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Nanomaterials Characterization

The CNMS maintains an exhaustive assortment of capabilities to characterize organic, inorganic, and hybrid functional materials and structures.

Signature Facilities

Inorganic and Hybrid Materials Characterization

     NEW!  SEM with Cathodoluminescence

     NEW!  Cryo-Optical Spectroscopies

     Tunable Low Frequency Raman Spectroscopy

     Dynacool Physical Property Measurement System

     Operando Raman Spectroscopy for Catalytic Systems

     Catalysis and Operando IR Spectroscopy

     X-ray Diffraction Laboratory

     Multifunctional Environmental Chamber

Macromolecular Characterization

     Broadband Dielectric Spectroscopy

     Nuclear Magnetic Resonance

     Bruker Lumos

     Bruker MALDI Mass Spectrometry

     Vertex 70

     Woolam Ellipsometer

Neutron Scattering

  • CNMS users are encouraged to take advantage of the world-class neutron scattering facilities that are available at ORNL’s High-Flux Isotope Reactor (HFIR) and the Spallation Neutron Source (SNS). Beamlines of particular relevance to CNMS Scientific Themes include the small-angle scattering and diffractometry instruments on the HFIR cold source, HFIR thermal neutron diffraction and spectroscopy capabilities, and instruments at the SNS including the backscattering spectrometer and the liquids and magnetism reflectometers. Please visit the ORNL Neutron Sciences website for more information about these neutron scattering facilities.

    CNMS users who would like to incorporate neutron scattering as a supporting component in their user proposals may request neutron beamtime by checking the appropriate box on the CNMS proposal form and attaching the 2-page Neutron Scattering appendix to provide details of their beamtime request. However, if the primary thrust of the proposal is to obtain access to neutron scattering, prospective users must submit the proposal directly to the neutron scattering user program.

Other Facilities

Inorganic Characterization

  • Semiconductor parameter analyzer, cryogenic probe station, and both DC and AC characterization systems
    • AC impedance spectroscopy system based on the Zahner analyzer IM6 supports traditional electrochemical investigations like impedance measurements (10 µHz-8 MHz, 10 Ohm-1 GOhm), cyclic voltammetry, corrosion, current-potential curves, etc. with modeling software by THALES. AC-amplitude range 1 mV to 1 V. Impedance range 10 mOhm to 1 GOhm (+/-1 dB).
    • Special configuration Zahner controlled intensity modulated photospectroscopy capability enables dynamic photo-electric investigations including mixed photo electric transfer functions on photo-sensitive objects (e.g. photovoltaic materials).
  • Intensity modulated (LED based: UV-NIR) Photocurrent/Photovoltage measurement (solid, liquid samples).
  • Optical characterization (UV-NIR): absorbance, transmittance, reflectance (diffuse and specular), PL, Raman under electrical excitation. Cary 5000 with special attachments. Calibrated OLED efficiency measurement system (including angular light distribution).
  • Cathodoluminescence microscopy including spectrally, spatially, polarization, temperature, angle, and time resolved analysis.
  • Spectral photoresponse and calibrated PV efficiency measurement system
  • Spectroelectrochemical Characterization of Nanomaterials and Composites
  • Combined electrochemical measurements during spectrophotometry. Investigations of reduction-oxidation reactions; nA sensitivity using Faraday cage with three-electrode stand.
  • Thermogravimetric analyzer with mass spectrometry (TGA-MS)
  • Volumetric gas adsorption
    • BET analysis of surface area and pore size distribution using nitrogen. (Quantachrome Autosorb 1-C and Micromeritics Gemini).
  • Electrocatalyst (EC), Photocatalysis (PC), and Photoelectrocatalysis (PEC) Reactor Systems
    • Reactor systems available for studying catalytic reactions, including PC and PEC (UV, visible and simulated sunlight illumination), with reaction products analyzed with gas chromatography and combinable with Raman spectroscopy for catalyst structure and surface species analysis.

