Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy

Hanglong Wu; Hao Su; Rick R.M. Joosten; Arthur D.A. Keizer; Laura S. van Hazendonk; Maarten J.M. Wirix; Joseph P. Patterson; Jozua Laven; Gijsbertus de With; Heiner Friedrich

doi:10.1002/smtd.202001287

Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy

Hanglong Wu
, Hao Su
, Rick R.M. Joosten
, Arthur D.A. Keizer
, Laura S. van Hazendonk
, Maarten J.M. Wirix
, Joseph P. Patterson
, Jozua Laven
, Gijsbertus de With
, Heiner Friedrich (Corresponding author)

Research output: Contribution to journal › Article › Academic › peer-review

41 Citations (Scopus)

252 Downloads (Pure)

Abstract

Liquid-Phase (Scanning) Transmission Electron Microscopy (LP-(S)TEM) has become an essential technique to monitor nanoscale materials processes in liquids in real-time. Due to the pressure difference between the liquid and the microscope vacuum, bending of the silicon nitride (SiN_x) membrane windows generally occurs. This causes a spatially varying liquid layer thickness that makes interpretation of LP-(S)TEM results difficult due to a locally varying achievable resolution and diffusion limitations. To mediate these difficulties, it is shown: 1) how to quantitatively map liquid layer thickness for any liquid at less than 0.01 e⁻ Å⁻² total dose; 2) how to dynamically modulate the liquid thickness by tuning the internal pressure in the liquid cell, co-determined by the Laplace pressure and the external pressure. It is demonstrated that reproducible inward bulging of the window membranes can be realized, leading to an ultra-thin liquid layer in the central window area for high-resolution imaging. Furthermore, it is shown that the liquid thickness can be dynamically altered in a programmed way, thereby potentially overcoming the diffusion limitations towards achieving bulk solution conditions. The presented approaches provide essential ways to measure and dynamically adjust liquid thickness in LP-(S)TEM experiments, enabling new experiment designs and better control of solution chemistry.

Original language	English
Article number	2001287
Number of pages	9
Journal	Small Methods
Volume	5
Issue number	6
DOIs	https://doi.org/10.1002/smtd.202001287
Publication status	Published - 15 Jun 2021

Bibliographical note

Funding Information:
H.W. and H.S. contributed equally to this work. The authors gratefully acknowledge Shell Global Solutions and the Dutch Research Council (NWO) for funding H.S. through the CHIPP program. H.W. was supported by the EU H2020 Marie Sklodowska‐Curie Action project “MULTIMAT” (676045). The authors thank Dr. Remco Fijneman and Jason Heinrichs (Eindhoven University of Technology) for the assistance with the slow evaporation experiments, and Joeri Opdam (Eindhoven University of Technology) for beneficial discussions and the help with creating 3D liquid cell images.

Publisher Copyright:
© 2021 The Authors. Small Methods published by Wiley-VCH GmbH

Copyright:
Copyright 2021 Elsevier B.V., All rights reserved.

Funding

H.W. and H.S. contributed equally to this work. The authors gratefully acknowledge Shell Global Solutions and the Dutch Research Council (NWO) for funding H.S. through the CHIPP program. H.W. was supported by the EU H2020 Marie Sklodowska‐Curie Action project “MULTIMAT” (676045). The authors thank Dr. Remco Fijneman and Jason Heinrichs (Eindhoven University of Technology) for the assistance with the slow evaporation experiments, and Joeri Opdam (Eindhoven University of Technology) for beneficial discussions and the help with creating 3D liquid cell images.

Funders	Funder number
Marie Skłodowska‐Curie
Shell Global Solutions B.V.
European Union's Horizon 2020 - Research and Innovation Framework Programme
Marie Skłodowska‐Curie	676045
Eindhoven University of Technology
Nederlandse Organisatie voor Wetenschappelijk Onderzoek

Keywords

(scanning) transmission electron microscopy
dynamic thickness control
liquid-phase
thickness maps

Access to Document

10.1002/smtd.202001287

published versionFinal published version, 1.49 MB

Cite this

@article{156bdafde46c4f30baa798e20f735b99,

title = "Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy",

abstract = "Liquid-Phase (Scanning) Transmission Electron Microscopy (LP-(S)TEM) has become an essential technique to monitor nanoscale materials processes in liquids in real-time. Due to the pressure difference between the liquid and the microscope vacuum, bending of the silicon nitride (SiNx) membrane windows generally occurs. This causes a spatially varying liquid layer thickness that makes interpretation of LP-(S)TEM results difficult due to a locally varying achievable resolution and diffusion limitations. To mediate these difficulties, it is shown: 1) how to quantitatively map liquid layer thickness for any liquid at less than 0.01 e− {\AA}−2 total dose; 2) how to dynamically modulate the liquid thickness by tuning the internal pressure in the liquid cell, co-determined by the Laplace pressure and the external pressure. It is demonstrated that reproducible inward bulging of the window membranes can be realized, leading to an ultra-thin liquid layer in the central window area for high-resolution imaging. Furthermore, it is shown that the liquid thickness can be dynamically altered in a programmed way, thereby potentially overcoming the diffusion limitations towards achieving bulk solution conditions. The presented approaches provide essential ways to measure and dynamically adjust liquid thickness in LP-(S)TEM experiments, enabling new experiment designs and better control of solution chemistry.",

keywords = "(scanning) transmission electron microscopy, dynamic thickness control, liquid-phase, thickness maps",

author = "Hanglong Wu and Hao Su and Joosten, \{Rick R.M.\} and Keizer, \{Arthur D.A.\} and \{van Hazendonk\}, \{Laura S.\} and Wirix, \{Maarten J.M.\} and Patterson, \{Joseph P.\} and Jozua Laven and \{de With\}, Gijsbertus and Heiner Friedrich",

