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Microreactor-Based TG-TEM Synchronous Analysis.

Fanglan Yao1,2, Pengcheng Xu1,2, Ming Li1

  • 1State Key Lab of Transducer Technology, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai 200050, China.

Analytical Chemistry
|June 2, 2022
PubMed
Summary
This summary is machine-generated.

A new silicon microreactor enables simultaneous thermogravimetric-transmission electron microscopy (TG-TEM) analysis, precisely measuring material mass changes during structural evolution. This technique successfully distinguished various dehydration and transformation processes in nickel hydroxide (Ni(OH)2) samples.

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Area of Science:

  • Materials Science
  • Analytical Chemistry
  • Nanotechnology

Background:

  • Measuring heating-induced mass changes during material morphological/structural evolution is challenging.
  • Existing methods lack the resolution to correlate mass changes with specific structural transformations.
  • In situ characterization techniques are crucial for understanding dynamic material processes.

Purpose of the Study:

  • To develop a novel silicon microreactor for synchronous thermogravimetric-transmission electron microscopy (TG-TEM) analysis.
  • To enable simultaneous measurement of mass change and high-resolution imaging during heating.
  • To characterize the dehydration and phase transformation processes of nickel hydroxide (Ni(OH)2) materials.

Main Methods:

  • Integration of a self-heating resonant microcantilever for mass-change detection (TGA).
  • Incorporation of a dummy microcantilever with SiN windows for in situ TEM imaging.
  • Development of a silicon microreactor enabling TG-TEM analysis in a 100 mbar air atmosphere with Ångström-level TEM resolution.

Main Results:

  • Successfully distinguished intercalated H2O desorption and lattice OH dehydration in amorphous Ni(OH)2·xH2O nanosheets.
  • Differentiated physiosorbed water desorption, surface OH condensation, and lattice OH dehydration in single-crystal Ni(OH)2 nanosheets.
  • Identified amorphous Ni(OH)2 to polycrystalline NiO transformation at 290 °C and single-crystal Ni(OH)2 to NiO decomposition at 315 °C.

Conclusions:

  • The developed microreactor facilitates synchronous TG-TEM analysis, providing interrelated characterization.
  • This platform enables comprehensive understanding of material evolution processes by correlating mass change with structural changes.
  • The technique is effective for studying dehydration and phase transitions in nanomaterials like Ni(OH)2.