X-ray diffraction and H-storage in ultra-small palladium particles

Narehood, D. G.; Kishore, Somasundaram Chandra; Goto, Hajime; Adair, James H.; Nelson, Jennifer; Gutiérrez, Humberto; Eklund, P. C.

doi:10.1016/j.ijhydene.2008.10.080

Cited by 118 publications

(114 citation statements)

References 12 publications

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“…An important decrease of the enthalpy of hydride formation was earlier proposed for Pd nanoparticles with size around 2.6 nm (Yamauchi et al, 2008). Moreover, a narrowing of the two-phase regions of solid solution and hydride phases and a decrease in the critical temperature of the two-phase state have been reported for ultrasmall Pd nanoparticles (Yamauchi et al, 2008;Narehood et al, 2009). Nanosizing to ultrasmall dimensions even suppresses the hydride formation, as we recently proven for the supported nanoalloy Pd90Co10 ~2.4 nm, as compared with the bulk alloy counterpart that forms a hydride phase at ambient pressure and temperature conditions (Zlotea et al, 2015c).…”

Section: Characterization Of Hydrogen Absorptionmentioning

confidence: 72%

“…The synthesis of ultrasmall noble metal-based nanoparticles supported on a porous host is well documented due to extensive study of such materials for catalysis and hydrogen sorption (Campesi et al, 2008;Narehood et al, 2009;Zlotea et al, 2010a;Contescu et al, 2011). Typically, a metal salt is used as precursor for porous host impregnation followed by a reduction step (H2, NaBH4, etc.)…”

Section: Synthesismentioning

confidence: 99%

“…Typically, a metal salt is used as precursor for porous host impregnation followed by a reduction step (H2, NaBH4, etc.) at different temperatures depending on the reducing agent (Narehood et al, 2009;Zlotea et al, 2010bZlotea et al, , 2015bEssinger-Hileman et al, 2011). For pure Pd and Rh nanoparticles, the use of high temperature, typically above 300°C, as well as high metal loadings usually induces the growth of nanoparticles size and the increase of the particle size distribution (Zhao et al, 2012;Bastide et al, 2013;Zlotea et al, 2015b).…”

Section: Synthesismentioning

confidence: 99%

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Experimental Challenges in Studying Hydrogen Absorption in Ultrasmall Metal Nanoparticles

et al. 2016

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Recent advances on synthesis, characterization, and hydrogen absorption properties of ultrasmall metal nanoparticles (defined here as objects with average size ≤3 nm) are briefly reviewed in the first part of this work. The experimental challenges encountered in performing accurate measurements of hydrogen absorption in Mg-and noble metal-based ultrasmall nanoparticles are addressed. The second part of this work reports original results obtained for ultrasmall bulk-immiscible Pd-Rh nanoparticles. Carbonsupported Pd-Rh nanoalloys in the whole binary chemical composition range have been successfully prepared by liquid impregnation method followed by reduction at 300°C. EXAFS investigations suggested that the local structure of these nanoalloys is partially segregated into Rh-rich core and Pd-rich surface coexisting within the same nanoparticles. Downsizing to ultrasmall dimensions completely suppresses the hydride formation in Pd-rich nanoalloys at ambient conditions, contrary to bulk and larger nanosized (5-6 nm) counterparts. The ultrasmall Pd90Rh10 nanoalloy can absorb hydrogen-forming solid solutions under these conditions, as suggested by in situ X-ray diffraction (XRD). Apart from this composition, common laboratory techniques, such as in situ XRD, DSC, and PCI, failed to clarify the hydrogen interaction mechanism: either adsorption on developed surfaces or both adsorption and absorption with formation of solid solutions. Concluding insights were brought by in situ EXAFS experiments at synchrotron: ultrasmall Pd75Rh25 and Pd50Rh50 nanoalloys absorb hydrogen-forming solid solutions at ambient conditions. Moreover, the hydrogen solubility in these solid solutions is higher with increasing Pd content, and this trend can be understood in terms of hydrogen preferential occupation in the Pd-rich regions, as suggested by in situ EXAFS. The Rh-rich nanoalloys (Pd25Rh75 and Pd10Rh90) only adsorb hydrogen on the developed surface of ultrasmall nanoparticles. In summary, in situ characterization techniques carried out at large-scale facilities are unique and powerful tools for in-depth investigation of hydrogen interaction with ultrasmall nanoparticles at local level.

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Section: Characterization Of Hydrogen Absorptionmentioning

confidence: 72%

Section: Synthesismentioning

confidence: 99%

Section: Synthesismentioning

confidence: 99%

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Experimental Challenges in Studying Hydrogen Absorption in Ultrasmall Metal Nanoparticles

et al. 2016

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“…Hydrogen insertion can be also achieved electrochemically from aqueous electrolyte by application of a suitably cathodic potential as shown for Pd theoretically [6,7] and practically in alkaline [8][9][10][11][12][13] and acidic electrolyte [14,15]. The simplicity of hydrogen uptake makes Pd a promising candidate for hydrogen storage [16][17][18][19], for example as catalyst for hydrogen uptake and removal in other hydride forming metals [20]. Its properties enable also application as membrane for hydrogen purification [21][22][23].…”

Section: Introductionmentioning

confidence: 99%

“…Formation of the β-phase leads to change in several material properties such as decrease in electrical conductivity [28] and volume expansion of the Pd metal lattice [29]. On the one hand, this change in properties is the basis for hydrogen sensing [30][31][32], but on the other hand, it leads to drawbacks like hydrogen embrittlement [16,[33][34][35]. Based on the work of the Rohwerder group [36][37][38][39], Pd was introduced for sensing hydrogen in metals with Kelvin probe (KP) technique.…”

Section: Introductionmentioning

confidence: 99%

Influence of atmospheric oxygen on hydrogen detection on Pd using Kelvin probe technique

Schimo

Burgstaller

Hassel

2017

J Solid State Electrochem

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Influence of oxygen concentration in the measurement atmosphere on detection of hydrogen using Kelvin probe was studied. The studied material was a 100-μm-thick palladium foil, which was mounted in a 3D printed electrochemical flow cell. The used setup enables hydrogen loading with in-situ contact potential measurement of the hydrogen exit side of the Pd electrode. The hydrogen loading and unloading procedure, including insertion of different amounts of hydrogen into the Pd membrane and recording resulting values of contact potential difference, was performed at distinct oxygen concentrations ranging between 1 and 80 vol%. An increasing amount of oxygen in the atmosphere surrounding the hydrogen-loaded Pd electrode resulted in an accelerated removal of hydrogen from the Pd. The kinetics of this reaction was studied based on Kelvin probe measurements, and a reaction mechanism is discussed.

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Electrochemical Hydrogen Evolution Reaction

Zhao¹,

Sun²

2022

Photo‐ and Electro‐Catalytic Processes

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X-ray diffraction and H-storage in ultra-small palladium particles

Cited by 118 publications

References 12 publications

Experimental Challenges in Studying Hydrogen Absorption in Ultrasmall Metal Nanoparticles

Experimental Challenges in Studying Hydrogen Absorption in Ultrasmall Metal Nanoparticles

Influence of atmospheric oxygen on hydrogen detection on Pd using Kelvin probe technique

Electrochemical Hydrogen Evolution Reaction

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