Nanoscale Probing of Local Hydrogen Heterogeneity in Disordered Carbon Nitrides with Vibrational Electron Energy-Loss Spectroscopy

ACS Nano
Diane M Haiber, Peter A Crozier

Abstract

In graphitic carbon nitrides, (photo)catalytic functionality is underpinned by the effect that residual hydrogen content, manifesting in amine (N-H x) defects, has on its optoelectronic properties. Therefore, a detailed understanding of the variation in the local structure of graphitic carbon nitrides is key for understanding structure-activity relationships. Here, we apply aloof-beam vibrational electron energy-loss spectroscopy in the scanning transmission electron microscope (STEM) to locally detect variations in hydrogen content in two different layered carbon nitrides with nanometer resolution. Through low dose rate TEM, we obtain atomically resolved images from crystalline and disordered carbon nitrides. By employing an aloof-beam configuration in a monochromated STEM, radiation damage can be dramatically reduced, yielding vibrational spectra from carbon nitrides to be assessed on 10's of nanometer length scales. We find that in disordered graphitic carbon nitrides the relative amine content can vary locally up to 27%. Cyano (C≡N) defects originating from uncondensed precursor are also revealed by probing small volumes, which cannot be detected by infrared absorption or Raman scattering spectroscopies. The utility of this...Continue Reading

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Citations

Aug 1, 2018·Advanced Materials·Jacob R JokisaariRobert F Klie
May 14, 2019·Angewandte Chemie·Michael J ZachmanMiaofang Chi
Dec 24, 2018·Ultramicroscopy·O L KrivanekT C Lovejoy
May 20, 2021·ACS Nano·Andrea KonečnáF Javier García de Abajo
Jun 27, 2021·Microscopy and Microanalysis : the Official Journal of Microscopy Society of America, Microbeam Analysis Society, Microscopical Society of Canada·Kartik Venkatraman, Peter A Crozier
Oct 5, 2019·Chemistry of Materials : a Publication of the American Chemical Society·Hendrik SchlombergBettina V Lotsch

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