High-Pressure, High-Temperature Synthesis and Characterization of Boron Suboxide (B 6O)

Hervé Hubert, Laurence Garvie, Bertrand Devouard, P R Buseck, William Petuskey, Paul F. McMillan

Research output: Contribution to journalArticle

113 Citations (Scopus)

Abstract

Boron suboxide, nominally B 6O, was synthesized by reducing B 2O 3 with B up to 10 GPa in a multianvil press at temperatures between 1200 and 1800°C. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and parallel electron energy-loss spectroscopy (PEELS). We used high-pressure techniques to synthesize boron suboxide of improved purity and crystallinity and less oxygen-deficient (i.e., closer to the nominal B 6O composition) in comparison to products of room-pressure syntheses. We describe the preparation of grains ranging from 20 nm to 40 μm in diameter, as well as the first synthesis of micrometer-sized B 6O icosahedral twins and euhedral "crystals". The best materials are obtained for starting mixtures containing an excess B 2O 3 reacted at 1700-1800°C between 4 and 5.5 GPa. After the products were washed in water, well-crystallized single-phase product dominated by icosahedrally twinned particles to 30 μm in diameter was easily recovered. Oxygen occupancies ascertained from Rietveld refinements show data consistent with the chemical compositions determined by PEELS. These results give a composition of B 6O 0.77 for our room-pressure material. The highest O occupancy, B 6O 0.96, is obtained for the micrometer-size icosahedral particles prepared at 1700°C between 4 and 5.5 GPa.

Original languageEnglish (US)
Pages (from-to)1530-1537
Number of pages8
JournalChemistry of Materials
Volume10
Issue number6
StatePublished - Jun 1998

Fingerprint

Boron
Electron energy loss spectroscopy
Chemical analysis
Water wells
Oxygen
Rietveld refinement
X ray powder diffraction
Temperature
Particle size
Transmission electron microscopy
Crystals
Scanning electron microscopy

ASJC Scopus subject areas

  • Materials Chemistry
  • Materials Science(all)

Cite this

High-Pressure, High-Temperature Synthesis and Characterization of Boron Suboxide (B 6O). / Hubert, Hervé; Garvie, Laurence; Devouard, Bertrand; Buseck, P R; Petuskey, William; McMillan, Paul F.

In: Chemistry of Materials, Vol. 10, No. 6, 06.1998, p. 1530-1537.

Research output: Contribution to journalArticle

@article{6320b86c63b54db4840007728b90baa1,
title = "High-Pressure, High-Temperature Synthesis and Characterization of Boron Suboxide (B 6O)",
abstract = "Boron suboxide, nominally B 6O, was synthesized by reducing B 2O 3 with B up to 10 GPa in a multianvil press at temperatures between 1200 and 1800°C. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and parallel electron energy-loss spectroscopy (PEELS). We used high-pressure techniques to synthesize boron suboxide of improved purity and crystallinity and less oxygen-deficient (i.e., closer to the nominal B 6O composition) in comparison to products of room-pressure syntheses. We describe the preparation of grains ranging from 20 nm to 40 μm in diameter, as well as the first synthesis of micrometer-sized B 6O icosahedral twins and euhedral {"}crystals{"}. The best materials are obtained for starting mixtures containing an excess B 2O 3 reacted at 1700-1800°C between 4 and 5.5 GPa. After the products were washed in water, well-crystallized single-phase product dominated by icosahedrally twinned particles to 30 μm in diameter was easily recovered. Oxygen occupancies ascertained from Rietveld refinements show data consistent with the chemical compositions determined by PEELS. These results give a composition of B 6O 0.77 for our room-pressure material. The highest O occupancy, B 6O 0.96, is obtained for the micrometer-size icosahedral particles prepared at 1700°C between 4 and 5.5 GPa.",
author = "Herv{\'e} Hubert and Laurence Garvie and Bertrand Devouard and Buseck, {P R} and William Petuskey and McMillan, {Paul F.}",
year = "1998",
month = "6",
language = "English (US)",
volume = "10",
pages = "1530--1537",
journal = "Chemistry of Materials",
issn = "0897-4756",
publisher = "American Chemical Society",
number = "6",

}

TY - JOUR

T1 - High-Pressure, High-Temperature Synthesis and Characterization of Boron Suboxide (B 6O)

AU - Hubert, Hervé

AU - Garvie, Laurence

AU - Devouard, Bertrand

AU - Buseck, P R

AU - Petuskey, William

AU - McMillan, Paul F.

PY - 1998/6

Y1 - 1998/6

N2 - Boron suboxide, nominally B 6O, was synthesized by reducing B 2O 3 with B up to 10 GPa in a multianvil press at temperatures between 1200 and 1800°C. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and parallel electron energy-loss spectroscopy (PEELS). We used high-pressure techniques to synthesize boron suboxide of improved purity and crystallinity and less oxygen-deficient (i.e., closer to the nominal B 6O composition) in comparison to products of room-pressure syntheses. We describe the preparation of grains ranging from 20 nm to 40 μm in diameter, as well as the first synthesis of micrometer-sized B 6O icosahedral twins and euhedral "crystals". The best materials are obtained for starting mixtures containing an excess B 2O 3 reacted at 1700-1800°C between 4 and 5.5 GPa. After the products were washed in water, well-crystallized single-phase product dominated by icosahedrally twinned particles to 30 μm in diameter was easily recovered. Oxygen occupancies ascertained from Rietveld refinements show data consistent with the chemical compositions determined by PEELS. These results give a composition of B 6O 0.77 for our room-pressure material. The highest O occupancy, B 6O 0.96, is obtained for the micrometer-size icosahedral particles prepared at 1700°C between 4 and 5.5 GPa.

AB - Boron suboxide, nominally B 6O, was synthesized by reducing B 2O 3 with B up to 10 GPa in a multianvil press at temperatures between 1200 and 1800°C. The samples were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and parallel electron energy-loss spectroscopy (PEELS). We used high-pressure techniques to synthesize boron suboxide of improved purity and crystallinity and less oxygen-deficient (i.e., closer to the nominal B 6O composition) in comparison to products of room-pressure syntheses. We describe the preparation of grains ranging from 20 nm to 40 μm in diameter, as well as the first synthesis of micrometer-sized B 6O icosahedral twins and euhedral "crystals". The best materials are obtained for starting mixtures containing an excess B 2O 3 reacted at 1700-1800°C between 4 and 5.5 GPa. After the products were washed in water, well-crystallized single-phase product dominated by icosahedrally twinned particles to 30 μm in diameter was easily recovered. Oxygen occupancies ascertained from Rietveld refinements show data consistent with the chemical compositions determined by PEELS. These results give a composition of B 6O 0.77 for our room-pressure material. The highest O occupancy, B 6O 0.96, is obtained for the micrometer-size icosahedral particles prepared at 1700°C between 4 and 5.5 GPa.

UR - http://www.scopus.com/inward/record.url?scp=0001202604&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0001202604&partnerID=8YFLogxK

M3 - Article

AN - SCOPUS:0001202604

VL - 10

SP - 1530

EP - 1537

JO - Chemistry of Materials

JF - Chemistry of Materials

SN - 0897-4756

IS - 6

ER -