Aerosol synthesis and Rietveld analysis of tetragonal (β1) PdZn

Eric J. Peterson; Barr Halevi; Boris Kiefer; Michael N. Spilde; Abhaya K. Datye; Joe Peterson; Luc Daemen; Anna Llobet; Heinz Nakotte

doi:10.1016/j.jallcom.2010.09.149

Aerosol synthesis and Rietveld analysis of tetragonal (β₁) PdZn

Eric J. Peterson, Barr Halevi, Boris Kiefer, Michael N. Spilde, Abhaya K. Datye, Joe Peterson, Luc Daemen, Anna Llobet, Heinz Nakotte

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

17 Scopus citations

Abstract

The β₁ PdZn intermetallic of nominal 50:50 Pd:Zn at% was synthesized using an aerosol method. The aerosol method provided atomically mixed precursor oxy-nitrate powder that was then reduced to form β₁ PdZn, having a surface area amenable to catalytic measurements. Formation of the β₁ PdZn during reduction was found to occur rapidly (4 h) and at moderate temperature (500 °C), serving to minimize the loss of volatile Zn. Chemical and structural characterization confirms that β₁ PdZn (95-99 wt% phase pure) of the same composition as the nitrate feedstock solution can be prepared using this method. Detailed structural analysis shows that this material contains little or no vacancies and minimal Pd/Zn disorder.

Original language	English
Pages (from-to)	1463-1470
Number of pages	8
Journal	Journal of Alloys and Compounds
Volume	509
Issue number	5
DOIs	https://doi.org/10.1016/j.jallcom.2010.09.149
State	Published - Feb 3 2011
Externally published	Yes

Funding

Financial support for this work was provided by the US Department of Energy , Grant DE-FG02-05ER15712 . Additional support was provided by the US Department of Energy, EPSCoR Grant DE-FG02-08ER46530 . We gratefully acknowledge computing resources provided by the New Mexico Computing Applications Center (NMCAC) on Encanto. A portion of the research was performed using EMSL, a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory.

Funders	Funder number
Office of Biological and Environmental Research
US Department of Energy	DE-FG02-05ER15712
U.S. Department of Energy
Office of Experimental Program to Stimulate Competitive Research	DE-FG02-08ER46530
Pacific Northwest National Laboratory

Keywords

Catalysis
Crystal structure
Diffraction
Intermetallics
Neutron
Order-disorder effects
PdZn
Phase diagrams
SEM
Scanning electron microscopy
Thermal analysis
Transition metal alloys and compounds
X-ray diffraction

Access to Document

10.1016/j.jallcom.2010.09.149

Cite this

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title = "Aerosol synthesis and Rietveld analysis of tetragonal (β1) PdZn",

abstract = "The β1 PdZn intermetallic of nominal 50:50 Pd:Zn at% was synthesized using an aerosol method. The aerosol method provided atomically mixed precursor oxy-nitrate powder that was then reduced to form β1 PdZn, having a surface area amenable to catalytic measurements. Formation of the β1 PdZn during reduction was found to occur rapidly (4 h) and at moderate temperature (500 °C), serving to minimize the loss of volatile Zn. Chemical and structural characterization confirms that β1 PdZn (95-99 wt% phase pure) of the same composition as the nitrate feedstock solution can be prepared using this method. Detailed structural analysis shows that this material contains little or no vacancies and minimal Pd/Zn disorder.",

keywords = "Catalysis, Crystal structure, Diffraction, Intermetallics, Neutron, Order-disorder effects, PdZn, Phase diagrams, SEM, Scanning electron microscopy, Thermal analysis, Transition metal alloys and compounds, X-ray diffraction",

author = "Peterson, {Eric J.} and Barr Halevi and Boris Kiefer and Spilde, {Michael N.} and Datye, {Abhaya K.} and Joe Peterson and Luc Daemen and Anna Llobet and Heinz Nakotte",

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AU - Peterson, Eric J.

AU - Halevi, Barr

AU - Kiefer, Boris

AU - Spilde, Michael N.

AU - Datye, Abhaya K.

AU - Peterson, Joe

AU - Daemen, Luc

AU - Llobet, Anna

AU - Nakotte, Heinz

PY - 2011/2/3

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N2 - The β1 PdZn intermetallic of nominal 50:50 Pd:Zn at% was synthesized using an aerosol method. The aerosol method provided atomically mixed precursor oxy-nitrate powder that was then reduced to form β1 PdZn, having a surface area amenable to catalytic measurements. Formation of the β1 PdZn during reduction was found to occur rapidly (4 h) and at moderate temperature (500 °C), serving to minimize the loss of volatile Zn. Chemical and structural characterization confirms that β1 PdZn (95-99 wt% phase pure) of the same composition as the nitrate feedstock solution can be prepared using this method. Detailed structural analysis shows that this material contains little or no vacancies and minimal Pd/Zn disorder.

AB - The β1 PdZn intermetallic of nominal 50:50 Pd:Zn at% was synthesized using an aerosol method. The aerosol method provided atomically mixed precursor oxy-nitrate powder that was then reduced to form β1 PdZn, having a surface area amenable to catalytic measurements. Formation of the β1 PdZn during reduction was found to occur rapidly (4 h) and at moderate temperature (500 °C), serving to minimize the loss of volatile Zn. Chemical and structural characterization confirms that β1 PdZn (95-99 wt% phase pure) of the same composition as the nitrate feedstock solution can be prepared using this method. Detailed structural analysis shows that this material contains little or no vacancies and minimal Pd/Zn disorder.

KW - Catalysis

KW - Crystal structure

KW - Diffraction

KW - Intermetallics

KW - Neutron

KW - Order-disorder effects

KW - PdZn

KW - Phase diagrams

KW - SEM

KW - Scanning electron microscopy

KW - Thermal analysis

KW - Transition metal alloys and compounds

KW - X-ray diffraction

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