FIELD EMISSION SCANNING ELECTRON MICROSCOPY

Transcription

1 FIELD EMISSION SCANNING ELECTRON MICROSCOPY Make: Carl Zeiss, Germany Model: SUPRA 55VP, Gemini Column. With air lock system Detectors; 1, Secondary Electron 1 (In Lens) 2, Secondary Electron 2(SE2) 3, Backscattered Electron (BSE) 4, VPSE (Variable Pressure Mode) Energy Dispersive X-ray Analysis (Edx) Oxford Instruments X-MAX (20mm²) Resolution: 1.2 nm gold particle separation on a carbon substrate Magnification: From a min of 100x to > 5, 00,000 X Description SUPRA 55VP FE-SEM is a general purpose ultra high resolution FE-SEM based on the unique GEMINI Technology. It provided excellent imaging properties combined with analytical capabilities which make this high end FE-SEM suitable for a wide range of applications in materials science, life science and semiconductor technology. The large specimen chamber for the integration of optional detectors and accessories enables the user to configure the SUPRA for specific applications without sacrificing productivity or efficiency. Sample requirement sample should be in dried condition and it can be powder, film, pellet, coating etc..

2 NMR SPECTROMETER 500MHz Make: Bruker Model: AVANCE III HD Major Specifications/ Accessories available: 11.7 Tesla Magnet. a) 5mm BBO probe with gradient facilities and auto-sampler with VT facility. Tuning range from 109 Ag to P 31 also observation of 19 F with 1 H decoupling. b) 3,2mm CP/MAS probe with VT facility. Tuning range from 15 N to 31 P + 1 H + 19 H. Type of measurement/analysis available: 1D NMR, 2D NMR, Multi-nuclear NMR; Variable temperature measurements. Sample requirement for liquid samples: 5 mg for 1 H NMR and 50 mg for 13 C NMR experiment. Compounds should be highly pure and soluble in commonly available solvents. Solubility, nature of compound [carcinogenic, toxic, lachrymatory, explosive, hygroscopic] and Structural formula [contemplated / known] to be mentioned. The sample must be soluble in 0.6 ml of deuterated solvent. Facilities available for 1D NMR, 2D NMR, Multi-nuclear NMR; Variable temperature measurements. RADIOACTIVE MATERIAL should not be submitted. Sample requirement for solid samples: For Solid State NMR, 750 mg fine powder is required.

3 NMR SPECTROMETER 400MHz Make: Bruker Model: AVANCE III HD Major Specifications/ Accessories available: 9.4 T magnet. a)5mm BBO probe with gradient facility and auto sampler with VT facility. Tuning range from 109 Ag to P 31 also observation of 19 F with 1 H decoupling. b) 4mm CP/MAS probe with VT facility. Tuning range from 15 N to 31 P + 1 H. Type of measurement/analysis available: 1D NMR, 2D NMR, Multi-nuclear NMR; Variable temperature measurements. Sample requirement for liquid samples: 5 mg for 1 H NMR and 50 mg for 13 C NMR experiment. Compounds should be highly pure and soluble in commonly available solvents. Solubility, nature of compound [carcinogenic, toxic, lachrymatory, explosive, hygroscopic] and Structural formula [contemplated / known] to be mentioned. The sample must be soluble in 0.6 ml of deuterated solvent. Facilities available for 1D NMR, 2D NMR, Multi-nuclear NMR; Variable temperature measurements. RADIOACTIVE MATERIAL should not be submitted. Sample requirement for solid samples: For Solid State NMR, 750 mg fine powder is required.

4 ELECTRON PARAMAGNETIC RESONANCE (EPR) SPECTROSCOPY Make: BRUKER BIOSPIN, Germany Model: EMX Plus Source: Microwave X Band Operation mode: Powder, liquid and crystal samples at RT and down to 100 K Software: Bruker WIN EPR Acquisition, and Processing Applications: Physics : Susceptibility, semiconductors, Quantum dots, Defect centers Chemistry : Free radicals formation, ET reaction kinetics, Organo metallic, catalysis, molecular magnets, electrochemical studies Biology and spin labels : Enzyme reaction. ET reaction, folding & dynamics, metal centers, structural elucidation Material research : Polymers, glasses, superconductors, corrosion, fullerenes, carbon dating Medical research : In vivo free radical concentration and EPR imaging.

