What's behind "hexagonal molybdenum oxide"?

Hans Joachim Lunk; Hans Hartl; Timothy A. Frisk; Ilya G. Shenderovich; Daniel Mauder; Michael Feist; Martin J.G. Fait; Monika A. Hartl; Luke L. Daemen; Reinhard Eckelt

What's behind "hexagonal molybdenum oxide"?

Hans Joachim Lunk, Hans Hartl, Timothy A. Frisk, Ilya G. Shenderovich, Daniel Mauder, Michael Feist, Martin J.G. Fait, Monika A. Hartl, Luke L. Daemen, Reinhard Eckelt

Research output: Chapter in Book/Report/Conference proceeding › Conference contribution › peer-review

Abstract

Over the last 40 years, a large number of isostructural compounds in the system MoO₃-NH₃-H₂O have been published. The reported molecular formulae of "hexagonal molybdenum oxide" varied from MoO₃, MoO₃·0.33NH₃, MoO ₃·nH₂O (0.09<n<0.69) to MoO ₃·mNH₃·nH₂O (0.09<m<0.20; 0.18<n<0.60). Samples, prepared by the acidification route, were investigated using Thermal Analysis coupled online to a mass spectrometer for evolved gas analysis; X-ray powder diffraction; Fourier Transform Infrared, Raman and Magic-Angle-Spinning H-NMR spectroscopy; Incoherent Inelastic Neutron Scattering. The X-ray study of a selected monocrystal confirmed the presence of the well-known framework of edge-sharing MoO6 octahedra. The colorless monocrystal crystallizes in the hexagonal system with space group P6 ₃/m, Z = 6 and unit cell parameters of a = 10.527(1), c = 3.7245(7) Å, γ = 120°, V = 357.44(8) Å³. The structure of the synthesized samples can best be described by the structural formula (NH4)[Mox 1/2+p/2(O3x+1/2-p/2)(OH)p] · yH₂O (x = 5.9-7.1; p∼0.1; y = 1.2-2.6), which is consistent with the existence of one vacancy for 12-15 molybdenum sites. The "chimie douce" reaction of MoO ₃·0.155NH3·0.440H₂O with a 1:1 mixture of NO/NO₂ at 100°C resulted in the synthesis of MoO ₃·0.539H₂O.

Original language	English
Title of host publication	Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009
Pages	872-886
Number of pages	15
State	Published - 2009
Externally published	Yes
Event	2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009 - Las Vegas, NV, United States Duration: Jun 28 2009 → Jul 1 2009

Publication series

Name	Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009

Conference

Conference	2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009
Country/Territory	United States
City	Las Vegas, NV
Period	06/28/09 → 07/1/09

Cite this

Lunk, H. J., Hartl, H., Frisk, T. A., Shenderovich, I. G., Mauder, D., Feist, M., Fait, M. J. G., Hartl, M. A., Daemen, L. L., & Eckelt, R. (2009). What's behind "hexagonal molybdenum oxide"? In Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009 (pp. 872-886). (Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009).

Lunk, Hans Joachim ; Hartl, Hans ; Frisk, Timothy A. et al. / What's behind "hexagonal molybdenum oxide"?. Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009. 2009. pp. 872-886 (Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009).

@inproceedings{bf017b780cbb4993b0817bb6311bc877,

title = "What's behind {"}hexagonal molybdenum oxide{"}?",

abstract = "Over the last 40 years, a large number of isostructural compounds in the system MoO3-NH3-H2O have been published. The reported molecular formulae of {"}hexagonal molybdenum oxide{"} varied from MoO3, MoO3·0.33NH3, MoO 3·nH2O (0.093·mNH3·nH2O (0.093/m, Z = 6 and unit cell parameters of a = 10.527(1), c = 3.7245(7) {\AA}, γ = 120°, V = 357.44(8) {\AA}3. The structure of the synthesized samples can best be described by the structural formula (NH4)[Mox 1/2+p/2(O3x+1/2-p/2)(OH)p] · yH2O (x = 5.9-7.1; p∼0.1; y = 1.2-2.6), which is consistent with the existence of one vacancy for 12-15 molybdenum sites. The {"}chimie douce{"} reaction of MoO 3·0.155NH3·0.440H2O with a 1:1 mixture of NO/NO2 at 100°C resulted in the synthesis of MoO 3·0.539H2O.",

author = "Lunk, {Hans Joachim} and Hans Hartl and Frisk, {Timothy A.} and Shenderovich, {Ilya G.} and Daniel Mauder and Michael Feist and Fait, {Martin J.G.} and Hartl, {Monika A.} and Daemen, {Luke L.} and Reinhard Eckelt",

year = "2009",

language = "English",

isbn = "9780981949611",

series = "Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009",

pages = "872--886",

booktitle = "Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009",

note = "2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009 ; Conference date: 28-06-2009 Through 01-07-2009",

}

Lunk, HJ, Hartl, H, Frisk, TA, Shenderovich, IG, Mauder, D, Feist, M, Fait, MJG, Hartl, MA, Daemen, LL & Eckelt, R 2009, What's behind "hexagonal molybdenum oxide"? in Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009. Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009, pp. 872-886, 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009, Las Vegas, NV, United States, 06/28/09.

What's behind "hexagonal molybdenum oxide"? / Lunk, Hans Joachim; Hartl, Hans; Frisk, Timothy A. et al.
Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009. 2009. p. 872-886 (Advances in Powder Metallurgy and Particulate Materials - 2009, Proceedings of the 2009 International Conference on Powder Metallurgy and Particulate Materials, PowderMet 2009).

Research output: Chapter in Book/Report/Conference proceeding › Conference contribution › peer-review