Cross-sectional observation of nanostructured catalyst layer of polymer electrolyte fuel cell using FIB/SEM

Katayanagi, Yuta; Shimizu, Takahiro; Hashimasa, Yoshiyuki; Matsushita, Nobuhiro; Yamazaki, Yohtaro; Yamaguchi, Takeo

doi:10.1016/j.jpowsour.2015.01.085

Cited by 25 publications

(15 citation statements)

References 12 publications

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“…is methodology has been demonstrated by studies of various hierarchical porous materials, such as, zeolite beads [27], silicon [53], monolithic UiO-66-NH2 material [54], and concrete [46]. e curtain effect may occur in the milling process, which appears as parallel scratches varying in the same direction of ion beam milling and making the image appears to be covered by a semitransparent curtain [27,55,56]. e potential reasons are as follows: (1) roughness of the slicing surface varies the angles of the ion beam and causes the differences of the milling rate, and depositing protection layers may mitigate the surface roughness; (2) different characteristics of the elements in the targeting materials can cause curtain effect as well; (3) presence of internal pores in the samples can change the intensity or pathway of ion beam when it passes through the pores.…”

Section: Potential Applications Of Fib-sem 3d Tomography In Carbon-bamentioning

confidence: 99%

“…e algorithm tools for quantification analysis are lab-made MATLAB [58] and Java [59]. e existing reported studies that used the FIB-SEM quantitative 3D reconstruction are porous carbon-based electrode [54], carbon nanofiber based supercapacitor [49], and mesoporous carbon electrode material [56].…”

Section: Carbon-based Electrodesmentioning

confidence: 99%

“…e FIB-SEM 3D tomography technique is a useful method for the diagnosis of the catalyst [56,60], coating [61], or hybrid [31] layer structure as well. It can reconstruct the geometrical properties of the catalyst layer in 3D space.…”

Section: Carbon-based Catalyst/coating/hybrid Layersmentioning

confidence: 99%

“…It can thermally damage the catalyst layer(s). e liquid nitrogen cooling and thermoelectric cooling via Peltier elements methods have been demonstrated and proved that they can mitigate the heating damage [56]. e thermoelectric cooling is considered to exceed the liquid nitrogen cooling since the thermoelectric cooling enables a short-time sample fabrication at the FIB stage.…”

Section: Carbon-based Catalyst/coating/hybrid Layersmentioning

confidence: 99%

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FIB-SEM Three-Dimensional Tomography for Characterization of Carbon-Based Materials

Nan

Wang

2019

Advances in Materials Science and Engineering

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A review on the recent advances of the three-dimensional (3D) characterization of carbon-based materials was conducted by focused ion beam-scanning electron microscope (FIB-SEM) tomography. Current studies and further potential applications of the FIB-SEM 3D tomography technique for carbon-based materials were discussed. The goal of this paper is to highlight the advances of FIB-SEM 3D reconstruction to reveal the high and accurate resolution of internal structures of carbon-based materials and provide suggestions for the adoption and improvement of the FIB-SEM tomography system for a broad carbon-based research to achieve the best examination performances and enhance the development of innovative carbon-based materials.

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Section: Potential Applications Of Fib-sem 3d Tomography In Carbon-bamentioning

confidence: 99%

Section: Carbon-based Electrodesmentioning

confidence: 99%

Section: Carbon-based Catalyst/coating/hybrid Layersmentioning

confidence: 99%

Section: Carbon-based Catalyst/coating/hybrid Layersmentioning

confidence: 99%

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FIB-SEM Three-Dimensional Tomography for Characterization of Carbon-Based Materials

Nan

Wang

2019

Advances in Materials Science and Engineering

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“…[2][3][4][5][6][7][8][9] The diamond blade used in the microtome technique has the advantage of slicing through the electrocatalyst layer without inflicting thermal damage. However, it is difficult to cut through e.g.…”

mentioning

confidence: 99%

Correlating Cathode Microstructure with PEFC Performance Using FIB-SEM and TEM

Okumura

Noda

Matsuda

et al. 2017

J. Electrochem. Soc.

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The cathode electrocatalyst layers of polymer electrolyte membrane fuel cells (PEFCs) are quantitatively investigated for different ratios of Nafion ionomer. This is achieved using focused-ion-beam coupled scanning electron microscopy (FIB-SEM) to reconstruct the three-dimensional microstructure via tomography. Parameters such as the porosity and pore size distribution were calculated from this data. The distributions of Nafion ionomer, carbon support, and platinum nanoparticles were then further clarified using transmission electron microscopy (TEM). Changes in the PEFC performance (notably the I-V characteristics, the electrochemical surface area, the activation overvoltage, and the concentration overvoltage) are thus correlated to electrode microstructure. The electrocatalyst layers of PEFCs have complicated, threedimensional (3D) porous microstructure. This microstructure plays a key role in transporting reactant gases (i.e. hydrogen and oxygen), product water vapor, charge-carrying ions, and electrons either to or from the active sites. Therefore, the overall PEFC performance is linked inextricably to the 3D microstructure of the electrocatalyst layer, and in particular to the Nafion content.1 Making quantitative correlations between the Nafion ratio, the microstructure, and the cell performance is thus essential in order to optimize the performance and efficiency of PEFCs.The microstructure of electrocatalyst layers in PEFCs is generally studied by obtaining microtome sections, or by using focused-ionbeam (FIB) techniques.2-9 The diamond blade used in the microtome technique has the advantage of slicing through the electrocatalyst layer without inflicting thermal damage. However, it is difficult to cut through e.g. individual carbon particles using this method, meaning that the resulting cross-section is typically too rough to analyze the microstructure quantitatively.2 Meanwhile, clear and well-defined cross-sections can be obtained by FIB sectioning. However, in this case there remain difficulties in quantitative observation due to thermal damage and ion damage during the sputtering process, in which the gallium ion beam generates heat locally, melting or damaging the ionomer. This can be mitigated somewhat by cooling the sample using liquid nitrogen, as described by e.g. Katayanagi et al. 2,9Electron microscopy and X-ray computed tomography (CT) are two other common methods to observe electrocatalyst layers in PEFCs. For example, Wargo et al. observed electrocatalyst layers using both nano-CT and FIB-SEM techniques, 3 whilst Litster et al. observed electrocatalyst layers using high-resolution (50 nm) nano-CT. 4 Despite CT having the distinct advantage of being a non-destructive technique, it has the disadvantage of inferior resolution compared with SEM, TEM, or scanning transmission electron microscope (STEM).Therefore, in this study we focus on sectioning samples by FIB, and performing observation using electron microscopy. FIB-SEM has already been utilized as a powerful tool to observe the microstruct...

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Power Density and Durability in Fuel Cell Vehicles

Heidary¹,

Moein‐Jahromi²

2023

Hydrogen Electrical Vehicles

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Cross-sectional observation of nanostructured catalyst layer of polymer electrolyte fuel cell using FIB/SEM

Cited by 25 publications

References 12 publications

FIB-SEM Three-Dimensional Tomography for Characterization of Carbon-Based Materials

FIB-SEM Three-Dimensional Tomography for Characterization of Carbon-Based Materials

Correlating Cathode Microstructure with PEFC Performance Using FIB-SEM and TEM

Power Density and Durability in Fuel Cell Vehicles

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