\ue00b \ue013\ue007\ue01c \ue012\ue00f\ue013\ue007\ue017\ue02a\ue00b \ue02b \ue00c\ue006\ue00b direc tly d ete ct Li wit h EELS Element analysis function 1 Morphology Observation & Surface Analysis Instruments 1-2 Energy Dispersive X-ray Fluorescence Spectrometer (XRF) \ue019\ue00d\ue007\ue00b \ue030\ue033\ue013 \ue00c\ue023\ue00b \ue018 \ue012\ue003\ue013\ue007\ue009\ue002\ue007\ue006\ue002\ue007\ue00b \ue009\ue005\ue007\ue002\ue008\ue013\ue003\ue004\ue007\ue008\ue007\ue013\ue00b \ue00f\ue009\ue00b \ue00c\ue006\ue00b \ue00f \ue006\ue009\ue008\ue013\ue012\ue004\ue007\ue006 \ue008\ue00b \ue015\ue003\ue013\ue00b \ue00c\ue006 \ue00c\ue014 \ue023\ue034 \ue00f\ue006 \ue011\ue00b \ue008\ue00d\ue007\ue00b \ue008\ue023 \ue005\ue007\ue009\ue00b \ue00c\ue006\ue017\ue00b \ue002\ue003\ue006\ue002\ue007 \ue006\ue008\ue013\ue00c\ue008\ue00f \ue003\ue006\ue009\ue00b \ue003\ue015\ue00b \ue007 \ue014\ue007\ue004\ue007\ue006\ue008\ue009\ue00b \ue00f\ue006\ue00b\ue00c\ue00b\ue009\ue00c \ue004\ue005\ue014 \ue007\ue00b\ue01a\ue023\ue00b\ue00f \ue013\ue013\ue00c \ue017\ue00f \ue00c \ue008\ue00f\ue006 \ue011\ue00b\ue008\ue00d\ue007\ue00b\ue009\ue00c\ue004\ue005 \ue014\ue007\ue00b\ue00e\ue00f \ue008\ue00d\ue00b\ue030\ue033\ue013 \ue00c \ue023\ue00b\ue00c\ue006\ue017\ue00b\ue004\ue007\ue00c\ue009\ue012 \ue013\ue00f \ue006\ue011\ue00b\ue008\ue00d\ue007\ue00b\ue007\ue004 \ue00f\ue008\ue008\ue007\ue017\ue00b\ue018\ue012\ue003\ue013\ue007\ue009\ue002\ue007\ue006\ue008\ue00b\ue030 \ue033\ue013\ue00c \ue023\ue009 \ue016\ue00b\ue035\ue008\ue00b\ue00f\ue009\ue00b\ue004 \ue00c\ue00f \ue006 \ue014 \ue023\ue00b\ue012\ue009\ue007\ue017\ue00b for app l ica tion s l ik e assess i ng gra des of steel , contro l l in g product qu al i t y , and R oHS comp l ia nce ( Cd, Pb , H g, \ue02b \ue013 \ue00a \ue00b\ue036 \ue013 \ue00b\ue002 \ue003 \ue006 \ue008 \ue007 \ue006 \ue008 \ue02a \ue016 \ue00b\ue019 \ue00d \ue00f \ue009 \ue00b\ue00f \ue006 \ue009 \ue008 \ue013 \ue012 \ue004 \ue007 \ue006 \ue008 \ue00b\ue009 \ue012 \ue005 \ue005 \ue003 \ue013\ue008 \ue009 \ue00b\ue013 \ue00c \ue005 \ue00f \ue017 \ue00b\ue00c \ue006 \ue00c \ue014 \ue023 \ue009 \ue00f \ue009 \ue00a \ue00b\ue00e \ue00f \ue008 \ue00d \ue00b\ue00c \ue006 \ue00b\ue007 \ue01b \ue008 \ue013 \ue007 \ue004 \ue007 \ue014 \ue023 \ue00b\ue009 \ue00d \ue003 \ue013 \ue008 \ue00b\ue008 \ue00f \ue004 \ue007 \ue00b\ue013 \ue007\ue01c \ue012 \ue00f \ue013 \ue007\ue017 \ue00b\ue015 \ue013 \ue003 \ue004 \ue00b\ue009 \ue005\ue007 \ue002 \ue00f \ue004 \ue007 \ue006 \ue00b prepar ati on un ti l a resul t is ob tai ned. Features Ana lys is e lements: N a to U Ana lys is regi on : 1 to 1 2 mm Specimen f orm: so l id, po wder , li qui d Non-destru ctiv e an a ly s is Detec tion l ower l i mi t: from severa l ppm Element Analyzer T ablets ar e formed of a powder material that is used for lithium ion batteries, and 