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Macromolecular Nanomaterials

The Macromolecular Nanomaterials laboratories include a wide range of polymer synthesis capabilities with special emphasis on selective deuteration and ionic polymerization. 

Polymerization Techniques

  • Ionic Polymerizations: World-class expertise in the preparation of well-defined, narrow molecular distribution polymers and copolymers including complex polymer architectures (i.e. block, star, comb, graft and hyperbranched polymers) by anionic and cationic polymerizations. (Kunlun Hong)
  • Controlled Radical Polymerization: Extensive expertise in free radical and controlled radical (ATRP, NMP, RAFT) polymerizations. (Brad Lokitz, Kunlun Hong)
  • Ring Opening Polymerization: Expertise in the controlled ring-opening polymerization for the synthesis of well-defined polymeric materials. (Kunlun Hong)
  • Metal-catalyzed Cross-Coupling: Growing expertise in the synthesis of conjugated polymers by KCTP, Suzuki coupling, and other polymerization mechanisms. (Peter Bonnesen, Kunlun Hong)
  • Deuterated Polymers: Selective deuteration of polymers, enabled by our expertise in deuteration of small molecules, for the study of polymer morphololgy, dynamics and structure with neutron techniques. (Peter Bonnesen, Kunlun Hong)

Small Molecule Synthesis

  • Synthesis of novel monomers and small molecule building blocks: Expertise in small organic molecule synthesis and characterization. (Peter Bonnesen, Kunlun Hong)
  • Deuterated monomers, polymers, and specialty molecules: Unique expertise in synthesis of deuterated monomers and building blocks for neutron studies. (Peter Bonnesen, Kunlun Hong)

3D Printing and Additive Manufacturing

  • 3D Printing and Additive Manufacturing capabilities: SLA, FDM, SLS, DLP and other methods for a variety of polymer and composite materials. (Gobet Advincula)

Macromolecular Characterization

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.

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

  • 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. Bruker NEO console with broadband multinuclear probes, gradient diffusion probes, and Prodigy Cryoprobe.
  • 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.
  • Fourier Transform Infrared Spectrometer (FTIR) 
    Bruker Vertex70 spectrometer with a variety of sample configurations including transmission, diffuse reflectance, variable angle ATR, and temperature controlled ATR. Instrument has capabilities for vibrational circular and IR reflectance absorbance spectroscopy.
  • Fourier Transform Infrared Spectrometer (FTIR)  Microscope
    Bruker LUMOS is a fully automated stand-alone FTIR microscope with an 8x objective and can be used in transmission, reflection and ATR mode. The measurement results in a single file including visible images, spectral data and sample information. For evaluation and visualization of the microscopic data the software provides powerful and intuitive Chemical Imaging functionality.
  • 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. Temperature controlled and liquid sample environments available.
  • 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.

Chemical Imaging

  • ION-TOF NCS, AFM/FIB-ToF-SIMS consists of a high resolution time-of-flight secondary ion mass spectrometer (TOF-SIMS) including a 30keV BiMn cluster ion gun, 20keV Ar gas cluster source for dual-beam depth profiling and 3D analysis, dual-source O and Cs ion guns for low energy sputtering and thermal ionization and on-axis FIB tomography for very rough samples with a Ga ion source. The FIB-TOF-SIMS/SPM is capable of surface spectroscopy, surface imaging and depth profiling with co-registered in-situ SPM characterization. The coregistered SPM characterization includes non-contact mode analysis using MFM magnetic force microscopy, EFM electrostatic force microscopy, Kelvin probe microscopy; and in contact mode for topography, nanomechanical properties and conductivity.
  • Zeiss Orion Nanofab Helium Ion Microscope with SIMS features four primary capabilities: imaging, detailed ion-milling/patterning using He and Ne-ions, 3D direct write using gas and liquid precursors and chemical analysis using a doubly focusing magnetic sector secondary ion mass spectrometer (SIMS) with 4 separate detection channels. The microscope has down to 0.5 nm imaging resolution and down to 10 nm lateral chemical imaging resolution. The system is also equipped with Oxygen and Cs gas flooding to enhance SIMS signal.
  • Anasys Instruments NanoIR2-s is equipped with a 4-chip QCL laser and is capable of simultaneously providing AFM topographic imaging with nanometer-scale resolution infrared spectroscopy and IR imaging with sub-100nm spatial resolution, IR-SNOM with sub-20nm resolution. The instrument consists of an atomic force microscope designed for seamless integration with scattering Scanning Near Field Optical Microscopy (s-SNOM) and Atomic Force Microscopy Infrared (AFM-IR) techniques. In addition to nanoscale IR spectroscopy, the instrument can measure contact resonance frequencies of an AFM cantilever using the Lorentz Contact Resonance technique (LCR) in order to map variations in the sample’s mechanical properties; and provide local thermal properties via the nanoTA technique, for quantitative measurements of thermal transition temperatures at nanoscale spatial resolution.
  • Bruker Autoflex Speed II MALDI-ToF Imaging system is capable of imaging mass spectrometry (IMS) with a laser focus size between 10-100 μm with a mass resolution of >10,000 and a mass range of > 30,000.  The instrument is equipped MS/MS capability using (FAST/PSD) method with a mass accuracy of <0.4 Dalton on average. The resulting imaging data is analyzed by SCiLS Lab 2D Software.  The system must be capable of acquiring data in both the linear and reflectron configuration.
  • Zeiss Merlin VP Scanning Electron Microscope
    This SEM features variable-pressure capability to optimize studies of nonconductive samples or samples with low vapor pressures. Equipped with BF-STEM detector, surface profile backscatter imaging, and EDS spectroscopy.