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CATALYSIS CAPABILITIES
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
- Graphitization (located outside of the CNMS) and carbonization
- Facilities
for handling air sensitive compounds - Schlenk
lines, glove boxes
Structural
characterization of oxide and metal nanomaterials, surface and
bulk structure
- Thermal
gravimetric analyzer
Capability for characterization of catalysts and analysis of catalyst preparation
and
treatments
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).
- ICP
for composition analysis
Capability for elemental analysis of samples by
ion coupled plasma analysis. Uses optical emission spectroscopy
for detection. (Located outside of the CNMS.)
Catalyst
performance characterization including gas and condensed phase
reactivity and selectivity
- 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 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 and liquid phase 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 system.
- Pulsed
chemisorption
Measurement of specific gas adsorption using the Altamira AMI-200.
- Plug
flow reactor
Ambient pressure operation currently optimized for studies
of desulfurization and H2S reduction reactions,
product detection by dedicated gas
chromatograph and/or FTIR. (Located outside of the CNMS).
- Automated
potentiometric surface acid/base titration
To measure proton binding isotherms, and proton affinity
distributions by Laplace transform analysis (located
outside of the CNMS).
- Electrocatalysis
Current-voltage relations to probe electrocatalytic processes.
- 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:
- q
-2q 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.
- X-ray
Fluorescence (see Electron Microscopy, Neutron and X-ray Scattering)
Bulk, powder, liquids, thin-film, standardless and standards-based
analysis. Mapping and multipoint capale with 50-micrometer resolution.
- Z-Contrast
Scanning Transmission Electron Microscopy (see Electron Microscopy,
Neutron and X-ray Scattering)
Hitachi HD2000 STEM
- 500
MHZ Liquid/Solid NMR Spectroscopy (see Macromolecular Nanomaterials)
- 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
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