- 2-circle X-ray diffraction
X-ray powder diffraction with temperature-controlled sample environment. 77K to 1200K at 1 Bar, 273K to 1200K up to 10 Bar. Reactive gasses such as H2, CO for varying chemical composition in sample environment.
- 4-circle X-ray diffraction
4-circle plus translation stage, high temperature, in-plane thin film diffraction. Also texture, reflectivity, microdiffraction, reciprocal space mapping.
- Small-angle X-ray scattering, SAXS
Anton Paar SAXSess instrument for small-angle scattering to obtain nanoscale structural information. Also equipped for grazing-incidence measurements on nanomaterial films.
- 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.
The synthetic capabilities are complemented by extensive analytical resources for rigorous characterization of materials produced by CNMS staff and our user community. Additional capabilities applicable to polymeric materials (scanning probes, electron microscopy, Raman spectroscopy, etc.) are available in other groups within the CNMS or as shared resources at ORNL.
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.
- 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
-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.
- Matrix Assisted Laser Desorption Ionization-Time of Flight Mass Spectrometry (MALDI-TOF-MS)
Bruker MALDI-TOF Autoflex LRF instrument with imaging capabilities (5 micron spatial resolution) and capabilities for collisionally induced dissociation (CID) of any species. This system is equipped with the latest FlashDetector technology, enabling the instrument outstanding resolution (R > 26,000) and mass accuracy (≤ 2 ppm) in reflection mode for addressing the complexity of co-polymer samples. With its real on-axis detector design (in linear mode), the system is capable of detecting extremely large molecules > 500 kDa.
- Novocontrol broadband dielectric/impedance spectrometer
Turnkey broadband dielectric spectrometer with temperature control and data acquisition system. Broad frequency range and high measurement accuracy based on high-resolution ALPHA-A analyzer. Frequency range: 3×10-5 – 4×107 Hz; Capacity: 10-15 – 1 F; Impedance: 0.01 – 1014 W; Loss factor accuracy < 3×10-5, resolution 10-5. QUATRO Cryosystem: -160°C to 400°C, with temperature stability 0.01°C. A few different sample cells are available, including plate electrodes of different sizes, liquid sample cells, and devices for ultrathin film measurements. The Alpha-A Modular Measurement System from Novocontrol for dielectric, conductivity and electrochemical impedance spectroscopy is developed especially for materials research. A wide range of topics can be addressed by the dielectric technique, including molecular dynamics in confining space, collective dynamics of liquid crystals, molecular dynamics in thin polymer films, and dielectric properties of semiconducting materials.
- 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.
- Nuclear Magnetic Resonance Spectroscopy (NMR)
500 MHz multinuclear solution NMR Spectroscopy.
Hewlett-Packard 7890 GC with a 5975 mass spectrometer with EI and CI ionization capabilities.
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.
- Fourier Transform Infrared Spectrometer (FTIR)
Mid and far IR vacuum spectrometer with a variety of sample configurations including transmission, diffuse reflectance, ATR, as well as an IR microscope. Instrument has capabilities for vibrational circular and IR reflectance absorbance spectroscopy.
- 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
- Spectroscopic Ellipsometer
JA Woollam M-2000U for analysis of the thickness and refractive index of multi-layered structures.
- Phase Modulated Ellipsometer
Beaglhole Instruments Picometer Ellipsometer uses a photoelastic birefringence modulator to analyze the ellipticity of the reflected beam with a 1 ms response time and a detection limit of 1x 10 m. The Picometer Ellipsometer operates at a fixed wavelength of 632 nm.
- 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.
Soft Matter Transmission Electron Microscopy (TEM)
(listed in the Microscopy section of the proposal form)
A Zeiss LIBRA 120 TEM capable of operating voltage between 60 keV and 120 keV is available for soft matter imaging (e.g., polymers and their nanocomposites). The instrument can be used to acquire electron energy loss spectra for quantitative chemical and electronic structure analysis and is suitable for generating nano-diffraction patterns from regions as small as a few hundred nanometers.