Macromolecular Nanomaterials

Macromolecular Nanomaterials

Performs precise synthesis of functional polymers with special emphasis on selective deuteration, small molecule synthesis, and ionic polymerization, as well as macromolecular characterization.  Capabilities available to users:

  • 500 MHz Solution NMR Spectroscopy

    • Multinuclear solution NMR Spectroscopy. Bruker NEO console with broadband multinuclear probes, gradient diffusion probes, and Prodigy Cryoprobe.

  • Deuterated monomers, polymers, ionic liquids, and specialty molecules

    • 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)
       
    • Unique expertise in synthesis of deuterated monomers and building blocks for neutron studies. (Peter Bonnesen, Kunlun Hong)
       

  • Macromolecular characterization- molecular weight, spectroscopy, scattering, thermal analysis,  broadband dielectric spectroscopy

    • 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.
       
    • 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.
       
    • 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.
       
    • 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.
       
    • 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.
       
    • 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. 
       

  • MALDI-ToF MS/MS and MALDI-ToF Imaging 

    • 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. 
       
    • 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.
       

  • Polymer synthesis (Anionic, radical, cationic, and step growth polymerizations; composite materials)

    • 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)
       
    • Extensive expertise in free radical and controlled radical (ATRP, NMP, RAFT) polymerizations. (Brad Lokitz, Kunlun Hong)
       
    • Expertise in the controlled ring-opening polymerization for the synthesis of well-defined polymeric materials. (Kunlun Hong)
       
    • Growing expertise in the synthesis of conjugated polymers by KCTP, Suzuki coupling, and other polymerization mechanisms. (Peter Bonnesen, Kunlun Hong)
       

  • Synthesis of novel monomers and precursors

  • Thin Film Characterization- ellipsometry, FTIR-ATR, FTIR microscopy, contact angle goniometer

    • JA Woollam M-2000U spectroscopic ellipsometer for analysis of the thickness and refractive index of multi-layered structures. Temperature controlled and liquid sample environments available.
       
    • The KRÜSS DSA 30 contact angle goniometer is equipped with a CCD camera and automated liquid handling controls allowing for precise measurements.
       
    • Leica DM4500P optical microscope 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.
       
    • Bruker Vertex70 FTIR spectrometer with variable angle ATR, and temperature controlled ATR.
       
    • 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.
       

  • 3D printing and additive manufacturing capabilities include SLA, FDM, SLS, DLP and other methods for a variety of polymer and composite materials

    • SLA, FDM, SLS, DLP and other methods for a variety of polymer and composite materials. (Gobet Advincula)
       

  • X-ray diffraction and small-angle scattering  ​​​​​​​​​​​​​​​​​(Jong Keum)