30 second measurements ar e made, providing r esults that allow quantitative analysis of the element composition. The results shown her e indicate that the specimen is composed of the expected mixture of Mn : CO : Ni in a 1 : 1 : 1 ratio. [ Measurement conditions ] T ube voltage : 50 kV Collimator : 1.0 mm Atmosphere : Air Measurement time : 30 s Exc ellen t for el ement an aly sis of t r ace met als! LIB note 4 Component Mass % Atomic % Mn 1 6. 1 7 .3 Co 1 6.9 7 . 1 Ni 1 6.4 7 .0 Balance 50.6 78.6 \ue00a\ue00b\ue00c\ue005\ue00d\ue004\ue007\ue00e\ue00c\ue00d\ue004\ue00f\ue005\ue006\ue010\ue011\ue012\ue00b\ue008\ue00d\ue006 Mn : Co : Ni = 1 : 1 : 1 Li Mn Co Ni O x Analys is exa m p l e Positiv e elec trode mater ial analysis ( t ablet of a po wder sample ) 1 Morphology Observation & Surface Analysis Instruments \ue00c\ue00d\ue00e\ue00d\ue009\ue00f\ue007\ue010\ue011\ue005\ue005\ue003\ue008\ue012\ue007\ue013\ue011\ue005\ue006\ue009\ue014\ue003\ue007\ue004\ue006\ue009\ue005\ue009\ue007\ue003\ue00b\ue003\ue013\ue005\ue008\ue009\ue00f\ue007\ue00d\ue015\ue011\ue016\ue003\ue007\ue017\ue00b\ue003\ue018\ue005\ue019 The stage scanning method makes it possible to acquire wide images of up to 50 mm x 18 mm. Performing photoelectron imaging is useful for identifying locations with differ ent wettability due to differ ences in the chemical bonding state or sample contamination that cannot be determined from optical information. \ue01a\ue014\ue003\ue00f\ue005\ue00d\ue00a\ue013\ue011\ue005\ue00d\ue009\ue00f\ue007\ue009\ue018\ue007\ue010\ue009\ue00f\ue014\ue00d\ue00f\ue016\ue007\ue01b\ue005\ue011\ue005\ue003\ue007\ue010\ue011\ue01b\ue003\ue014\ue007\ue009\ue00f\ue007\ue004\ue003\ue011\ue01c\ue007\ue004\ue009\ue01b\ue00d\ue005\ue00d\ue009\ue00f\ue007\ue014\ue00d\ue01d\ue003\ue008\ue003\ue00f\ue013\ue003\ue01b Since peak position differ ences occure due to variations in the chemical bonding state, it is possible to identify the chemical bonding state of the Li by interpreting the peak positions. Chemical bonding state Li1s Li 52.6 eV Li 2 O 53.5 eV Li 2 CO 3 54.6 eV Li 3 PO 4 55.5 eV Li 3 PO 4 Li 2 CO 3 Li 2 O \ue00c\ue00d\ue01e\ue01b Li 2mm Metallic lithium Standard sample Analys is exa m p l e Photoelectron image, Analysis of chemi cal bonding s tate 5 LIB note 1-3 X-ray Photoelectron Spectrometer (XPS) \ue025 \ue00f \ue006 \ue002 \ue007 \ue00b\ue017 \ue00f \ue013 \ue007 \ue002 \ue008 \ue00b\ue003 \ue01a \ue009 \ue007 \ue013 \ue01e \ue00c \ue008 \ue00f \ue003 \ue006 \ue00b\ue003 \ue015 \ue00b\ue008 \ue00d \ue007 \ue00b\ue005 \ue00d \ue003 \ue008 \ue003 \ue007 \ue014 \ue007 \ue002 \ue008 \ue013 \ue003 \ue006 \ue009 \ue00b\ue007 \ue01b \ue002 \ue00f \ue008 \ue007 \ue017 \ue00b\ue01a \ue023 \ue00b\ue008 \ue00d \ue007 \ue00b\ue030 \ue033 \ue013 \ue00c \ue023 \ue00b\ue00f \ue009 \ue00b\ue005 \ue007 \ue013 \ue015 \ue003 \ue013 \ue004 \ue007 \ue017 \ue00a \ue00b\ue030 \ue021 \ue025 \ue00b\ue00d \ue00c \ue009 \ue00b\ue008 \ue00d \ue007 \ue00b\ue00c \ue017 \ue01e \ue00c \ue006 \ue008 \ue00c \ue011 \ue007 \ue00b of bei ng able t o ana lyz e surface-sens itiv e sol ids w ith hi gh energ y resol ution. As a resu lt, for L IB an al yses, it is poss ible t o detec t Li , a ke y component, and t o ana lyze the c hemi cal bond in g st ate . Fu r t hermore, depth \ue005\ue013\ue003\ue010 \ue014 \ue00f\ue006 \ue011\ue00b\ue007\ue006\ue00c\ue01a \ue014\ue007\ue009\ue00b\ue00c\ue006\ue00c \ue014\ue023\ue009 \ue00f\ue009\ue00b\ue003\ue015\ue00b\ue006\ue003\ue008\ue00b\ue003\ue006 \ue014\ue023\ue00b\ue008\ue00d\ue007\ue00b\ue009\ue012\ue013 \ue015\ue00c\ue002\ue007 \ue00a\ue00b\ue01a\ue012\ue008\ue00b\ue00c\ue014 \ue009\ue003\ue00b\ue008\ue00d\ue007\ue00b\ue013\ue007\ue011\ue00f\ue003\ue006\ue009\ue00b\ue00f \ue006\ue009\ue00f \ue017 \ue007\ue00b\ue008\ue00d\ue007\ue00b\ue009\ue00c\ue004\ue005 \ue014\ue007\ue016 Features Ana lys is elements: L i to U Surface ana lys is i nstrument ( detec tion depth of about 6 nm ) Chem ical bond ing state an alys is Detec table el ement s from Li to U Detec tion l ower l im it of about 0. 1 % \ue00b\ue025\ue012\ue005\ue005\ue003\ue013 \ue008 \ue009\ue00b\ue017\ue007\ue005\ue008 \ue00d\ue00b\ue005\ue013\ue003\ue010\ue014 \ue00f\ue006\ue011 Direct det ection of Li ! JPS-9200 Li C 1 Morphology Observation & Surface Analysis Instruments \ue01f\ue021\ue011\ue015\ue004\ue00b\ue003\ue007\ue009\ue018\ue007\ue014\ue003\ue004\ue005\ue006\ue007\ue004\ue008\ue009\ue00a\ue00b\ue003\ue007\ue011\ue00f\ue011\ue00b\ue012\ue01b\ue00d\ue01b\ue007\ue009\ue018\ue007\ue004\ue009\ue01b\ue00d\ue005\ue00d\ue022\ue003\ue007\ue003\ue00b\ue003\ue013\ue005\ue008 \ue009\ue014\ue003\ue007\ue015\ue011\ue005\ue003\ue008\ue00d\ue011\ue00b The image on the left is a powder of the raw material for a lithium-ion battery positive electrode that has been formed \ue004\ue005\ue00d\ue00f\ue006\ue00c\ue006 \ue00d\ue00c\ue013\ue008\ue011\ue00d\ue014\ue006 \ue015\ue003\ue011\ue005\ue006 \ue016\ue011\ue017\ue00d\ue003\ue006 \ue017\ue010\ue00f\ue007\ue008\ue004\ue005\ue018\ue006 \ue004\ue012\ue006 \ue017\ue011\ue010\ue019\ue00f\ue010\ue009\ue011\ue016\ue01a\ue006 \ue004\ue00d\ue006 \ue004\ue012\ue006 \ue00f\ue013\ue012\ue011\ue010\ue01b\ue011\ue016\ue006 \ue00d\ue003\ue00c\ue00d\ue006 \ue00d\ue003\ue011\ue006 \ue01c\ue004\ue006 \ue004\ue012\ue006 \ue012\ue011\ue018\ue010\ue011\ue018\ue00c\ue00d\ue011\ue016\ue006\ue004\ue005\ue006 \ue00c\ue006 \ue010\ue011\ue018\ue004\ue00f\ue005\ue006\ue00f\ue019\ue006 \ue00c\ue013\ue00f\ue00b\ue00d\ue006 \ue01d\ue01e\ue006 \ue005\ue009\ue006 \ue00f\ue005\ue006 \ue00d\ue003\ue011\ue006 surface, as shown in the graph on the right. Analysis region 1 mm Li Li Co Co CoO Co 3 O 4 Co Co F O C P Mn Ni Measured data Co oxides standard spectrum LIB