Imaging and Analytical Modes

• SEM secondary electron (SE) imaging of topography, morphology, and fine surface structure (at low <2 kV accelerating voltage)
• EDS elemental mapping and semi-quantitative composition analysis from millimeter to micrometer level

Features

• Cold field emission electron gun
• Accelerating voltage: 0.5 – 30 kV
• Magnification: up to 500,000x
• Secondary electron image resolution:
  • 2.5 nm at 2 kV
  • 1.5 nm at 15 kV
• Sample size: up to 25 mm diameter
• Sample tilt: -5 – +45°
• Sample rotation: 360°
• WD: 2.5 – 27.5 mm 

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Imaging and Analytical Modes

• TEM bright field and dark field imaging, and selected area electron diffraction (SAED)
  • Determine the internal structure of materials
    • Crystalline: lattice fringes, SAED spots (single crystals) or SAED concentric rings (polycrystalline materials)
    • Amorphous: no lattice fringes, no SAED patterns
  • Determine the microstructure of materials
    • Grain size
    • Defects
    • Dislocations
    • Local microstructure (interfaces, individual nanostructures)
• EDS elemental mapping and semi-quantitative composition analysis from micrometer to nanometer level

Features

• Electron gun filament: LaB6
• High resolution TEM: 0.10 nm (lattice), 0.18 nm (point-to-point)
• Accelerating voltage: 300 kV, 200 kV, 100 kV
• Magnification: up to 1,500,000
• Hitachi single tilt holder (tilt α = ±15°)
• Hitachi double tilt holder (tilt α = ±15°, β = ±15°)
• Hitachi in-situ gas injection heating holder
• TEM grid size: 3mm diameter

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Typical Uses and Applications

• FIB – used for site-specific material removal or deposition
  • Removal = Sputtering/Milling
    • Create site-specific cross-sections of materials for in-situ viewing be SEM in defect analysis, materials characterization
      • Mill and Monitor (automated process, use SEM to record images of thin slices incrementally milled by FIB)
    • Site-selective TEM sample preparation (use SEM to monitor preparation of sample cross-section by FIB)
      • Prepare micro-sample from the original sample
      • Lift-out micro-sample onto FIB grid (micro-sample carrier) with micro-sampling probe
      • Thin micro-sample to ~100 nm thickness for TEM observation
  • Deposition
    • W films – to protect sample surface during FIB processing, bond micro-sample to micro-sampling probe
    • C films – use before W deposition to preserve sample surface features
• SEM – used for sample imaging, enables the use of ED
  • Imaging at 30 kV for thinned (~100 nm) TEM samples using STEM detector
• EDS elemental mapping and semi-quantitative composition analysis from millimeter to micrometer level

Features

• Vertical Ga+ ion column (FIB)
• Electron column tilted at 58° to vertical (SEM)
• FIB accelerating voltage: 1 – 40 kV
• SEM accelerating voltage: 0.5 – 30 kV
• SEM magnification: up to 800,000x
• Eucentric stage: SEM-style sample holder, max. sample size: 30mm diam.
• Side entry stage: TEM-style sample holder, sample size: 3mm diam.
• FIB-SEM holder compatible with TEM

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Analytical Modes and Applications

• Analytical Modes
  • AC Mode Imaging in Air – Repulsive Mode (intermittent contact mode) – for imaging hard materials and polymers
  • AC Mode Imaging in Air – Attractive Mode (non-contact mode) – imaging dried biological (soft) materials that should not be perturbed
  • Contact Mode – for imaging hard materials
• Uses and Applications
  • Imaging of topography
    • Measure nanoscale surface roughness
    • Measure nanoscale step height
    • Determine size distribution of deposited nanoparticles
  • Conductive AFM (CAFM) imaging – measurement of electrical behavior of thin films (current passing through a sample and a tip is sensed)
    • Determine conductivity
  • Force spectroscopy – measurement of the deflection of the cantilever on the sample surface
    • Determine the interaction force between the tip and the sample surface