note = "Funding Information: H.W. and H.S. contributed equally to this work. The authors gratefully acknowledge Shell Global Solutions and the Dutch Research Council (NWO) for funding H.S. through the CHIPP program. H.W. was supported by the EU H2020 Marie Sklodowska‐Curie Action project {\textquotedblleft}MULTIMAT{\textquotedblright} (676045). The authors thank Dr. Remco Fijneman and Jason Heinrichs (Eindhoven University of Technology) for the assistance with the slow evaporation experiments, and Joeri Opdam (Eindhoven University of Technology) for beneficial discussions and the help with creating 3D liquid cell images. Publisher Copyright: {\textcopyright} 2021 The Authors. Small Methods published by Wiley-VCH GmbH Copyright: Copyright 2021 Elsevier B.V., All rights reserved.",

year = "2021",

month = jun,

day = "15",

doi = "10.1002/smtd.202001287",

language = "English",

volume = "5",

journal = "Small Methods",

issn = "2366-9608",

publisher = "Wiley",

number = "6",

}

TY - JOUR

T1 - Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy

AU - Wu, Hanglong

AU - Su, Hao

AU - Joosten, Rick R.M.

AU - Keizer, Arthur D.A.

AU - van Hazendonk, Laura S.

AU - Wirix, Maarten J.M.

AU - Patterson, Joseph P.

AU - Laven, Jozua

AU - de With, Gijsbertus

AU - Friedrich, Heiner

N1 - Funding Information: H.W. and H.S. contributed equally to this work. The authors gratefully acknowledge Shell Global Solutions and the Dutch Research Council (NWO) for funding H.S. through the CHIPP program. H.W. was supported by the EU H2020 Marie Sklodowska‐Curie Action project “MULTIMAT” (676045). The authors thank Dr. Remco Fijneman and Jason Heinrichs (Eindhoven University of Technology) for the assistance with the slow evaporation experiments, and Joeri Opdam (Eindhoven University of Technology) for beneficial discussions and the help with creating 3D liquid cell images. Publisher Copyright: © 2021 The Authors. Small Methods published by Wiley-VCH GmbH Copyright: Copyright 2021 Elsevier B.V., All rights reserved.

PY - 2021/6/15

Y1 - 2021/6/15

N2 - Liquid-Phase (Scanning) Transmission Electron Microscopy (LP-(S)TEM) has become an essential technique to monitor nanoscale materials processes in liquids in real-time. Due to the pressure difference between the liquid and the microscope vacuum, bending of the silicon nitride (SiNx) membrane windows generally occurs. This causes a spatially varying liquid layer thickness that makes interpretation of LP-(S)TEM results difficult due to a locally varying achievable resolution and diffusion limitations. To mediate these difficulties, it is shown: 1) how to quantitatively map liquid layer thickness for any liquid at less than 0.01 e− Å−2 total dose; 2) how to dynamically modulate the liquid thickness by tuning the internal pressure in the liquid cell, co-determined by the Laplace pressure and the external pressure. It is demonstrated that reproducible inward bulging of the window membranes can be realized, leading to an ultra-thin liquid layer in the central window area for high-resolution imaging. Furthermore, it is shown that the liquid thickness can be dynamically altered in a programmed way, thereby potentially overcoming the diffusion limitations towards achieving bulk solution conditions. The presented approaches provide essential ways to measure and dynamically adjust liquid thickness in LP-(S)TEM experiments, enabling new experiment designs and better control of solution chemistry.

AB - Liquid-Phase (Scanning) Transmission Electron Microscopy (LP-(S)TEM) has become an essential technique to monitor nanoscale materials processes in liquids in real-time. Due to the pressure difference between the liquid and the microscope vacuum, bending of the silicon nitride (SiNx) membrane windows generally occurs. This causes a spatially varying liquid layer thickness that makes interpretation of LP-(S)TEM results difficult due to a locally varying achievable resolution and diffusion limitations. To mediate these difficulties, it is shown: 1) how to quantitatively map liquid layer thickness for any liquid at less than 0.01 e− Å−2 total dose; 2) how to dynamically modulate the liquid thickness by tuning the internal pressure in the liquid cell, co-determined by the Laplace pressure and the external pressure. It is demonstrated that reproducible inward bulging of the window membranes can be realized, leading to an ultra-thin liquid layer in the central window area for high-resolution imaging. Furthermore, it is shown that the liquid thickness can be dynamically altered in a programmed way, thereby potentially overcoming the diffusion limitations towards achieving bulk solution conditions. The presented approaches provide essential ways to measure and dynamically adjust liquid thickness in LP-(S)TEM experiments, enabling new experiment designs and better control of solution chemistry.

KW - (scanning) transmission electron microscopy

KW - dynamic thickness control

KW - liquid-phase

KW - thickness maps

UR - https://www.scopus.com/pages/publications/85105112187

U2 - 10.1002/smtd.202001287

DO - 10.1002/smtd.202001287

M3 - Article

C2 - 34927906

AN - SCOPUS:85105112187

SN - 2366-9608

VL - 5

JO - Small Methods

JF - Small Methods

IS - 6

M1 - 2001287

ER -

Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy

Abstract

Bibliographical note

Funding

Keywords

Access to Document

Other files and links

Fingerprint

Center for Multiscale Electron Microscopy (CMEM)

Cite this

Mapping and Controlling Liquid Layer Thickness in Liquid-Phase (Scanning) Transmission Electron Microscopy

Abstract

Bibliographical note

Funding

Keywords

Access to Document

Other files and links

Fingerprint

Equipment

Center for Multiscale Electron Microscopy (CMEM)

Cite this