note 6 Analys is exa m p l e \ue002\ue003\ue004\ue005\ue006\ue007\ue004\ue008\ue009\ue00a\ue00b\ue003\ue007\ue00c\ue00d\ue00c\ue00b \ue00e\ue00f\ue010\ue00f\ue007\ue009\ue011\ue007\ue00d\ue003\ue012\ue00c \ue005\ue010\ue013\ue003\ue007\ue003\ue00b\ue003\ue014\ue005\ue008\ue009 \ue015\ue003\ue007\ue016\ue00c\ue005\ue003\ue008 \ue010\ue00c\ue00b\ue007\ue00c\ue011\ue005\ue003\ue008\ue007\ue014\ue006\ue00c\ue008\ue012\ue003\ue017 \ue015\ue010\ue00f\ue014\ue006\ue00c\ue008\ue012\ue003 \ue023\ue00f\ue011\ue00b\ue012\ue01b\ue00d\ue01b\ue007\ue009\ue018\ue007\ue00f\ue003\ue016\ue011\ue005\ue00d\ue022\ue003\ue007\ue003\ue00b\ue003\ue013\ue005\ue008\ue009\ue014\ue003\ue007\ue015\ue011\ue005\ue003\ue008\ue00d\ue011\ue00b\ue007\ue011\ue018\ue005\ue003\ue008\ue007\ue013\ue006\ue011\ue008 \ue016\ue00d\ue00f\ue016\ue024\ue014\ue00d\ue01b\ue013\ue006\ue011\ue008\ue016\ue003\ue007\ue013\ue012\ue013\ue00b\ue003 The graph below shows the qualitative analysis results for the negative electr ode material. Li is detected. There is also Co detected, which was not present in the negative electr ode originally . Comparing the spectrum of the Co in the negative electrode material (below left) with the standar d sample spectra of simple Co and Co oxides (below right) clearly shows that the Co in the negative electrode material exists in a metallic state. It can be inferred that the Co in the positive electr ode has ionized, migrated to the negative electrode, and precipitated as metallic Co. 1 Morphology Observation & Surface Analysis Instruments Incident electron beam Analyzing crystal Rowland circle Sample Detector Characteristic X-ray Au coating Au coating Intrinsic region measurement system -1000V N layer Electron Hole P layer Comparison of W DS and EDS The detection principles and structures for WDS \ue00c\ue005\ue016\ue006 \ue01f\ue021\ue022\ue006 \ue016\ue004\ue019\ue019\ue011\ue010\ue006 \ue012\ue004\ue018\ue005\ue004\ue007\ue00e\ue00c\ue005\ue00d\ue008\ue023 \ue014\ue006 \ue024\ue005\ue006 \ue00e\ue00f\ue009\ue017\ue00c\ue010\ue004\ue012\ue00f\ue005\ue006 \ue00d\ue00f\ue006 \ue01f\ue021\ue022\ue006 (lower left), which simultaneously detects all the characteristic X-rays that are generated, WDS only detects the characteristic X-ray of the target detection element. \ue002\ue003\ue011\ue006 \ue007\ue018\ue00b\ue010\ue011\ue006 \ue00f\ue005\ue006 \ue00d\ue003\ue011\ue006 \ue00c\ue013\ue00f\ue01b\ue011\ue006 \ue010\ue004\ue018\ue003\ue00d\ue006 \ue012\ue003\ue00f\ue027\ue012\ue006 \ue00c\ue006 \ue00e\ue00f\ue009\ue017\ue00c\ue010\ue004\ue012\ue00f\ue005\ue006 of the EDS and WDS analyses of SI oxides and T a \ue00f\ue02b\ue004\ue016\ue011\ue012\ue006 \ue004\ue005\ue006 \ue009\ue00b\ue008\ue00d\ue004\ue03b\ue008\ue00c\ue023\ue011\ue010\ue006 \ue007\ue008\ue009\ue012\ue014\ue006 \ue002\ue003\ue011\ue006 \ue022\ue004\ue006 \ue00c\ue005\ue016\ue006 \ue002 \ue00c\ue006 \ue017\ue011\ue00c\ue03c\ue012\ue006 \ue00c\ue010\ue011\ue006 overlapped in the EDS spectrum, but are separated in the WDS spectrum, demonstrating the high energy resolution attainable with WDS. Features \ue047 \ue00c\ue01e\ue007 \ue014\ue007\ue006\ue011\ue008\ue00d\ue00b\ue017\ue00f\ue009\ue005\ue007\ue013\ue009\ue00f \ue01e\ue007\ue00b\ue009\ue005\ue007\ue002 \ue008\ue013\ue003\ue004\ue007 \ue008\ue007\ue013\ue00b\ue027 \ue047\ue01f\ue025\ue02a\ue00a\ue00b\ue04b\ue00c\ue01b\ue016\ue00b\ue051 \ue002\ue00d Ana lys is elements: ( Be) B to U Ana lys is region : s ever al µm to sev eral c m Ana lys is depth: up to about 1 µm Detec tion l ower l im it: severa l 1 0 ppm WDS ( W aveleng t h dis pe rsive X-ray s pe c t ro me ter ) WDS-EDS spectra comparison EDS ( Energy dispersiv e X-ra y spe ctrome ter X-ray energy (keV) X-ray intensity a.u. WDS principles EDS principles 7 LIB note JXA-8530F 1-4 Electron Probe Micro Analyzer (EPMA) \ue024 \ue021 \ue04b \ue056 \ue00b\ue012 \ue009 \ue00f \ue006 \ue011 \ue00b\ue00c \ue006 \ue00b\ue007 \ue014 \ue007 \ue002 \ue008 \ue013 \ue003 \ue006 \ue00b\ue01a \ue007 \ue00c \ue004 \ue00b\ue00c \ue009 \ue00b\ue008 \ue00d \ue007 \ue00b\ue007 \ue01b \ue002 \ue00f \ue008 \ue00c \ue008 \ue00f \ue003 \ue006 \ue00b\ue009 \ue003 \ue012 \ue013 \ue002 \ue007 \ue00b\ue00f \ue009 \ue00b\ue007 \ue01c \ue012 \ue00f \ue005 \ue005 \ue007 \ue017 \ue00b\ue00e \ue00f \ue008 \ue00d \ue00b\ue012 \ue005 \ue00b\ue008 \ue003 \ue00b\ue051 \ue00b\ue002 \ue00d \ue00c \ue006 \ue006 \ue007 \ue014 \ue009 \ue00b\ue003 \ue015 \ue00b\ue047 \ue01f \ue025 \ue00a \ue00b\ue00c \ue006 \ue017 \ue00b\ue00f \ue009 \ue00b capabl e of elementa l ana lys is of m icro a reas with a h igh energy resoluti on. I n add itio n, the SEM fu nction al it y \ue00f\ue009\ue00b\ue007 \ue01b \ue002\ue007\ue014 \ue014\ue007\ue006\ue008\ue00a\ue00b\ue004\ue00c \ue059\ue00f\ue006\ue011\ue00b\ue00f \ue008\ue00b\ue005 \ue003\ue009\ue009 \ue00f\ue01a \ue014\ue007\ue00b\ue008\ue003\ue00b\ue005\ue007\ue013\ue015\ue003\ue013\ue004\ue00b\ue01a\ue003\ue008\ue00d\ue00b\ue00c\ue006 \ue00c\ue014 \ue023\ue009\ue00f \ue009\ue00b\ue002\ue003\ue004\ue01a\ue00f \ue006\ue007\ue017\ue00b\ue00e\ue00f\ue008\ue00d\ue00b\ue009\ue012\ue013\ue015\ue00c\ue002\ue007\ue00b\ue004\ue003\ue013\ue005\ue00d\ue003\ue014 \ue003\ue011 \ue023\ue00b\ue003\ue01a\ue009\ue007\ue013 \ue01e\ue00c\ue008\ue00f \ue003\ue006\ue009\ue00b\ue012\ue009\ue00f \ue006\ue011\ue00b secondary electron i mag es and bac k scattere d el ec tron i mag e s. 1 Morphology Observation & Surface Analysis Instruments The spectra shown below on the right are the r esults of qualitative analysis for Co and F contained in a positive electrode material after a charge/discharge cycle. The EDS result has a low energy r esolution and a high background level, and the F-K \ue006 \ue008\ue004\ue005\ue011\ue006 \ue004\ue012\ue006 \ue004\ue005\ue03e\ue00b\ue011\ue005\ue00e\ue011\ue016\ue006 \ue013\ue023\ue006 \ue00d\ue003\ue011\ue006 \ue03f\ue00f\ue01a\ue006 \ue012\ue00f\ue006 \ue00d\ue003\ue011\ue006 \ue017\ue011\ue00c\ue03c\ue006 \ue004\ue012\ue006 \ue016\ue004\ue019\ue007\ue00e\ue00b\ue008\ue00d\ue006 \ue00d\ue00f\ue006 \ue016\ue011\ue00d\ue011\ue00e\ue00d\ue014\ue006 \ue015\ue004\ue00d\ue003\ue006 \ue015\ue021\ue022\ue01a\ue006 \ue00d\ue003\ue011\ue010\ue011\ue006 \ue004\ue012\ue006 \ue005\ue00f\ue006 \ue03f\ue00f\ue03b\ue01c line effect, and the F-K line can be detected. The images on the right show an example of element mapping with WDS for a cross section of Li-ion battery positive electrode material through r epeated charge/discharge cycles. The signal intensity of the F and C that have migrated from the collector (Al) in the center portion increases. The profile in the element mapping is obtained by averaging the signal intensity in the longitudinal direction. What should have originally been a uniform distribution of the elements is now shown to be biased, which is considered to be one of the factors in the deterioration of battery performance. A feature of EPMA is the ability to confirm minute changes in the element distribution. The analysis area is 180 µm × 180 µm. Positive electrode materials Negative electrode materials Separator Positive electrode materials LiCoO 2 LiMn 2 O 4 LiFePO 4 , etc. Negative electrode materials C Si SnO 2 , etc. Electrolyte LiPF 6 , LiClO 4 , etc. X-ray energy (keV) X-ray intensity (a.u.) LIB note 8 \ue002\ue003\ue004\ue005 \ue002\ue003\ue004\ue005 \ue002\ue003\ue004\ue005 \ue002\ue003\ue004\ue005 C Composition image Co F Analys is exa m p l e Qualitativ e analysis o f positive electrode mater ials, Wide region analysis 1 Morphology Observation & Surface Analysis Instruments Li se nsit ivity Because the JAMP-9510F uses a concentric hemispherical electrostatic analyzer , it is possible to obtain peaks even in \ue008\ue00f\ue027\ue006 \ue011\ue005\ue011\ue010\ue018\ue023\ue006 \ue010\ue011\ue018\ue004\ue00f\ue005\ue012\ue01a\ue006\ue012\ue00b\ue00e\ue003\ue006 \ue00c\ue012\ue006 \ue00d\ue003\ue00f\ue012\ue011\ue006 \ue00f\ue019\ue006 \ue01c\ue004\ue01a\ue006 \ue027\ue004\ue00d\ue003\ue006 \ue003\ue004\ue018\ue003\ue006 \ue017\ue010\ue011\ue00e\ue004\ue012\ue004\ue00f\ue005\ue01a\ue006 \ue003\ue004\ue018\ue003\ue006 \ue012\ue011\ue005\ue012\ue004\ue00d\ue004\ue01b\ue004\ue00d\ue023\ue006 \ue00c\ue005\ue016\ue006 \ue003\ue004\ue018\ue003\ue006 \ue011\ue005\ue011\ue010\ue018\ue023\ue006 \ue010\ue011\ue012\ue00f\ue008\ue00b\ue00d\ue004\ue00f\ue005\ue014\ue006 \ue002\ue003\ue011\ue006 \ue007\ue018\ue00b\ue010 \ue011\ue006 \ue00f\ue005\ue006 \ue00d\ue003\ue011\ue006 right below shows the results of measur ements with the JAMP-9510F for standard samples of Li, Li 2 O, and Li 2 CO 3 . This clearly illustrates the changes in the peak position and shape for each of the differ ent chemical bonding states. 