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