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Temperature-Programmed Desorption of Single Zeolite Nanoparticles.

Xuannuo Yi¹, Shasha Liu^1,2, Taotao Zhao³

¹State Key Laboratory of Analytical Chemistry for Life Science, Chemistry and Biomedicine Innovation Center (ChemBIC), School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210023, China.

Journal of the American Chemical Society

|November 20, 2024

Summary

We developed optical TPD (oTPD) to measure single zeolite nanoparticles, revealing intrinsic acidity and kinetics. This method overcomes limitations of bulk measurements for better catalyst design.

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Area of Science:

Materials Science
Catalysis
Nanotechnology

Background:

Zeolites are crucial solid acid catalysts in chemical processes.
Temperature-programmed desorption (TPD) is a standard technique for zeolite acidity characterization.
Conventional TPD uses bulk samples, limiting the measurement of intrinsic acid properties due to mass transfer and thermal conduction effects.

Purpose of the Study:

To develop a novel method for measuring the intrinsic acid properties of single zeolite nanoparticles.
To overcome the limitations of conventional bulk TPD for zeolite characterization.
To establish a correlation between zeolite acidity and its structural features at the nanoscale.

Main Methods:

Developed an optical microscopy approach (oTPD) to measure TPD spectra of individual zeolite nanoparticles.
Utilized in situ monitoring of reduced scattering intensity during heating to track probe molecule desorption.
Correlated oTPD data with micro-Raman spectra of the same single nanoparticles.

Main Results:

oTPD revealed intrinsic desorption temperatures approximately 300 °C lower than apparent values from bulk TPD.
The peak width of desorption spectra was significantly narrowed from ~150 °C to ~15 °C using oTPD.
A linear relationship was found between zeolite acidity and silicon island content in single nanoparticles.

Conclusions:

oTPD enables precise measurement of intrinsic acid properties and desorption kinetics of single zeolite nanoparticles.
This technique provides unprecedented insights into the structure-acidity relationship in zeolites.
The findings have significant implications for the rational design of improved zeolite catalysts.