1-5 Auger Electron Spectrometer (AES) \ue056 \ue012 \ue011 \ue007 \ue013 \ue00b\ue007 \ue014 \ue007 \ue002 \ue008 \ue013 \ue003 \ue006 \ue00b\ue009 \ue005 \ue007 \ue002 \ue008 \ue013 \ue003 \ue009 \ue002 \ue003 \ue005 \ue023 \ue00a \ue00b\ue014 \ue00f \ue059 \ue007 \ue00b\ue030 \ue021 \ue025 \ue00a \ue00b\ue00c \ue013 \ue007 \ue00b\ue003 \ue006 \ue007 \ue00b\ue00e \ue00c \ue023 \ue00b\ue008 \ue003 \ue00b\ue017 \ue00f \ue013 \ue007 \ue002 \ue008 \ue014 \ue023 \ue00b\ue017 \ue007 \ue008 \ue007 \ue002 \ue008 \ue00b\ue022 \ue00f \ue016 \ue00b\ue05a \ue003 \ue013 \ue00b\ue056 \ue012 \ue011 \ue007 \ue013 \ue00b\ue007 \ue014 \ue007 \ue002 \ue008 \ue013 \ue003 \ue006 \ue00b\ue007 \ue01b \ue002 \ue00f \ue008 \ue00c \ue008 \ue00f \ue003 \ue006 \ue00b\ue00c \ue006 \ue00b \ue007\ue014 \ue007\ue002 \ue008\ue013\ue003\ue006\ue00b\ue01a\ue007\ue00c\ue004\ue00b\ue00f \ue009\ue00b\ue012\ue009\ue007\ue017\ue00b\ue00c\ue009\ue00b\ue008\ue00d\ue007\ue00b\ue007\ue01b \ue002\ue00f \ue008\ue00c\ue008\ue00f \ue003\ue006\ue00b\ue009\ue003\ue012\ue013\ue002 \ue007\ue00a\ue00b\ue005\ue013\ue003 \ue01e\ue00f\ue017 \ue00f\ue006\ue011\ue00b\ue00c\ue00b\ue00d \ue00f\ue011 \ue00d\ue00b\ue009\ue005\ue00c \ue008\ue00f \ue00c\ue014\ue00b\ue013\ue007\ue009\ue003\ue014 \ue012\ue008\ue00f\ue003 \ue006\ue016\ue00b\ue019\ue00d\ue007\ue00b\ue022 \ue00f\ue00b\ue017\ue00f\ue009\ue008\ue013 \ue00f\ue01a\ue012\ue008\ue00f \ue003\ue006\ue00b\ue00f\ue006\ue00b\ue007 \ue01e\ue007 \ue006\ue00b\ue00c\ue00b si ngl e partic le of pos itive e lectrode materi al can be ob tai ned. Features Hi gh spatia l re soluti on of Auger an al ysi s: 8 nm V ari able energy resolution : From 0 .05 % to 0 .6 % Ana lys is rang e: U p to 95 m m with the l arge stag e Insu lati ng mater ia ls can be ana lyzed us ing the neutral izi ng gun and sampl e til ting method Wide ra nge of option s (BE I, EB SD etc. ) \ue01f\ue007\ue005\ue008\ue00d\ue00b\ue005\ue013\ue003\ue010\ue014 \ue00f\ue006 \ue011 \ue023\ue025\ue016\ue003\ue008\ue007\ue015\ue011\ue004\ue007\ue009\ue018\ue007\ue00c\ue00d\ue007\ue026\ue00d\ue005\ue006\ue00d\ue00f\ue007\ue005\ue006\ue003\ue007\ue004\ue009\ue01b\ue00d\ue005\ue00d\ue022\ue003\ue007\ue003\ue00b\ue003\ue013\ue005\ue008\ue009\ue014\ue003\ue007\ue015\ue011\ue005\ue003\ue008\ue00d\ue011\ue00b\ue007\ue004\ue011\ue008\ue005\ue00d\ue013\ue00b\ue003\ue01b Since the Auger Electron Spectr ometer uses an electron beam as the excitation sour ce, it is possible to acquire element maps for micro ar eas corresponding to the secondary electr on images and backscattered electr on images. SEI Li 9 LIB note JAMP-9510F Li can be det ec ted di rectly !

lithium ion battery (everything you need to know)

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