Transmission IR and In-Situ DRIFTS
To examine the FTIR spectra of a specific material or investigate gas adsorption on its surface, Operando Diffuse Reflection Infrared Fourier-Transform Spectroscopy (DRIFTS) can be employed. This technique captures the adsorbent reaction spectra as a function of temperature over the desired material. The data is recorded using a Bruker Vertex 70 spectrometer equipped with a liquid nitrogen-cooled mercury cadmium telluride (MCT) detector.
The samples for DRIFTS and the absorbing gas are positioned within a Praying Mantis High-Temperature Reaction Chamber from Harrick Scientific Co., located in Ossining, NY. This chamber is equipped with ZnSe windows to facilitate observations. The gas flow during experiments is precisely controlled at a specific rate (mL∙min−1), comprising either the carrier gas, the reducing gas, or the adsorbent gas.
The instrument operates under the control of OPUS v 7.8 software, ensuring accurate and reliable data acquisition and analysis.
Instrument Managers
Jennifer Naglic: jnaglic@email.sc.edu
Azadeh Mehrani: amehrani@mailbox.sc.edu
Thermogravimetric Analysis (TGA)
We utilized a 2010 Shimadzu thermogravimetric analyzer, model TG-50H, featuring a TA-60WS thermal analysis unit, a GC-60A flow control unit, and a BLW-50 cooling blower. The instrument is equipped to handle a wide range of heating rates, ensuring precise thermal analysis. The thermal analysis technique employed involves measuring the mass of a sample as the temperature varies over time. TGA offers valuable insights into various material properties, including phase transitions, coke formation, reduction/oxidation states, and thermal decomposition. The instrument supports different gas environments, such as air, nitrogen, oxygen, argon, enabling versatile experimentation.
Moreover, the TGA is versatile enough to accommodate both dense and non-dense materials, with balance options of 20 or 100 mg for dense or non-dense materials, respectively. This adaptability extends to the capability of taking material measurements in different environments, including air, CO, argon, or other specified conditions.
Instrument Managers
Kaveh Shariati: shariati@email.sc.edu
Thossaporn Onsree: onsree@mailbox.sc.edu
Physisorption/Chemisorption/TPX
Static Chemisorption is employed to assess the dispersion of active metals and analyze the adsorption characteristics of selected molecules, ranging from weak to strong interactions.
Physisorption is utilized to elucidate the structure of supports, with a particular focus on determining pore sizes and surface area.
Temperature-Programmed Desorption, Oxidation, and Reduction (TPX) are employed for the in-depth analysis of desorption, oxidation, and reduction processes of selected molecules, providing valuable insights into their dynamic behaviors.
Instrument Managers
Jennifer Naglic: jnaglic@email.sc.edu
Samuel Drummond: drummos@email.sc.edu
Powder X-Ray Diffraction
The Rigaku MiniFlex II benchtop XRD, featuring an automatic 6-position sample changer and equipped with the D/teX Ultra high-speed silicon strip detector, supported by an available 600 W X-ray source.
This multipurpose powder diffraction analytical instrument offers comprehensive capabilities, allowing for:
- Crystalline phase identification and quantification
- Percent crystallinity determination
- Analysis of crystallite size and strain
- Lattice parameter refinement
- Rietveld refinement
- Molecular structure analysis
Instrument Manager
Jennifer Naglic: jnaglic@email.sc.edu
Patrick Holcombe: holcomp@email.sc.edu
In-Situ and Ex-Situ Raman Spectroscopy
The Horiba XploRA PLUS is a versatile Raman microscope. The instrument is a compact benchtop analytical instrument for chemical analysis. The instrument features two laser sources: 638 nm and 473 nm, along with four gratings at 600 (750 nm), 1200 (750 nm), 1800 (450 - 850 nm), and 2400 (400 nm). This allows for versatile spectral analysis.
Raman Spectroscopy is a non-destructive chemical analysis technique providing comprehensive insights into chemical structure, phase and polymorphism, crystallinity, and molecular interactions. This information is derived from the interaction of light with chemical components within a substance.
To facilitate in-situ Raman spectroscopy and investigate changes in substances upon contact with probe molecules, a gas line is connected to the instrument. This capability enhances the instrument's versatility for dynamic studies of chemical transformations.
Additionally, the instrument functions as an optical microscope, enabling the observation of materials at the micrometer scale.
Instrument Manager
Kaveh Shariati: shariati@email.sc.edu
Thossaporn Onsree: onsree@mailbox.sc.edu
High-throughput Reactor System
High-throughput experimentation has been demonstrated to accelerate the discovery and development of new catalyst formulations and routes for desired products while optimizing reaction conditions. Our group has two multi-channel parallel fixed-bed reactor systems with well-designed flow and temperature controls. A Bruker Equinox 55 FTIR spectrometer with a 128 × 128-pixel mercury cadmium telluride FPA detector (Santa Barbara Focalplane, Goleta, CA, USA), as well as Gas Chromatography with Flame Ionization and Thermal Conductivity detectors, can be employed to analyze the product downstream.
