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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 polymerizations, including GRIM polymerizations of pi-conjugated monomers,
and Zeigler-Natta polymerizations.
- Novel
Architectures: Linear,
Block, Star, Graft and Dendrimeric Architectures.
- Bio-Inspired,
Stimuli-Responsive Polymers: Controlled ring-opening polymerizations of lactone/lactide and N-carboxyanhydride (NCA) monomers.
- 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 Solution NMR Spectroscopy. Solid-state NMR
available by prior arrangement only (contact: Peter
Bonnesen)
- 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).
- Transmission Electron Microscopy (TEM)
A Zeiss LIBRA 120 TEM (being brought on-line in Spring 2011) capable of operating between 60 keV and 120 keV is available for soft matter imaging (e.g., polymers and copolymers 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 high angular resolution nano-diffraction patterns from regions as small as a few hundred nanometers.
Capabilities
provided by other CNMS groups
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