Approachable Raman Solutions The Shortest Path from Problem to Answer Michael S. Bradley The world leader in serving science
Thermo Scientific Raman Spectroscopy: Discover. Solve. Assure. Raman Spectroscopy Discovers Imaging provides a wide view of your sample High spatial resolution gives specific insights Polarization probes molecular alignment Raman Spectroscopy Solves Identify materials Probe beneath the surface (confocal) Raman Spectroscopy Assures Image entire pharmaceutical tablet for composition 2
The Thermo Scientific DXR2 Raman Spectrometers With the DXR2 Microscope you can: Point and Shoot with high spatial resolution Map regions for step-by-step data collection You cover a lot of ground with the DXR2xi Fast collection to build an image Intuitive, image based software Thermo Scientific DXR 2 Raman microscope Thermo Scientific DXR 2xi Raman imaging microscope 3
The Thermo Scientific DXR2 Family of Raman Spectrometers DXR2 System Basics: Lasers Grating Aperture Filter Sample 455 nm 532 nm 633 nm 785 nm Rayleigh rejection filter 50 cm -1 cut-off Laser Apertures Multichannel detector Slit Pinhole (confocal mode) Gratings Standard, 5 cm -1 High Resolution, 2 cm -1 Detectors CCD, EMCCD 2D G 50 4
Point-and-Shoot: Raman Through Evidence Bags Trace Evidence Fiber Identification Single Nomex Aramid Fiber in Evidence Bag Single Nomex Aramid Fiber on Glass Slide Single Kevlar Fiber in Evidence Bag Single Kevlar Fiber Glass Slide 1800 1600 1400 1200 1000 cm-1 Raman Shift (cm -1 ) 800 600 400 5
Point-and-Shoot: Explosive Materials Trace TNT Specimen TNT PETN C-4 Raman Shift (cm -1 ) 6
Imaging: Focus on the IMAGE Chemical Imaging provides visualizations of chemical differences The individual spectra are of secondary importance DXR2xi sets parameters, collects data and provides real-time visual interpretation at the IMAGE level It s better to work with an image than with thousands of spectra 7
Imaging: Get Only What You Need Optimize IMAGE collection, not individual spectra Entire image is collected in a single scan Experimental results are clear before image collection is complete You can interactively balance parameters on the fly Stop whenever the results are good enough Better! Better? 20 micron pixels 1900 spectra, 2 scans 1 minute 5 micron pixels 30,000 spectra, 2 scans 4 minutes 1 micron pixels 191,000 spectra, 2 scans 25 minutes 8
Surface Analysis of an Entire Painkiller Tablet: Wide Area Scan MCR Analysis Determine: Size of each domain Distribution of domains Overall composition of tablet Collection Parameters 11 11 mm surface area 532 nm laser, 10 objective 226,000 spectra, 25 µm pixel size Acquisition at 550 Hz (1.8 ms/spectrum) 8 minute collect time! Aspirin Acetaminophen Caffeine Titanium Dioxide 9
Very High Resolution MCR Analysis of Pharmaceuticals 225 250 µm surface area 532nm laser, 100 objective 229,000 spectra, 0.5 µm pixel size Acquisition parameters: 100 Hz (10 ms/spectrum) 38 Minute Collection Time Aspirin Microcrystalline Cellulose Acetaminophen Caffeine Starch Sodium Lauryl Sulfate 10
Confocal Raman Microscopy Strongest Raman signal from focused laser point Weak signal from out-of-focus regions of the sample Non-destructive depth analysis Dependent on aperture size and objective Depth selected by focusing z-axis of microscope stage Detector Aperture Objective Focus Plane Sample Lift sample stage 11
Confocal 3D Imaging: Waveguide in LiNbO 3 100X Optical overlaid with Raman image constructed as area of ν(oh) band at 3500 cm -1 Notations for Raman images orientation. 3D XY areas acquired at different Z depths 12
Label-Free Raman Image of Live U2OS Cells Raman images of major biomolecular components within a living U2OS cell Video Image DNA 784 cm -1 Proteins 1640-1664 cm -1 60x Water Immersion Objective MCR Lipids 2900 2950 cm -1 Image Pixel size 0.50 microns, 8300 spectra, 3 second collect, 2:26 hr 13
Location and Identification of Mineral Phases Septarian Nodule: A concretion of sedimentary rock where angular cavities and cracks have been filled in with other minerals Visual 5.0 x 3.4 mm 27200 spectra 25 µm image pixel size Exposure Time 0.02 s 100 scans Quartz Dolomite Carbon + Dolomite Carbon + Arakite Apatite 14
More Intensive Look in a Small Area Zoom In To Smaller Area 385 x 340 µm 5236 spectra 5.0 µm image pixel size Exposure Time 0.02 s 100 scans Pyrite Lazurite + Pyrite + Carbon Apatite + Carbon Carbon + Siderite Carbon 15
Raman Polarization Used to characterize: Symmetry Molecular orientation Crystallinity Morphological traits Depolarization Ratio I (VH) I ǁ (VV) n 3 n 1 Perpendicular Parallel n 4 n 2 16
Orientation of SWCNT on a Surface Developing high speed, low power semiconductors Aligned SWCNTs are semiconducting University of Wisconsin Dept. of Material Science and Engineering 17
Quality of Alignment of SWCNT Imaged area on next slide Laser polarization parallel to SWCNT axis Z(YY)Z Laser polarization perpendicular to SWCNT axis Z(XX)Z 18
Imaging the Alignment of SWCNT Laser polarization parallel to SWCNT axis Z(YY)Z Laser polarization perpendicular to SWCNT axis Z(XX)Z An orientation image created from the ratio of polarized Raman images provides a complete assessment of SWCNT alignment quality: 19
Multimodal Raman Spectroscopy The Thermo Scientific ixr Raman Spectrometer Uses DXR components Designed for integration with other analytical techniques 20
XPS-Raman Integration XPS-Raman with Thermo Scientific Theta Probe XPS Counts / s 1.20E+06 1.00E+06 8.00E+05 6.00E+05 4.00E+05 2.00E+05 0.00E+00 1300 1200 G Band 15 Scans, 8 m 30.4 s, 400µm, CAE 200.0, 1.00 ev Ag 3d C 1s 1100 Zn2p 1000 Ni 2p O 1s 900 800 700 600 500 400 Binding Energy (ev) Radial Breathing Modes 300 200 Si 2s 100 0 Name Atomic % C 76.0 O 16.8 Ag 4.9 Si 1.3 Zn 0.5 Ni 0.4 1D Band 2D Band 21
Rheo-Raman MARSXR Study of Polystearate in Hand Cream Combined Rheometry-Raman results Black dots: Intensity of the CH 2 twisting mode of polystearate Green Curve: G (storage modulus) Open Circles: The intensity of a non-polymer vibration 22
Phase Transition Study A polyethylene disc was analyzed during a temperature sweep from 100º to 155 ºC The Raman scatter was based on the CH 2 twist mode (1296 cm -1 ) The solid, transition and melt phases are highlighted in blue, green and yellow 23
Thermo Scientific Raman Spectroscopy Thermo Scientific DXR 2xi Raman imaging microscope Thermo Scientific DXR 2 Raman microscope Thermo Scientific DXR 2 SmartRaman Thermo Scientific FirstDefender RM Chemical Identification System and Thermo Scientific TruScan RM Handheld Analyzer Thermo Scientific Nicolet is 50 FT-IR Spectrometer with Raman Module Thermo Scientific Raman Analyzer Solutions 24
Serving Your Science 25
Thank You Please join me in the Materials Science Research section of our booth where I ll address comments and questions. 26