Charges on a suspended silicon nitride membrane under a high-energy electron beam

Thin silicon nitride (SiN<sub><i>x</i></sub>) membranes are widely used in gas and liquid phase transmission electron microscopy (TEM) and as phase plates to enhance imaging contrast. SiN<sub><i>x</i></sub> contains trap sites for both positive and negative charges, which can be manipulated by high-energy electron irradiation, external potential biasing, or light exposure. Charge accumulation on the membrane can significantly affect <i>in situ</i> TEM processes, including chemical and electrochemical reactions, nanoparticle dynamics, and catalytic activity, or introduce unwanted phase shifts when used as a phase plate. In this study, charge accumulation on suspended SiN<sub><i>x</i></sub> membranes was investigated using off-axis electron holography combined with model-free charge analysis, supported by custom finite element analysis (FEA) simulations. An average residual positive charge density of approximately 2.8 × 10<sup>-4</sup> C m<sup>-2</sup> was measured. Localized and stable regions of both positive and negative charges were identified on the membrane. The global positive and localized positive/negative charges give rise to strong electric fields and electroosmotic slip velocities at the membrane surface, which are sufficient to induce non-Brownian particle behavior and directional fluid flow, offering a physical explanation for previously observed anomalies in particle dynamics, nucleation, and growth during gas and liquid phase TEM experiments. These results provide a benchmark for understanding charge behavior at SiN<sub><i>x</i></sub> interfaces in gas and liquid phase TEM. Furthermore, the FEA simulations establish a framework for future investigations into charge distribution, electrostatic potentials, and electrical double layers at solid-liquid interfaces, particularly in complex geometries and chemically dynamic environments.

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Publication Details

Journal
Nanoscale
Published
2025-07-14
DOI
https://doi.org/10.1039/d5nr01742d
Primary Topic
Advanced Electron Microscopy Techniques and Applications
Type
article
Field-Weighted Citation Impact
0.00

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article

Charges on a suspended silicon nitride membrane under a high-energy electron beam

Murat Nulati Yesibolati, Nestor J. Zaluzec, Kristian Mølhave, Ole Hansen et al.
Nanoscale
Advanced Electron Microscopy Techniques and Applications
article

Charges on a suspended silicon nitride membrane under a high-energy electron beam

Murat Nulati Yesibolati, Nestor J. Zaluzec, Kristian Mølhave, Ole Hansen, Mads Søndergaard Larsen
article en

Abstract

Thin silicon nitride (SiN<sub><i>x</i></sub>) membranes are widely used in gas and liquid phase transmission electron microscopy (TEM) and as phase plates to enhance imaging contrast. SiN<sub><i>x</i></sub> contains trap sites for both positive and negative charges, which can be manipulated by high-energy electron irradiation, external potential biasing, or light exposure. Charge accumulation on the membrane can significantly affect <i>in situ</i> TEM processes, including chemical and electrochemical reactions, nanoparticle dynamics, and catalytic activity, or introduce unwanted phase shifts when used as a phase plate. In this study, charge accumulation on suspended SiN<sub><i>x</i></sub> membranes was investigated using off-axis electron holography combined with model-free charge analysis, supported by custom finite element analysis (FEA) simulations. An average residual positive charge density of approximately 2.8 × 10<sup>-4</sup> C m<sup>-2</sup> was measured. Localized and stable regions of both positive and negative charges were identified on the membrane. The global positive and localized positive/negative charges give rise to strong electric fields and electroosmotic slip velocities at the membrane surface, which are sufficient to induce non-Brownian particle behavior and directional fluid flow, offering a physical explanation for previously observed anomalies in particle dynamics, nucleation, and growth during gas and liquid phase TEM experiments. These results provide a benchmark for understanding charge behavior at SiN<sub><i>x</i></sub> interfaces in gas and liquid phase TEM. Furthermore, the FEA simulations establish a framework for future investigations into charge distribution, electrostatic potentials, and electrical double layers at solid-liquid interfaces, particularly in complex geometries and chemically dynamic environments.

NanoscaleVol. 18(2)
University of Chicago (US), Technical University of Denmark (DK)
Villum Fonden, Danmarks Tekniske Universitet, Argonne National Laboratory
Openalex Percentile: Top 94%
Advanced Electron Microscopy Techniques and Applications
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