Features

• AFM scanning in air
• Closed-loop, low noise, high precision scanner
• Max. scan size: 90 x 90 μm
• Max. vertical range: 24 μm
• Sub-angstrom vertical resolution
• Lateral resolution is limited by tip geometry, not the instrument

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Analytical Modes and Applications

• Analytical Modes
  • Tapping Mode in Air – for imaging hard materials and polymers
  • Contact Mode in Air – for imaging hard materials
  • Contact Mode in Fluid – for imaging hard materials and biological materials
  • ScanAsyst Mode (enables auto-optimization of scanning parameters)
    • ScanAsyst and PeakForce Tapping Mode in Air
    • ScanAsyst and PeakForce Tapping Mode in Fluid
• Uses and Applications
  • Imaging of topography
    • Measure nanoscale surface roughness
    • Measure nanoscale step height
  • Analysis in fluid cells and in controlled environments

Features

• AFM scanning in air and in liquids
• Closed-loop, low noise, high precision scanner
• Max. scan size: 90 x 90 μm
• Max. vertical range: ~7 μm
• Sub-angstrom vertical resolution
• Lateral resolution is limited by tip geometry, not the instrument

Capabilities

• System is an optical microscope that uses fluorescence to generate an image
  • aqueous specimens, live or fixed cells, either fluorescent samples or samples marked with fluorescent molecules
• System is a confocal fluorescence microscope
  • Eliminates (blocks) out-of-focus signal in image formation, only in-focus signal is used
    • Increased resolution in the sample depth direction
  • Captures multiple 2D images at different depths in a sample (optical sectioning) and reconstructs 3D structures
  • Allows direct, noninvasive, serial optical sectioning of intact, thick living specimens with minimum sample preparation

Features

• Yokogawa CSU-X1 Spinning Disc with CSUX1FW high-speed filter wheel
• Zeiss Axio Observer Z1 Inverted Microscope with motorized X, Y, Z Stage
• X-Cite 200DC Illumination System (340 – 800 nm filter)
• Okolab Full Enclosure Incubator with Temperature Control
• Fluorescent filter sets: DAPI, GFP and TxRed
• Lasers: 488 nm (blue) and 561 nm (green)
• Objectives: 5x Air, 10x Air, 20x Air, 40x Oil, 63x Oil, 100x Oil
• Evolve EMCCD Camera for fast imaging
• Software: SlideBook

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Capabilities

• Combined system capable of both metal sputtering and carbon evaporation
  • Cool magnetron metal sputtering using Au, Au/Pd (80/20), Pt, Cr, Ir targets
  • Carbon rod evaporation
• Sputter coater is typically used for producing uniform metal coating on the surface of the specimen to improve SEM results
  • Inhibit charging effects
  • Reduce thermal damage
  • Improve secondary electron emission
• Coating
  • To a predetermined thickness (use film thickness monitor)
  • By a build-in timer

Features

• Fully automated coating process
• Scroll pump
• Turbomolecular pump
• Ultimate vacuum: 1 x 10˄-6 mbar
• Equipped with Film Thickness Monitor 

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Features

• Uses white light as a light source
• Eyepieces: 10x
• Objective lenses: 5x, 10x, 20x, 50x, 100x
• Manual stage
• Techniques
  • Brightfield (BF)
  • Darkfield (DF)
  • Differential Interference Contrast (DIC)
• Illumination – Reflected (EPI), Transmitted (DIA)
• Nikon CooPix950 digital camera for image capture

Features

• Stereomicroscope (3D visualization of a sample)
• Uses white light as a light source
• Eyepieces: 10x
• Objective lenses: Plan Apo 1x
• Total magnification: 10x – 63x 
• Working Distance (WD): 78 mm
• Reflected (EPI) illumination
• Nikon CooPix950 digital camera for image capture

Typical Applications

• Powder samples
  • Non-monochromatized Cu Kα radiation
  • SmartLab Studio II software to analyze XRD data
    • Phase identification
    • Phase composition (wt% of the phases present in the sample) determination
    • Lattice parameter refinement
    • Crystallite size and lattice strain determination
    • % Crystallinity determination

