The pathway for vanadium nitride (VN) formation obtained by milling treatment has been traced out. At the initial stages of the process, the reactant, vanadium metal, showing body-centered cubic (bcc) structure, becomes highly distorted. Simultaneously, the formation of a small nucleus of the product, VN, takes place. X-ray absorption spectroscopy (XAS) has allowed the quantification of the distortion degree as well as the detection of the VN nucleus in the early stages of their formation, while other standard structural characterization techniques are unable to detect such phenomena. For increasing milling times, apart from the expected increase in the size of the VN nucleus, a polymorphic transformation from bcc to fcc vanadium metal has been recorded. This phase might play a key role in the overall synthesis process and could be a reaction intermediate in other solid state processes involving V metal. The sensitivity of XAS to noncrystalline domains and to highly distorted environments, as well as the use of high resolution x-ray diffraction, has provided the relevant information to understand the whole reaction process.
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15 July 2008
Research Article|
July 23 2008
Polymorphic transformation from body-centered to face-centered cubic vanadium metal during mechanosynthesis of nanostructured vanadium nitride determined by extended x-ray absorption fine structure spectroscopy
Víctor López-Flores;
Víctor López-Flores
1Institute of Materials Science of Seville, Inorganic Chemistry Department, CSIC,
University of Seville
, Av. Americo Vespucio, No. 49, 41092 Seville, Spain
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Manuel A. Roldán;
Manuel A. Roldán
1Institute of Materials Science of Seville, Inorganic Chemistry Department, CSIC,
University of Seville
, Av. Americo Vespucio, No. 49, 41092 Seville, Spain
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Concepción Real;
Concepción Real
1Institute of Materials Science of Seville, Inorganic Chemistry Department, CSIC,
University of Seville
, Av. Americo Vespucio, No. 49, 41092 Seville, Spain
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Adela Muñoz Páez;
Adela Muñoz Páez
a)
1Institute of Materials Science of Seville, Inorganic Chemistry Department, CSIC,
University of Seville
, Av. Americo Vespucio, No. 49, 41092 Seville, Spain
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Germán R. Castro
Germán R. Castro
2
SpLine CRG at the European Synchrotron Radiation Facility
, BP220, F-38043 Grenoble Cedex, France
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Víctor López-Flores
1
Manuel A. Roldán
1
Concepción Real
1
Adela Muñoz Páez
1,a)
Germán R. Castro
2
1Institute of Materials Science of Seville, Inorganic Chemistry Department, CSIC,
University of Seville
, Av. Americo Vespucio, No. 49, 41092 Seville, Spain
2
SpLine CRG at the European Synchrotron Radiation Facility
, BP220, F-38043 Grenoble Cedex, France
a)
Electronic mail: [email protected].
J. Appl. Phys. 104, 023519 (2008)
Article history
Received:
September 10 2007
Accepted:
May 28 2008
Citation
Víctor López-Flores, Manuel A. Roldán, Concepción Real, Adela Muñoz Páez, Germán R. Castro; Polymorphic transformation from body-centered to face-centered cubic vanadium metal during mechanosynthesis of nanostructured vanadium nitride determined by extended x-ray absorption fine structure spectroscopy. J. Appl. Phys. 15 July 2008; 104 (2): 023519. https://doi.org/10.1063/1.2958324
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