Depth analysis for laminated film by confocal Raman mapping

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1 Newest modular 3D Imaging Raman Microspectroscopy System Simple operation and low cost with all the basic features of our top of the line system. Structural images of transparent samples (plastic, film, organic EL) with Raman and fluorescence spectroscopy. igh Performance, ompact Size, cost Features Raman imaging with 3 nm spatial resolution. igh sensitivity: 4th order Raman Si peak can be detected in less than 1 min. using a low intensity laser (4 mw) onfocal laser microscope designed for 3D Raman. ompact Raman optical system directly coupled to the microscope for high stability. No need adjustment because no moving parts. nm positional accuracy with piezo X-Y -Z stage. Modular optical system, spectrometer/d and laser. The simpler successor to the same powerful software. - using the 1. x improvement in spatial resolution using deconvolution software. Raman optical unit Fiber Fiber Laser SpectrometerD ompact and modular type Depth(m) 2 Poly lactic acid (PLA) film Adhesive Poly propylene (PP) film 1m 2 3 Depth profile of Plastic laminate film (This analysis is difficult by confocal laser microscope) i Normal part (Lio2) Degradation part (o 3 4 ) 3D Raman images of Lithium ion battery (using specific peak for each material) i i ead ffice Nishikasai Edogawa-ku, Tokyo Phone Fax

2 Finally, a high spatial resolution, high sensitivity, compact and low cost Raman microscopy system. Easy materials identifying with Raman The Nanofinder FLEX is a flexible 3D Raman microscope that retains the basic features and performance of our highend Nanofinder 3 system. Modular assemblies including a new compact Raman optical unit. The Raman optical unit is installed directly upon an upright microscope, creating a clean and compact installation taking no more bench space than a standard microscope. ther units are fiber optic coupled and can be placed in convenient locations for ease of operation and a space saving installation. Simple changeover of excitation laser and Raman optical system when required. ZnTe defect measurement Topographic measurement with confocal microscope mode Spectral window 6 nm Nanofinder FLEX has high special resolution < 3 nm and high sensitivity without complex optical adjustments. The system uses our highly acclaimed Nanofinder software with powerful imaging and data management capabilities. New, lower cost Raman unit and piezo stage are now in within the reach of most laboratory budgets. For further savings and flexibility, the Nanofinder FLEX system can be used with many existing lasers, D ameras, and spectrometers. Spectroscopic imaging of ZnTe with photoluminescence mode 3D mapping using the 6 nm Raman peak 2Dmapping measurement Spectral window Raman optical unit Spectrometer, D G-band m 1 m Raman spectrum of arbon nano tube 2D Raman image of NT (at G-band 193 cm -1 ) Measurement with high sensitivity Raman optical unit attached on microscope Si (3) 2 Si (4) Sample : Si wafer Exposure : 6 sec Laser : 32 nm Power : 4 mw (on the sample) bjective : x N.A. :.8 N2 ontrol-rack (Embedding P, spectrometer, D) Detection of 4th order Si Raman spectrum as demonstration of height sensitivity

3 Depth analysis for laminated film by confocal Raman mapping W e made a Raman mapping at a laminated area in depth direction. In confocal system, Spectral depth profile can be measured by moving focus position in Laminated film. Poly lactic acid Piezo-stage bjective lens Piezo stage move laser focus position. R 3 3 n Laser light Film 1 Laminated film Film 2 utline of measurement Poly propylene 3 n Structural formula of each film layers 4 i PLA film Poly lactic acid Adhesive Depth(m) 3 2 PP film Poly propylene 2 3 Spectral depth profile image Poly lactic acid adhesive Poly propylene Intensity profile for each materials (Specific peak) In spectral depth profile image, horizontal axis is Raman shift vertical axis is depth in laminated film. Various spectra were measured along depth direction. Raman spectra for each materials are shown below profile image. Right hand profiles in the profile image are intensity depth profiles for specific peak (orange color square). These 3 layers can be divided by this measurement. 2 3 Raman spectra for each materials

4 3D Raman image analysis on positive electrode suface of Li-Ion battery 3D Raman mapping on a positive electrode of a degradation Li-Ion battery were conducted. Distributions of normal electrode material (Lio2) and degradation material (o34) from it can be obsereved as raman images. Normal portion of the electrode (Lio2 ) Degradation portion of the electrode (o34) Raman intensity image of Lio2 peak (6 cm -1 ) Raman intensity image of o34 peak (7 cm -1 ) verlapped image from above images Typical Raman spectrum 3D Mapping conditions Excitation laser wavelength 32 nm Excitation laser power mw Exposure time 1 sec/point Total mapping time hours Mapping points 32x32x bjective lents x N.A..9 As a material for an positive electrode of Li-Ion battery, Lio2 is mainly used. The electrode material, however, degrades after repeating discharge and charge and then some porsions of it turn into o34, which can't contribute to charge. Material distributions on the surface can be observed with distinct peak intensity images, because different spectra are taken from these materials respectively. As shown in the upper images, there is a competely different pattern between normal Lio2 portion and degradation o34 portion.

5 Specifications FLEX 3D Raman microscope system System configuration -Upright microscope bjective lens (x, x) /Monitoring D -Raman optical unit (1 wavelength) -Imaging spectrometer -ooled D -Piezo stage (X-Y-Z) -Excitation laser (32 nm) -System controller, software / LD monitor verall specifications -Spatial resolution XY: < 3 nm (x, N.A..9) Z: < 9 nm (x, N.A..9) -Wavenumber range: cm -1 4 cm -1 (32 nm) -Wavenumber resolution: 2 cm -1 (f=3 cm imaging spectrometer) Each unit specifications -Raman optical unit Resettable filter unit Fiber connecting (incident and output) F connector coupling -Imaging spectrometer MS34i Focal length: 3 cm, F: 3.8 Reciprocal linear dispersion: 2.37 Wavelength resolution:.6 nm, 12G/mm Wavenumber resolution: 2 cm -1 nm, 12G/mm 4 gratings available (selectable) -ooled D detector Elements: 24 x 127 Element size: 26 x 26m ooling temperature:- (water), -8 (air) -Piezo stage X-Y-Z axis stroke: m (losed loop) Resolution: nm Repetition accuracy: nm -Excitation laser 1. LD pumped solid state laser Wavelength: 32 nm Power : mw 2. LD laser Wavelength: 78 nm Power : 7 mw ther lasers available -ontroller Software: Software for Nanofinder Main function: ontrol of spectrometer/piezo stage Measurement of Raman spectra and images orrelation of a spectral background 2D/3D data display Image restructure from 2D/3D data S: Windows(r) XP Professional -Size Microscope and Raman optical unit W3 x D4 x 77 mm Desk with 19 inch mount (option) W6 x D8 x 7 mm (Including as follows: spectrometer/d, laser, piezo/system controller) -Power supply VA-12A -ptions ompatibility with AFM for simultaneous AFM/Raman measurement