Features

• Benchtop X-ray diffractometer
• Cu X-ray tube (Cu Kα radiation)
• D/teX Ultra high speed 1D detector
• Vertical θ/2θ goniometer with a horizontal sample mount
• Standard sample stage
• ASC-8 automated sample changer with spinner
• SmartLab Studio II software

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Typical Applications

• Powder samples – use Bragg-Brentano (divergent beam) optics
  • Low angle XRD (Min. 0.5 °2θ) – for materials with a long-range order
  • In-situ high-temperature XRD analysis for phase transitions
• Thin film samples – use parallel beam optics and Cu Kα or Cu Kα1 radiation
  • Grazing incidence XRD (GIXRD) – for very thin films
  • Pole figure measurement – determine sample texture
  • High resolution XRD (HRXRD) – use Cu Kα1 radiation for near-perfect crystals, epitaxial films to improve resolution
    • Rocking curve (w-scan) – study defects in films (e.g., mosaic spread, curvature, misorientation)
    • 2θ-w coupled scan – study lattice mismatch, composition, strain/relaxation
    • X-ray reflectivity (XRR) – determine layer(s) thickness, density, and roughness
• Residual stress analysis of polycrystalline samples – use high 2θ angles (> 120 °2θ)
• Transmission small angle X-ray scattering (SAXS) analysis of powder samples in capillaries
  • Determine the particle or pore size distribution
• Micro area mapping – mapping of sample phase composition requiring spatial resolution of 500 and 100 μm

Features

• General purpose XRD system
• Cu X-ray tube
• HyPix-3000 high energy resolution 2D detector
• Vertical θ/θ goniometer with a horizontal sample mount
• Ge(220) 2 bounce crystal monochromator
• Sample plates: 4” Wafer, Height reference, Transmission SAXS
• Attachment heads: Standard, RxRy, XY 20 mm
• Attachment bases: Standard, ASC-6, φ, χφ
• Multipurpose high-temperature attachment (RT-1500 °C)

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Capabilities

• Surface analysis (analysis depth < 10 nm)
  • Determine sample elemental composition
  • Determine oxidation (bonding, chemical) states of specific element
• Sputter depth profiling (manual or programmable) – determine the composition change of a thin film along the entire film thickness
  • Series of spectra acquired at different sample depths after material was sputtered with Ar+ ions
• Angle resolved XPS – determine the composition change of a thin film at the near surface region without sputtering
  • Sample is tilted between 90° – 5° with respect to the electron energy analyzer. Analysis depth decreases with the decreasing sample tilt angle.
• Map acquisition – 2D display of elemental information
  • Map consists of an array of individual pixels. A complete spectrum is collected at each pixel.
• Typically use Al X-ray source, but if Auger peaks overlap photoelectron (XPS) peaks can use Mg X-ray source to separate them
  • Photon energy of Al Kα = 1486.6 eV, photon energy of Mg Kα = 1253.6 eV (Difference = 233 eV)
  • Shift Auger peaks positions by 233 eV, while XPS peaks positions remain unchanged on the binding energy scale

Features

• Monochromatic Al X-ray source (FXS)
• Achromatic Mg X-ray source (Conventional source)
• Electron energy analyzer
• Electron neutralizer
• Ar+ ion gun
• High vacuum: ~10˄-8 Pa (roughing pumps, TMPs, Ion pump, Titanium sublimation pump)
• Analysis spot: 10 – 100 μm