5 ELECTRON SPECTROSCOPY FOR CHEMICAL ANALYSIS (ESCA) OR X-RAY PHOTOELECTRON SPECTROSCOPY (XPS) Make: Thermo Scientific Model: ESCALAB 250XI BASE SYSTEM WITH UPS AND XPS IMAGE MAPPING Sources: XR6 Micro-focused Monochromator (Al Kα XPS) XR4 Twin Anode Mg/Al (300/400W) X-Ray Source. EX06 Ion gun Detector: Two types of detectors ensures optimum detection for each type of analysis- two dimensional detector for imaging and a detector based on channel electron multipliers for spectroscopy when high count rates are to be detected Salient Features: Twin anode non-monochromated XPS Large area XPS(LAXPS) Small area XPS (SAXPS) Fast Parallel Imaging(XPI) Energy Resolution Insulator analysis Depth profiling capability Angle resolved XPS Ion scattering spectroscopy(iss) UV Photoelectron Spectroscopy(UPS) E-Beam Evaporator REELS Facility Applications of ESCA 250 Xi: - ESCA is unique and non destructive tool to study the surfaces of the materials - The surfaces of a corroding sample can be analysed. - Contamination in the matrix of a catalyst can be analysed qualitatively and quantitatively - Inter faces (SEI in Li ion battery) of energy storage devises can be analysed qualitatively and quantitatively - Depth profiling which may give elemental composition as function of depth (1-2 µ) can be done Sample Requirements: - Solid Samples in the form of pellets of 6mm or 8mm diameter. - Thin films of area 10 mm2 Thickness 2 to 3 mm.

6 X-RAY PHOTOELECTRON SPECTROSCOPY (XPS) Make: Thermo Scientific Model: : MULTILAB 2000 Base system with X-Ray, Auger and ISS attachments. Sources: Twin Anode Mg/Al (300/400W) X-Ray Source. EX05 Ion gun for etching and ISS studies. Electron Gun with spot size < 50 m dia. Detector: -110 mm radius hemispherical analyzer with 7 channeltrons. - 4 variable analyzer slits viz 5, 2, 1 mm and 4mm. - Operates in CAE (Constant Analyser Energy) and CRR (Constant Retard Ratio) modes. Salient Features: - Sample heating and cooling stages in preparation and Analysis Chamber. - Sample manipulator with high precision four axes movement. - CCD camera and zoom microscope for optical viewing of the samples. Applications of MULTILAB 2000: - What elements and the quantity of those elements that are present within the top 1-12nm of the sample surface - What contamination, if any, exits on the surface or in the bulk of the sample - Empirical formula of a material that is free of excessive surface contamination - The chemical state identification of one or more of the elements in the sample - The binding energy of one or more electronic states - The thickness of one or more thin layers (1-8nm) of different materials within the top 12nm of the surfaces. Sample Requirements: - Solid Samples in the form of pellets of 6mm or 8mm diameter. - Thin films of area 10 mm2 and Thickness 2 to 3 mm.

7 TRANSMISSION ELECTRON MICROSCOPE (TEM) Make: FEI, The Netherlands Model: : Tecnai 20 G2 (FEI make) Resolution:: - Line-1.8 Å, Point-2.40 Å - Information limit (nm) Incorporated with STEM. - Bottom mount CCD Camera (Gatan-make) - TEM magnification range 25 x kx - TEM point resolution 0.27 nm - TEM line resolution (nm) TEM Holder: - Single tilt - Single tilt Low background - Double tilt - Double tilt Low background - STEM HAADF resolution 0.24 nm - STEM magnification range 150 x 230 Mx - EDS Detection: - Boron to higher (EDAX-make) Specimen stage: - Fully computer-controlled, eucentric side-entry, high stability CompuStage Sample Preparation: - - Ceramic sample preparation facility (Ion milling) (BALTEC make).

8 FT-IR SPECTROMETER Make : Bruker Optik GmbH, Germany Model No. : TENSOR 27 Source : Middle-infrared light (MIR) Detector : DLaTGS Spectral range : 370 to 7,500 cm-1 Spectral resolution : cm-1 Beam splitter: Ge-based coating on KBr Software : OPUS TM

9 UV-VIS-NIR DOUBLE BEAM SPECTROPHOTOMETER Make : VARIAN Model : Cary 500 Scan Wavelength range: nm Modes : Specular reflectance, Diffuse reflectance, Absorbance Make : VARIAN Model : Cary 5000 Scan Wavelength range: nm Spectral bandwidth: 0.01 nm Detector : PbS NIR Samples : Solid and liquid Accessories : Multi cell holder, Temperature attachment (-10 to 100 ºC) Modes : Specular reflectance, Diffuse reflectance, Absorbance

