TY - JOUR
T1 - Synthesis and characterization of a boron-aluminum oxochloride
AU - Yu, Jihong
AU - Xu, Ruren
AU - Xu, Yihua
AU - Yue, Yong
PY - 1996/2/15
Y1 - 1996/2/15
N2 - A novel microporous crystalline boron-aluminum oxochloride with a cationic framework, designated BAC(3), has been synthesized hydrothermally in the system B2O3-Al2O3-Na2O-H 2O and characterized using ICP, ion chromatograph, X-ray diffraction (XRD), magic-angle spinning nuclear magnetic resonance spectroscopy (MAS NMR), infrared spectroscopy (IR), thermal analysis, and adsorption measurement. Some factors, such as temperature, pH value, and anions have important effects on the crystallization. Chemical analysis shows that the as-synthesized solid has the molar composition 0.2B2O3 · 1.0 Al2O3 · 0.6HCl · 5.7H2O. XRD analysis shows that the crystal has a unique framework structure. The crystal is indexable on an orthorhombic unit cell with a = 22.55, b = 14.42, and c = 8.75 Å. The three-dimensional framework is built up from triangular BO3 and tetrahedral BO4 units with BO3/BO4 of 2.6, as well as octahedrally coordinated Al. XRD, IR, and DTA-TG studies demonstrated that the microporous crystal is unstable to thermal treatment above 300°C, with the decomposition of structural H2O and HCl confirmed by mass spectroscopy analysis. On calcination above 800°C, this microporous crystal is converted via an amorphous phase to a known crystalline Al18B4O33. The measurement of adsorption of water indicates that it possesses characteristic micropore adsorption properties. Ion-exchange analysis shows that the Cl- anions in BAC(3) can be partially exchanged by Br- anions, suggesting that this novel microporous crystal has a cationic framework.
AB - A novel microporous crystalline boron-aluminum oxochloride with a cationic framework, designated BAC(3), has been synthesized hydrothermally in the system B2O3-Al2O3-Na2O-H 2O and characterized using ICP, ion chromatograph, X-ray diffraction (XRD), magic-angle spinning nuclear magnetic resonance spectroscopy (MAS NMR), infrared spectroscopy (IR), thermal analysis, and adsorption measurement. Some factors, such as temperature, pH value, and anions have important effects on the crystallization. Chemical analysis shows that the as-synthesized solid has the molar composition 0.2B2O3 · 1.0 Al2O3 · 0.6HCl · 5.7H2O. XRD analysis shows that the crystal has a unique framework structure. The crystal is indexable on an orthorhombic unit cell with a = 22.55, b = 14.42, and c = 8.75 Å. The three-dimensional framework is built up from triangular BO3 and tetrahedral BO4 units with BO3/BO4 of 2.6, as well as octahedrally coordinated Al. XRD, IR, and DTA-TG studies demonstrated that the microporous crystal is unstable to thermal treatment above 300°C, with the decomposition of structural H2O and HCl confirmed by mass spectroscopy analysis. On calcination above 800°C, this microporous crystal is converted via an amorphous phase to a known crystalline Al18B4O33. The measurement of adsorption of water indicates that it possesses characteristic micropore adsorption properties. Ion-exchange analysis shows that the Cl- anions in BAC(3) can be partially exchanged by Br- anions, suggesting that this novel microporous crystal has a cationic framework.
UR - http://www.scopus.com/inward/record.url?scp=0004477211&partnerID=8YFLogxK
U2 - 10.1006/jssc.1996.0102
DO - 10.1006/jssc.1996.0102
M3 - Article
AN - SCOPUS:0004477211
SN - 0022-4596
VL - 122
SP - 200
EP - 205
JO - Journal of Solid State Chemistry
JF - Journal of Solid State Chemistry
IS - 1
ER -