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Capabilities

• Study and identify chemical substances or functional groups in solids and liquids
• VERTEX 70 FTIR Spectrometer – for bulk samples
  • Transmittance accessory (MIR = 8,000-350 cm-1, NIR = 12,800-5,800 cm-1)
    • For sufficiently thin and transparent solids (need to be pressed into thin pellets) and liquids
  • HARRICK Praying Mantis DRIFTS accessory (MIR = 4,000-400 cm-1)
    • For powders/ground samples, may need to dilute sample with KBr
  • Bruker Optics Platinum ATR (diamond crystal) accessory (MIR = 8,000-350 cm-1, NIR = 10,000-5,800 cm-1)
    • For strongly absorbing, black, thick samples
    • Liquids, solids, powders, rubber, pastes, gels, creams, films, surface coatings
    • Only thin layer (~0.5 – 2 μm) is analyzed
• Hyperion 2000 IR microscope – for micro samples, small sample areas, examination of inhomogeneities in heterogeneous samples
  • 15x objective – for transmittance and reflectance (MIR = 8,000-600 cm-1, NIR = 10,000-2,000 cm-1)
    • Transmittance mode – for sufficiently thin and transparent samples
    • Reflectance mode – for solid samples with very smooth surfaces
  • 20x ATR II (Ge crystal) objective – for ATR (MIR = 5,000-600 cm-1, NIR = 5,000-2,000 cm-1)
    • ATR mode – for strongly absorbing, black, thick solid samples
    • Only thin layer (~0.5 – 2 μm) is analyzed

Features

• VERTEX 70 FTIR spectrometer (resolution: 0.4 cm-1)
  • MIR source, KBr beamsplitter, RT DLaTGS detector
  • NIR source, CaF2 beamsplitter, RT InGaAs detector
  • Analysis spot: ~1.6 x aperture size
  • Transmittance, DRIFTS, ATR accessories
• Hyperion 2000 IR microscope (resolution: 0.4 cm-1)
  • MIR source, KBr beamsplitter, LN2-cooled MCT detector
  • NIR source, CaF2 beamsplitter, LN2-cooled MCT detector
  • 15x objective (Min. analysis spot: 15 μm)
  • 20x ATR II objective (Analysis spot: 5 – 100 μm)
• PIKE Crush IR hydraulic press with pellet press

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Capabilities

• Study and identify chemical substances or molecular structures in solids and liquids
• Senterra Dispersive Raman Microscope Spectrometer
  • 532 nm laser, spectral range 50 – 3,700 cm-1
  • 785 nm laser, spectral range 100 – 3,500 cm-1
  • For samples, which do not fluoresce when exposed to laser radiation in visible range
    • Micro samples, small sample areas, examination of inhomogeneities in heterogeneous samples
    • Chemical mapping or surface scan – acquire spectra at predefined measurement positions arranged by moving the sample in x- and y-direction using a motorized stage
    • Depth profiling – acquire spectra at the same x, y measurement position but in different predefined sample layers by moving the laser focus incrementally deeper into the sample
    • 3D map – combination of surface scan and depth profiling
• RAM II FT-Raman spectrometer and RamanScope III microscope
  • For samples, which tend to fluoresce when exposed to laser radiation in visible and UV range
  • Spectrometer – for bulk samples
  • Microscope – for micro samples, small sample areas, examination of inhomogeneities in heterogeneous samples

Features

• RAM II FT-Raman spectrometer / RamanScope III microscope
  • 1064 nm Nd:YAG laser (500 mW)
  • NIR LN2-cooled Ge detector
  • NIR CaF2 beamsplitter
  • Spectral resolution: 0.8 cm-1
  • 40x objective (microscope)
• Senterra Dispersive Raman Microscope Spectrometer
  • 785 nm (100 mW) and 532 nm (20 mW) lasers
  • Thermoelectrically cooled CCD detector
  • Spectral resolution: 3-5 cm-1
  • 4x, 20x, 50x objectives

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Capabilities

• Determine optical properties of materials (solids, liquids)
• Need the sample and the reference (baseline) spectra
• Powders
  • Use the HARRICK Praying Mantis diffuse reflectance accessory and matching sampling cups for the reference and the sample
    • Reference = Spectralon (PTFE powder)
    • Sample = Sample of interest
• Thin films
  • Use thin film sample holder and matching solid sample slides for the reference and the sample
    • Reference = Substrate alone
    • Sample = Film on substrate
• Liquids
  • Use liquid sample holder and matching cuvettes for the reference and the sample
  • Quartz cuvettes – transparent in the UV/Vis range
  • Glass cuvettes – transparent in the Vis range
  • Plastic cuvettes – noise below 250 nm
    • Reference = solvent alone
    • Sample = solute + solvent

