MACROMOLECULAR NANOMATERIALS CAPABILITIES

Polymer Synthesis

The Macromolecular Nanomaterials laboratories include a wide range of polymer synthesis capabilities, with extensive fume hoods (including walk-in hoods for large scale apparatus) and a glove box for handling sensitive materials.

• Ionic Polymerizations (cationic and anionic):Four dedicated high vacuum lines, two inert Schlenk lines, custom-made glove-box equipped with cold bath combined with custom glass blowing for preparation of well defined, narrow molecular distribution polymers and copolymers as well as complex polymer architectures, such as stars, combs, hyperbranched polymers, and bioinspired polymers.
• Controlled Radical Polymerizations: Expertise in free radical, controlled radical (ATRP, NMRP, RAFT) polymerizations.
• Other Polymerizations: Extensive experience in step-growth/condensation and Zeigler-Natta polymerizations.
• Polymer Composites: Expertise in polymer composites, especially polymer single-walled carbon nanotube composites.
• Novel Architectures: Linear, Block, Star, Graft and Dendrimeric Architectures.
• Bio-Inspired, Stimuli Responsive, and Conducting Polymers
• Deuterated Monomers & Polymers: Expertise in synthesis of deuterated monomers and polymers.

Macromolecular Characterization

The synthetic capabilities of the group are complemented by extensive analytical resources to provide rigorous characterization of materials produced by CNMS staff and Users. Multiple techniques are used to provide reproducible and accurate characterizations in the areas of: molecular weight and particle size determination, thermal analysis, Optical and spectroscopic analysis, imaging and structural characterization. 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.

• Nuclear Magnetic Resonance Spectroscopy (NMR)
  500 MHz Liquid/Solid NMR Spectroscopy. 400 and 700MHz Liquid/Solid NMRs available as shared resource.
• Organic Gel Permeation Chromatography (GPC)
  A Waters Alliance GPC system with quaternary gradient pumps, autosampler, column heater, differential refractive index detector, and photodiode array (PDA) detector in line with a 3 angle light scattering detector and viscosity detector from Wyatt Technology Incorporated.
• Aqueous GPC
  An Agilent 1100 series GPC system with a quaternary gradient pump, autosampler, vacuum degasser, column heater, refractive index detector, photodiode array detector, and a two angle light scattering detector from Precision Detectors.
• High-Temperature GPC
  A Waters Alliance GPCV 2000 system (up to 180°C) with autosampler, refractive index, viscosity, and two angle light scattering detectors for the analysis of polymers that are insoluble at ambient temperatures. All components are enclosed and heated to prevent precipitation or instability of solutions.
• Membrane Osmometer (MO)
  For measurement of absolute molecular weight from 20,000 to 1,000,000 g/mol.
• Vapor Phase Osmometer (VPO)
  For measurement of molecular weights from 100- 25,000 g/mol.
• Multi-angle Laser Light Scattering (18 angles) (MALLS)
  With Quasi-Elastic Light Scattering (QELS) capability of measuring molecular weight, size, hydrodynamic radii, and conformation of macromolecules in solution.
• Absolute and differential refractive index detector (DNDC)
  Wyatt Technology Optilab REX detector capable of measuring absolute refractive index and refractive index increment (dn/dc) of solutions at various temperatures. Photodiodes of several wavelengths are available to match the wavelengths of the various light scattering instruments in the CNMS Laboratories.
• Simultaneous Static and Dynamic Light Scattering
  (ALV) Goniometer system Based on a rotary disk allowing finest angular steps to be performed. Four detection angles separated each by 34° in angular space and temperature control 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.
• Rheometer
  TA Instruments ARES AR-G2 is capable of characterization of both the structure and flow properties of simple and structured fluids over a temperature range from -160 – 600°C. Cone and plate, parallel plates, and concentric cylinder geometries are available.
• Dynamic Mechanical Analyzer
  TA Instruments 800 dynamic mechanical analyzer 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.
• GC
  Hewlett-Packard 5890 GC with FID and autosampler for analysis of purity of small organic molecules.
• GC-MS
  Hewlett-Packard 7890 GC with a 5975 mass spectrometer with EI and CI ionization capabilities.
• Fluorescence Spectrometer (Spex Fluorolog 2) for probing the excitation and emission properties of small molecules and polymers.
• Matrix Assisted Laser Desorption Ionization- Time-of-Flight Mass Spectrometer (MALDI-TOF MS)
  The Bruker Autoflex is used for the determination of molecular weight of polymers and copolymers, end-group and compositional analysis, and protein identification and sequencing. Instrument can be run in linear and reflectron modes and contains a HIMAS detector sensitive to high molecular weight species.
• Thermogravimetric Analyzer
  (TA Instruments Q5000IR) capable of measuring weight losses (0.1 mg sensitivity) at very high heating rates up to 1200°C with very low drift under a variety of purge gases. Instrument has auto-sampler for unattended operation and sealed pan punch for analysis of sensitive samples. TGA with mass spectrometric analysis of the evolved gases (TA Instruments 2950TGA equipped with Pfeiffer Thermostar Mass spectrometer) is available as a shared resource for the simultaneous analysis of mass loss and evolved gas analysis (up to 300 amu).
• Differential Scanning Calorimeter
  (TA Instruments Q1000) with temperature range from -180 to 550°C. Sensitivity to 1 microwatt.
• UV-Visible-NIR
  Absorption spectrometer (Varian Cary 5000) 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)
  Spectrometer (mid and near IR regions, Bruker Vertex 70) Sample configurations including transmission, diffuse reflectance, ATR, as well as an IR microscope. Instrument has capabilities for vibrational circular or linear dichroism and IR reflectance absorbance spectroscopy. Spectral range from 30 cm-1 in the far IR to 25,000 cm-1 in the visible range.
• Spectroscopic Ellipsometer
  (JA Woollam M-2000U) for analysis of the thickness and refractive index of multi-layered structures. X-Y mapping stage.
• 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.
• 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 (programmable Linkam THMS 600 capable of -180°C < T < 600°C).

Capabilities provided by other CNMS groups
Catalytic Nanosystems
Functional Hybrid Nanostructures
Scanning Probes & Nanoscale Physics
Electron Microscopy, Neutron and X-ray Scattering
Nanomaterials Theory Institute
Bio-Inspired Nanomaterials
Nanofabrication Research Laboratory
General Characterization Facilities
Collaborating Facilities