Reciprocal-space and real-space neutron investigation of nanostructured Mo2C and WC

Katharine Page; Jun Li; Robert Savinelli; Holly N. Szumila; Jinping Zhang; Judith K. Stalick; Thomas Proffen; Susannah L. Scott; Ram Seshadri

doi:10.1016/j.solidstatesciences.2008.03.018

Reciprocal-space and real-space neutron investigation of nanostructured Mo₂C and WC

Katharine Page, Jun Li, Robert Savinelli, Holly N. Szumila, Jinping Zhang, Judith K. Stalick, Thomas Proffen, Susannah L. Scott, Ram Seshadri

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

54 Scopus citations

Abstract

As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo₂C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH₄)₆Mo₇O₂₄·4H₂O] and ammonium paratungstate [(NH₄)₁₀W₁₂O₄₁·5H₂O] in flowing 50%CH₄/50%H₂. Surface areas as high as 52 m²/g for Mo₂C and 24 m²/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.

Original language	English
Pages (from-to)	1499-1510
Number of pages	12
Journal	Solid State Sciences
Volume	10
Issue number	11
DOIs	https://doi.org/10.1016/j.solidstatesciences.2008.03.018
State	Published - Nov 2008
Externally published	Yes

Funding

This work has been supported by the Department of Energy, (DOE) Office of Basic Energy Sciences (BES) through grant DE-FG02-05ER15025. KP and HNS were supported by the National Science Foundation through a Graduate Research Fellowship and through an Undergraduate Internship (RISE Program), respectively. The work at UCSB made use of facilities of the Materials Research Laboratory, supported by the NSF (DMR05-20415). We acknowledge the support of the National Institute of Standards and Technology, U.S. Department of Commerce, in providing the neutron research facilities. This work benefited from the use of the Lujan Center at Los Alamos Neutron Science Center, funded by the Department of Energy, Office of Basic Energy Sciences. The upgrade of NPDF was funded by the National Science Foundation through grant DMR00-76488.

Funders	Funder number
Office of Basic Energy Sciences	DMR00-76488
National Science Foundation	DMR05-20415
U.S. Department of Energy
National Institute of Standards and Technology
U.S. Department of Commerce
Basic Energy Sciences	DE-FG02-05ER15025

Keywords

Metal carbides
Nanostructures
Neutron diffraction
Pair-distribution function method

Access to Document

10.1016/j.solidstatesciences.2008.03.018

Cite this

@article{1949c45823a149119449429c1664f428,

title = "Reciprocal-space and real-space neutron investigation of nanostructured Mo2C and WC",

abstract = "As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo2C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH4)6Mo7O24·4H2O] and ammonium paratungstate [(NH4)10W12O41·5H2O] in flowing 50%CH4/50%H2. Surface areas as high as 52 m2/g for Mo2C and 24 m2/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.",

keywords = "Metal carbides, Nanostructures, Neutron diffraction, Pair-distribution function method",

author = "Katharine Page and Jun Li and Robert Savinelli and Szumila, {Holly N.} and Jinping Zhang and Stalick, {Judith K.} and Thomas Proffen and Scott, {Susannah L.} and Ram Seshadri",

year = "2008",

month = nov,

doi = "10.1016/j.solidstatesciences.2008.03.018",

language = "English",

volume = "10",

pages = "1499--1510",

journal = "Solid State Sciences",

issn = "1293-2558",

publisher = "Elsevier",

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T1 - Reciprocal-space and real-space neutron investigation of nanostructured Mo2C and WC

AU - Page, Katharine

AU - Li, Jun

AU - Savinelli, Robert

AU - Szumila, Holly N.

AU - Zhang, Jinping

AU - Stalick, Judith K.

AU - Proffen, Thomas

AU - Scott, Susannah L.

AU - Seshadri, Ram

PY - 2008/11

Y1 - 2008/11

N2 - As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo2C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH4)6Mo7O24·4H2O] and ammonium paratungstate [(NH4)10W12O41·5H2O] in flowing 50%CH4/50%H2. Surface areas as high as 52 m2/g for Mo2C and 24 m2/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.

AB - As possible substitute materials for platinum group metal heterogeneous catalysts, high surface area carbides of the early transition metals Mo and W are of great interest. Here we report nanostructured, high surface area Mo2C and WC prepared by decomposing and carburizing ammonium paramolybdate [(NH4)6Mo7O24·4H2O] and ammonium paratungstate [(NH4)10W12O41·5H2O] in flowing 50%CH4/50%H2. Surface areas as high as 52 m2/g for Mo2C and 24 m2/g for WC were obtained, with both structures crystallizing in structures appropriate for catalytic activity. We have studied these materials using a combination of neutron diffraction Rietveld refinement, X-ray photoelectron spectroscopy, surface area measurements, and scanning transmission electron microscopy. In addition, we have used pair-distribution function (PDF) analysis of the neutron total scattering data as a means of establishing the presence of graphitic carbon in the as-prepared materials.

KW - Metal carbides

KW - Nanostructures

KW - Neutron diffraction

KW - Pair-distribution function method

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