Macromolecular Characterization

Molecular Weight Characterization

  • Size Exclusion Chromatography (SEC) 
    • Multiple SEC systems are available for molecular weight characterization in a variety of media (organic, aqueous) and temperatures. All systems are equipped with multidetector systems that include light scattering for absolute molecular weight determination.
  • Temperature Gradient Interaction Chromatography (TGIC) 
    • Unique chromatography technique for high resolution separation of polymers based on degree of polymerization rather than size. TGIC is particularly useful for the characterization of polymers with complex architectures.
  • Vapor Phase & Membrane Osmometry 
    • For measurement of absolute molecular weights from 100 to 1,000,000 g/mol.

Solution Properties

  • Multi-angle Laser Light Scattering (18 angles) (MALLS) 
    • Wyatt Heleos with Quasi-Elastic Light Scattering is capable of measuring molecular weight, hydrodynamic radii, and conformation of macromolecules in solution.
  • Simultaneous Static and Dynamic Light Scattering (DLS)
    • ALV Goniometer system based on a rotary disk allowing for precise angular steps. Four detection angles separated by 34° in angular space and temperature can be controlled from -10 to 140°C for simultaneous measurements of static and dynamic light scattering. Instrument contains prisms for depolarized detecting to obtain rotational diffusion coefficient.
  • Absolute and differential refractive index detector
    • Wyatt Technology Optilab Rex capable of measuring absolute refractive index and refractive index increment (dn/dc) of solutions at various temperatures and wavelengths.

Mechanical and Thermal Properties

  • Rheology 
    • TA Instruments Discovery Hybrid Rheometer (HR2) is capable of characterization of rheological properties of simple and complex fluids, gels, and elastomers over a wide temperature range of -160 - 600°C. Cone and plate, parallel plates (with solvent trap option), concentric cylindrical geometries, as well as the SER3 universal testing platform for extensional rheology are available.
      -Ubbelohde capillary viscometers of various sizes, capable of accurate measurement of low viscosity liquids from 0 - 150°C.
  • Dynamic Mechanical Analysis (DMA)
    • TA Instruments 800 DMA with various operating modes and test probes available with temperature range from -160 – 600°C. Three point bending, fiber, film, and cantilever geometries are available.
  • Thermogravimetric Analysis (TGA)
    • TA Instruments Q5000IR capable of measuring weight loss (0.1 mg sensitivity) at heating rates up to 1200°C under a variety of purge gases.
  • Differential Scanning Calorimeter (DSC)
    • TA Instruments Q2000 with temperature range from -180 to 550°C.
    • Nano DSC capable of characterization of the thermal stability and heat capacity of proteins and other macromolecules in dilute solutions. 

Spectroscopic Techniques

  • ​Rheo-dielectric capability
    • TA Instruments HR2 hybrid rheometer coupled with Keysight E4980 Precision LCR Meter, capable of performing simultaneous rheological and dielectric measurements, in the temperature range -160°C to 350°C. The voltage range is between 0.005 to 20 V with a frequency range of 20 Hz to 2 MHz. Disposable plates are available for curing system.
  • GC-MS 
    • Hewlett-Packard 7890 GC with a 5975 mass spectrometer with EI and CI ionization capabilities.
  • UV-Visible-NIR 
    • Varian Cary 5000 absorption spectrometer with liquid/solid sample holder, polarizers, diffuse reflectance, and specular reflectance accessory to probe the optical properties of solid, liquids, and solutions.
  • In Situ Fourier Transform Infrared Spectrometer (In-situ IR) 
    • Bruker IRCube with various probes for in-situ monitoring of chemical reactions in progress. Temperature range from cryogenic to 250°C, spectral range 7500-750 cm-1.

Thin Film Characterization

  • Contact Angle Goniometer 
    • The KRÜSS DSA 30 contact angle goniometer is equipped with a CCD camera and automated liquid handling controls allowing for precise measurements.
  • Optical Microscope 
    • The Leica DM4500P is an intelligent function research polarized microscope with one-button access to bright field transmission or reflected (incident), dark field transmission, as well as polarized (transmission or reflected) microscopy and auto tracking of calibration for spatial quantitation. Samples are examined on slides as well as a thermal stage.