Features

• Deuterium lamp – for the UV region
• Halogen lamp – for the Vis/NIR region
• Spectral range: 200 nm – 3000 nm
• Different accessories/holders for powders, thin films, liquid

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Features

• Split/Splitless (SSL) inlet for all capillary columns
• Automatic Liquid Sampler (ALS)
  • 16 vial turret
• Detector:
  • Mass Selective Detector (MSD)
  • Instrument Detection Limit (IDL): 24 fg
• Ionization mode: Electron ionization (EI)
  • Stainless steel source
  • Ion source temperature: 150–350 °C
  • Quadrupole temperature: 106–200 °C
• Micro-Ion vacuum gauge
• Column: Capillary Column
• Carrier: Helium
• Software:
  • GCMS MassHunter
  • MS Quantitative Analysis
• Library: NIST 2014 MS

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Capabilities

• Determination of the particle size distribution of particles suspended in water and other liquids
• Light source: two 3 mW Laser Diodes, wavelength 780 nm
• Principle of operation: dynamic light scattering (DLS)
  • Need to provide
    • Particle refractive index, shape (spherical, irregular), transparency (transparent, absorbing, reflecting)
    • Dispersing liquid viscosity and refractive index
• Need to have well dispersed particles
  • Use water, surfactants, solvents, ultrasonication
• Measurement range: 0.8 nm – 6.54 μm
• Size: hydrodynamic diameter = the equivalent spherical diameter of a particle with the same translational diffusion coefficient as the measured particle
• pH range: 3 – 11
• Min. sample volume: 3 mL
• Measurement temperature: 20 °C – 30 °C
• Sample concentration: must be within the optimal range determined by the instrument
• Software: Microtrac FLEX

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Features

• Determination of the particle size distribution of dry powders suspended in flowing air
• Model: Aerosizer LD
• Light source: 3 mW Laser Diode
• Principle of operation: Aerodynamic time-of-flight
  • Need to provide material density
• Aero-Disperser accessory: dry powder dispersing system
  • Advanced fluidization, controlled de-agglomeration and proprietary transonic flow dispersion technology
  • Very good results for both “free flowing” and “highly cohesive” powders
• Measurement range: 200 nm – 700 μm
• Size: geometric diameter = the equivalent spherical diameter of a particle with the same density as the measured particle

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Features

• Determination of the specific surface area, pore volume, and pore size distribution of microporous and mesoporous materials
• Automated gas sorption analyzer
• Adsorbate gas: Nitrogen
• Measurement temperature: LN2 boiling point (77.4 K)
• Two outgassing stations
• Two physisorption stations
• 6 mm, 9 mm, 12 mm physisorption cells
• 90,000 rpm TMP backed by dry diaphragm pump
• Outgassing temperature: up to 350 °C
• Software: ASiQwin

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Features

• Measurements of particles suspended in aqueous and other polar media
• Principle of operation: measurement of streaming potential
• Sample (particles + dispersing medium)
  • Particle size: < 100 μm
  • Volume: 10 mL
  • Concentration: 0.001 – 70 wt% or 0.001 – 40 vol%
  • pH: 2 – 12 (pH measurements only in aqueous media)
• Titrant
  • Aqueous media only (to avoid damage of the pH electrode)
  • Volume: 0 – 20 mL
  • Min. single titration step: 10 μL
  • pH: 2 – 12

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Features

• Measure the difference between the heat flows to the sample and reference crucible as a function of temperature
• Temperature range: -150 – 700 °C
• Measurements in: Dry air or Nitrogen  
• Crucible size: 40 μL
• Max. heating rate: 100 K/min
• Temperature accuracy: ±0.2 °C
• Resolution: 0.04 μW at RT
• LN2 cooling to -150 °C

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