CATALYTIC NANOSTRUCTURES

Solution synthesis of many functional inorganic nanostructures

Synthesis expertise is available for designing and executing many functional nanomaterial preparations. Expertise and capability 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 and nanorods (metals, oxides, semiconductors)
  • Chemical synthesis and exfoliation of 2-dimensional materials
  • Hydrothermal and solvothermal synthesis
  • Solid state synthesis-solid electrolytes, metal oxides and sulfides
  • Facilities for handling air sensitive compounds - Schlenk lines, glove boxes

Spectroscopic characterization of nano-catalytic materials

  • 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.
  • In-situ FTIR 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.

Bulk and surface structural characterization of nanomaterials

  • 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.
  • 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).

Catalyst performance characterization of nanomaterials

  • 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.
  • 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.

Electrocatalysis and photocatalysis characterization of nanomaterials

  • Full suite of electrochemical characterization including bi-potentiostat, rotating disk electrode, impedance spectroscopy, electrochemical mass spectrometry (via quadrupole analyzer).
  • Solid oxide fuel cell equipped with gas chromatographic and mass spectrometric analysis of products.
  • Photocatalysis (PC) and photoelectrocatalysis (PEC) reactor systems available under UV, visible and simulated sun light illuminations and products being analyzed with gas chromatography. In situ EC, PC and PEC Reactors combinable with Raman spectroscopy for catalyst structure and surface species analysis.

Battery Assembling and Testing

  • 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.
  • Frequency Response Analyzer
    Solartron 1260A with integrated potentiostat 1280 measuring frequency range from 32 MHz to 0.01 Hz.
  • Glove box with battery cell processing and assembly.

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.
  • Medium-resolution TEM – Zeiss Libra 120 TEM (see Microscopy, Neutron and X-ray Scattering) Support for synthetic activities; analysis of morphology, size distribution and elemental composition. 
  • High-performance electron microscopy (see Microscopy, Neutron and X-ray Scattering) High-resolution TEM, aberration-corrected ultraSTEM, energy-dispersive spectroscopy and electron energy-loss spectroscopy.
  • 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