Synthesis and characterization of mesoporous VOx/MgO aerogels with high surface area

Ekaterina V. Ilyina, Ilya V. Mishakov, Aleksey A. Vedyagin, Svetlana V. Cherepanova, Alexander N. Nadeev, Alexander F. Bedilo, Kenneth J. Klabunde

Research output: Contribution to journalArticle

18 Citations (Scopus)

Abstract

Homogeneously mixed mesoporous VOx/MgO aerogels with vanadium concentrations ranging up to 26 wt.% with the surface area as high as 1200 m2/g were synthesized by hydrolysis of a mixture of vanadium and magnesium alkoxides followed by gelation and high-temperature supercritical drying. Dehydration conditions were optimized to obtain nanocrystalline VO x/MgO oxides with the surface area exceeding 450 m2/g after calcination at 550 °C. The synthesized aerogels were extensively characterized by physicochemical methods (XRD, NMR, HRTEM, EDX). According to the EDX data, vanadium atoms were very uniformly distributed in the MgO structure of the mixed oxide aerogels. No magnesium vanadate phases were observed by XRD in the samples with the vanadium concentrations 26% or lower. As the vanadium concentration increased, vanadium ions were introduced into the MgO nanocrystals changing their symmetry from the initial cubic (Fm3 m) to orthorhombic (Cmca). Simulation of the XRD patterns of as-prepared aerogels suggests that the Mg(OH)2 phase in these samples is substantially distorted due to the presence of methoxide groups between the layers.

Original languageEnglish
Pages (from-to)32-40
Number of pages9
JournalMicroporous and Mesoporous Materials
Volume160
DOIs
Publication statusPublished - 15 Sep 2012
Externally publishedYes

Fingerprint

Vanadium
Aerogels
aerogels
vanadium
synthesis
Oxides
Magnesium
magnesium
Energy dispersive spectroscopy
Vanadates
vanadates
alkoxides
Crystal symmetry
gelation
mixed oxides
Gelation
Dehydration
dehydration
Calcination
roasting

Keywords

  • Aerogels
  • Nanocrystals
  • VO/MgO

ASJC Scopus subject areas

  • Materials Science(all)
  • Mechanics of Materials
  • Chemistry(all)
  • Condensed Matter Physics

Cite this

Synthesis and characterization of mesoporous VOx/MgO aerogels with high surface area. / Ilyina, Ekaterina V.; Mishakov, Ilya V.; Vedyagin, Aleksey A.; Cherepanova, Svetlana V.; Nadeev, Alexander N.; Bedilo, Alexander F.; Klabunde, Kenneth J.

In: Microporous and Mesoporous Materials, Vol. 160, 15.09.2012, p. 32-40.

Research output: Contribution to journalArticle

Ilyina, Ekaterina V. ; Mishakov, Ilya V. ; Vedyagin, Aleksey A. ; Cherepanova, Svetlana V. ; Nadeev, Alexander N. ; Bedilo, Alexander F. ; Klabunde, Kenneth J. / Synthesis and characterization of mesoporous VOx/MgO aerogels with high surface area. In: Microporous and Mesoporous Materials. 2012 ; Vol. 160. pp. 32-40.
@article{4c5e5ee5e9094ebd88d3f3453340a2af,
title = "Synthesis and characterization of mesoporous VOx/MgO aerogels with high surface area",
abstract = "Homogeneously mixed mesoporous VOx/MgO aerogels with vanadium concentrations ranging up to 26 wt.{\%} with the surface area as high as 1200 m2/g were synthesized by hydrolysis of a mixture of vanadium and magnesium alkoxides followed by gelation and high-temperature supercritical drying. Dehydration conditions were optimized to obtain nanocrystalline VO x/MgO oxides with the surface area exceeding 450 m2/g after calcination at 550 °C. The synthesized aerogels were extensively characterized by physicochemical methods (XRD, NMR, HRTEM, EDX). According to the EDX data, vanadium atoms were very uniformly distributed in the MgO structure of the mixed oxide aerogels. No magnesium vanadate phases were observed by XRD in the samples with the vanadium concentrations 26{\%} or lower. As the vanadium concentration increased, vanadium ions were introduced into the MgO nanocrystals changing their symmetry from the initial cubic (Fm3 m) to orthorhombic (Cmca). Simulation of the XRD patterns of as-prepared aerogels suggests that the Mg(OH)2 phase in these samples is substantially distorted due to the presence of methoxide groups between the layers.",
keywords = "Aerogels, Nanocrystals, VO/MgO",
author = "Ilyina, {Ekaterina V.} and Mishakov, {Ilya V.} and Vedyagin, {Aleksey A.} and Cherepanova, {Svetlana V.} and Nadeev, {Alexander N.} and Bedilo, {Alexander F.} and Klabunde, {Kenneth J.}",
year = "2012",
month = "9",
day = "15",
doi = "10.1016/j.micromeso.2012.04.016",
language = "English",
volume = "160",
pages = "32--40",
journal = "Microporous and Mesoporous Materials",
issn = "1387-1811",
publisher = "Elsevier",