10 FLUORESCENSE SPECTROPHOTOMETER Make : VARIAN Model : Cary Eclipse Wavelength range: nm Source : Xenon pulse lamp Detector : Photo multiplier tube Modes : Excitation, Emission

11 SCANNING ELECTRON MICROSCOPE(SEM) Make : TESCAN Model : VEGA3 Magnification: x 30 x 3, 00,000 Specimen size : Max. 150 mm diameter Accelerating voltage: kv Resolution : kV high vacuum mode Attachments : Energy-dispersive X-ray. Spectroscopy (EDS) & Backscattered Electron Detector (BSED) True Windows NT environment: - Image management system for image processing, searching and archiving - Network capability to transfer SEM images and data to external PCs and servers Applications: - To study surface morphology of samples - Evaluation of crystallographic orientation

12 X-RAY ANALYTICAL MICROSCOPE (XRF) Make : Horiba, Japan Model : XGT-5200 X-ray analytical microscope Source : X-ray tube 50 kv max, 1 ma, with Rh target Detector : Peltier cooled Silicon Drift Detector (SDD) Elements Detected: Na to U (with sample at normal atmospheric pressure) CCD camera : Magnification 30 and 100 approx. Samples : Metal plates, powders and coatings Energy Range: 0-40 kev Maximum Measurement Area / Maximum Sample Size: 100 mm x 100 mm / 350 mm x 400 mm x 40 mm Description : The XGT-5200 X-ray Fluorescence micro-analyzers combine the fast, non-destructive elemental analysis of energy dispersive X-ray Fluorescence (EDXRF) with the capability to pinpoint individual particles with diameters down to 10 µm in size. Automated sample scanning provides detailed images of element distribution, over areas as large as 10cm x 10cm.

13 High Resolution- Transmission Electron Microscope Make : FEI Model : Tecnai F20 The 200kV FEI Tecnai F20 Super-Twin is designed to produce optimum high resolution performance in both TEM and STEM. This microscope features a 1024x1024 CCD camera positioned after the Gatan Imaging Filter (GIF) that can be used for both dedicated spectroscopic analysis and energy-filtered imaging. The high Resolution Gatan Orius 2672x2672 CCD can deliver high resolution and real time speed for imaging application. The Tecnai F20 is equipped with Lorentz Lens for magnetic imaging in Fresnel and Fouccault modes and NanoMegas Astar system for automated phase/orientation mapping of nanocrystals materials. Specifications : Electron source Flexible high tension (20, 40, 80, 120, 160, 200 kv and values in between) Schottky field emitter with high maximum beam current (> 100 na) High probe current (0.5 na or more in 1 nm probe) Small energy spread (0.7 ev or less) Spot drift < 1 nm/minute Vacuum levels: specimen chamber < Pa; gun < Pa Imaging TEM point resolution (.24nm) TEM line resolution (.102nm) Information limit (.14nm) Extended resolution (TrueImage) Minimum focus step (.16nm) TEM magnification range 25X-1030kx Camera length mm Maximized tilts for any X, Y, Z, α and β combination EDAX Energy-Dispersive X-ray detector Detector window: S-UTW Active area: 30 mm 2 Specimen-detector distance Collection angle Elevation angle Detector resolution 15 mm sterad 0 o 135 ev@ Mn K-α at 100 μs

14 Tip Enhanced Raman Spectroscopy (TERS) Raman: Renishew Invia Reflex Spectrometer focal length 250mm Raman Spectrum: 50cm-1 to 4000cm-1 Microscope: Specially adapted Research Grade Leica microscope allowing confocal measurements with better than 2.5µm depth resolution (using a 100x objective),2.5x, 20x and 50x objective. Laser: Air cooled Argon Ion Laser, 50Mw at 514nm, High power Infrared diode laser 250Mw at 785nm, Auto align and optimisation of input laser power Detector CCD array detector near infrared enhanced, deep resolution (576x384 pixels). Peltier cooler to -70 C AFM & Raman Atomic Force Microscopy (AFM) provides a variety of nanometric characterizations such as topography, conductivity, and thermal measurements. While very effective at measuring certain properties, AFM cannot identify the chemical composition of a given material. Raman spectroscopy, however, has emerged as a critical technique in the field of chemical characterization, accurately identifying and classifying materials in a number of diverse fields and industries such as: material science, chemistry, biophysics, semiconductors, and many more.