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In-situ TEM on (de)hydrogenation of Pd at 0.5¿4.5 bar hydrogen pressure and 20¿400°C. / Yokosawa, T; Alan, T; Pandraud, G; Dam, B; Zandbergen, HW.

In: Ultramicroscopy, Vol. 112, No. 1, 2012, p. 47-52.

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@article{588022a73501478dafa5fad6ca158931,
title = "In-situ TEM on (de)hydrogenation of Pd at 0.5¿4.5 bar hydrogen pressure and 20¿400°C",
abstract = "We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 9.5 bar. The Pd film consisted of islands being 15 nm thick and 50-500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10-16 degrees C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5-4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale.",
keywords = "academic journal papers",
author = "T Yokosawa and T Alan and G Pandraud and B Dam and HW Zandbergen",
year = "2012",
doi = "10.1016/j.ultramic.2011.10.010",
language = "English",
volume = "112",
pages = "47--52",
journal = "Ultramicroscopy",
issn = "0304-3991",
publisher = "Elsevier",
number = "1",

}

RIS

TY - JOUR

T1 - In-situ TEM on (de)hydrogenation of Pd at 0.5¿4.5 bar hydrogen pressure and 20¿400°C

AU - Yokosawa, T

AU - Alan, T

AU - Pandraud, G

AU - Dam, B

AU - Zandbergen, HW

PY - 2012

Y1 - 2012

N2 - We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 9.5 bar. The Pd film consisted of islands being 15 nm thick and 50-500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10-16 degrees C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5-4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale.

AB - We have developed a nanoreactor, sample holder and gas system for in-situ transmission electron microscopy (TEM) of hydrogen storage materials up to at least 4.5 bar. The MEMS-based nanoreactor has a microheater, two electron-transparent windows and a gas inlet and outlet. The holder contains various O-rings to have leak-tight connections with the nanoreactor. The system was tested with the (de)hydrogenation of Pd at pressures up to 9.5 bar. The Pd film consisted of islands being 15 nm thick and 50-500 nm wide. In electron diffraction mode we observed reproducibly a crystal lattice expansion and shrinkage owing to hydrogenation and dehydrogenation, respectively. In selected-area electron diffraction and bright/dark-field modes the (de)hydrogenation of individual Pd particles was followed. Some Pd islands are consistently hydrogenated faster than others. When thermally cycled, thermal hysteresis of about 10-16 degrees C between hydrogen absorption and desorption was observed for hydrogen pressures of 0.5-4.5 bar. Experiments at 0.8 bar and 3.2 bar showed that the (de)hydrogenation temperature is not affected by the electron beam. This result shows that this is a fast method to investigate hydrogen storage materials with information at the nanometer scale.

KW - academic journal papers

U2 - 10.1016/j.ultramic.2011.10.010

DO - 10.1016/j.ultramic.2011.10.010

M3 - Article

VL - 112

SP - 47

EP - 52

JO - Ultramicroscopy

JF - Ultramicroscopy

SN - 0304-3991

IS - 1

ER -

ID: 2795818