}

TY - JOUR

T1 - Synthesis and characterization of mesoporous VOx/MgO aerogels with high surface area

AU - Ilyina, Ekaterina V.

AU - Mishakov, Ilya V.

AU - Vedyagin, Aleksey A.

AU - Cherepanova, Svetlana V.

AU - Nadeev, Alexander N.

AU - Bedilo, Alexander F.

AU - Klabunde, Kenneth J.

PY - 2012/9/15

Y1 - 2012/9/15

N2 - Homogeneously mixed mesoporous VOx/MgO aerogels with vanadium concentrations ranging up to 26 wt.% with the surface area as high as 1200 m2/g were synthesized by hydrolysis of a mixture of vanadium and magnesium alkoxides followed by gelation and high-temperature supercritical drying. Dehydration conditions were optimized to obtain nanocrystalline VO x/MgO oxides with the surface area exceeding 450 m2/g after calcination at 550 °C. The synthesized aerogels were extensively characterized by physicochemical methods (XRD, NMR, HRTEM, EDX). According to the EDX data, vanadium atoms were very uniformly distributed in the MgO structure of the mixed oxide aerogels. No magnesium vanadate phases were observed by XRD in the samples with the vanadium concentrations 26% or lower. As the vanadium concentration increased, vanadium ions were introduced into the MgO nanocrystals changing their symmetry from the initial cubic (Fm3 m) to orthorhombic (Cmca). Simulation of the XRD patterns of as-prepared aerogels suggests that the Mg(OH)2 phase in these samples is substantially distorted due to the presence of methoxide groups between the layers.

AB - Homogeneously mixed mesoporous VOx/MgO aerogels with vanadium concentrations ranging up to 26 wt.% with the surface area as high as 1200 m2/g were synthesized by hydrolysis of a mixture of vanadium and magnesium alkoxides followed by gelation and high-temperature supercritical drying. Dehydration conditions were optimized to obtain nanocrystalline VO x/MgO oxides with the surface area exceeding 450 m2/g after calcination at 550 °C. The synthesized aerogels were extensively characterized by physicochemical methods (XRD, NMR, HRTEM, EDX). According to the EDX data, vanadium atoms were very uniformly distributed in the MgO structure of the mixed oxide aerogels. No magnesium vanadate phases were observed by XRD in the samples with the vanadium concentrations 26% or lower. As the vanadium concentration increased, vanadium ions were introduced into the MgO nanocrystals changing their symmetry from the initial cubic (Fm3 m) to orthorhombic (Cmca). Simulation of the XRD patterns of as-prepared aerogels suggests that the Mg(OH)2 phase in these samples is substantially distorted due to the presence of methoxide groups between the layers.

KW - Aerogels

KW - Nanocrystals

KW - VO/MgO

UR - http://www.scopus.com/inward/record.url?scp=84861408935&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84861408935&partnerID=8YFLogxK

U2 - 10.1016/j.micromeso.2012.04.016

DO - 10.1016/j.micromeso.2012.04.016

M3 - Article

VL - 160

SP - 32

EP - 40

JO - Microporous and Mesoporous Materials

JF - Microporous and Mesoporous Materials

SN - 1387-1811

ER -