NANOMATERIALS SYNTHESIS AND FUNCTIONAL ASSEMBLY (CATALYSIS)

Synthesis: porous materials, nanoparticles, sol-gel, hydrothermal and ALD

Three labs are available for catalyst preparation using a wide variety of synthesis methods. In-house synthesis expertise is available for designing and executing many catalyst preparations. Expertise in several synthesis techniques including:

  • Porous materials - oxides and carbon
  • Sol-gel materials – oxides and hydrid materials
  • Surface functionalization of oxides and carbon
  • Chemical synthesis of nanoparticles (metals, oxides, semiconductors)
  • Chemical synthesis of 1-dimensional materials (metals, oxides)
  • Atomic layer deposition (ALD) and surface sol-gel processing (SSG) for conformal functionalization of support surfaces (located outside of the CNMS).
  • Hydrothermal and solvothermal synthesis
  • Solid state synthesis-solid electrolytes, metal oxides and sulfides
  • Facilities for handling air sensitive compounds - Schlenk lines, glove boxes

Structural characterization of nanomaterials, surface and bulk structure

  • Thermal gravimetric analyzer with mass spectrometry
    Capability for characterization of catalysts and analysis of catalyst preparation and treatment procedures.
  • Volumetric gas adsorption
    Two instruments for volumetric gas adsorption (Quantachrome Autosorb 1-C and Micromeritics Gemini). Capable of measuring metal surface areas using specific reactive gases in addition to total BET analysis of surface area and pore size distribution using nitrogen.
  • Raman spectroscopy
    Raman spectroscopy with multi-wavelength laser system (~20 laser excitations, from UV Raman to NIR Raman) and online mass spectrometry for in situ/operando study of catalysis (laser training required, users must work with personnel assigned to equipment).
  • CHNS/O elemental analyzer
    Simultaneous determination of total nitrogen, carbon, sulfur, and hydrogen or oxygen in a wide range of organic and inorganic samples in amounts ranging from 0.01 (100 ppm) to 100%. (Thermo Scientific Flash 2000)

Functional characterization of nanomaterials including catalytic and electrochemistry performance

  • Plug-flow gas phase catalytic reactor
    Measurements of catalytic activity and selectivity under variable temperature, steady state plug-flow reaction conditions with mass spectrometer and gas chromatographic analysis of reaction products. Reactions performed using an Altamira AMI-200 or 300 system.  A SSITKA (Steady State Isotopic Transient Kinetic Analysis) capability is also available using the AMI-300 system.
  • Pulsed catalytic reactor
    With dynamic FTIR analysis of samples under transmission or diffuse reflectance modes and with continuous analysis of reaction products by mass spectrometry. System permits rapid gas switching and pulsing.
  • High Pressure Flow reactor
    Capable of running gas reactions up to 20 bar and temperatures to 800°C. Contains dedicated gas chromatographic and mass spectrometric analysis of products. Uses a PID Engineering reactor system.
  • Temperature programmed transformations
    Temperature programmed oxidation (TPO), temperature programmed reduction (TPR) and temperature programmed desorption (TPD) with thermal conductivity detector and with product detection by gas chromatography and mass spectrometry product detection. Processes performed using an Altamira AMI-200 and AMI-300 systems.
  • Pulsed chemisorption
    Measurement of specific gas adsorption using the Altamira AMI-200 or AMI-300.
  • Automated potentiometric surface acid/base titration
    To measure proton binding isotherms, and proton affinity distributions by Laplace transform analysis (located outside of the CNMS).
  • Battery Test Station
    Maccor 4000 battery cycler equipped with a temperature chamber for accurate temperature control from -20 to 100 °C. The cycler has 24 channels and allows simultaneous testing of 24 cells. Also available is a glove box with battery cell processing and assembly.
  • Frequency Response Analyzer
    Solartron 1260A with integrated potentiostat 1280 measuring frequency range from 32 MHz to 0.01 Hz.
  • Electrocatalysis

    Full suite of electrochemical characterization including bi-potentiostat, rotating disk electrode, impedance spectroscopy, electrochemical mass spectrometry (via quadrupole analyzer).

  • Additional specialized reactors including High-Pressure Flow Reactor, Benchtop Flow Reactor, and Ex-Situ Reactor may be available by separate arrangement. See Collaborating Facilities.

Related Techniques supported in other CNMS laboratories:

  • X-ray powder diffraction (see Electron Microscopy, Neutron and X-ray Scattering)
    Analysis of catalyst structure and transformations. In situ capabilities including temperature-controlled sample environment for 77 K to 1200 K operation at 1 Bar, 273 K to 1200 K at 10 Bar. Reactive gases such as H2, CO for varying chemical composition in sample environment.
  • 4-circle x-ray diffraction (see Electron Microscopy, Neutron and X-ray Scattering)
    4-circle plus translation stage, high temperature, in-plane thin film diffraction. Also texture, reflectivity, microdiffraction.
  • Z-Contrast Scanning Transmission Electron Microscopy (see Electron Microscopy, Neutron and X-ray Scattering)
    Hitachi HD2000 STEM
  • 500 MHZ Solution NMR Spectroscopy (see Macromolecular Nanomaterials). Solid-state NMR available by prior arrangement only (contact: Peter Bonnesen)
  • Raman Spectroscopy (see Optical-Nanostructure Interactions)
    Renishaw Raman microscope with He-Ne or Ar laser excitation.
  • First principles Computational catalysis (see Nanomaterials Theory Institute)
    Modeling based on first-principles quantum mechanical calculations; analysis of reaction thermodynamics and kinetics and reaction mechanisms. Offered under Nanomaterials Theory Institute as “NTI Staff Support, experimental project.”

 

Capabilities provided by other CNMS groups