skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Hydrothermal synthesis and structural characterization of (NH{sub 4})GaPO{sub 4}F, KTP-type and (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4}) (HPO{sub 4})F{sub 3}, pseudo-KTP-type materials

Abstract

Two new fluorinated gallium phosphates have been hydrothermally synthesized in the system GaOOH/H{sub 2}O/H{sub 3}PO{sub 4}/HF/guanidine or NH{sub 4}F (180 C, autogenous pressure, 4 days). The structures of both compounds have been characterized by single-crystal X-ray diffraction. The (NH{sub 4})GaPO{sub 4}F phase is isostructural with the KTiOPO{sub 4} (KTP) structural type. The structure of the second phase (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4})(HPO{sub 4})F{sub 3}, named pseudo-KTP or p-KTP, is closely related to that of KTP. In the latter, the existence of terminal P-OH and Ga-F bond along the b axis prevents the full connection by corner-sharing of the PO{sub 4} and Ga(O,F){sub 6} units as it occurs in KTP structure. It results in a more distorted framework in which the occluded ammonium cations interact mainly with the P-OH and Ga-F terminal bonds. The structure of p-KTP was examined by {sup 19}F and {sup 31}P solid-state nuclear magnetic resonance spectroscopy using high-speed MAS experiments (30 kHz). {sup 19}F NMR indicates a full occupancy by fluorine for the atomic sites bridging the gallium atoms. Crystal data is given for (NH{sub 4})GaPO{sub 4}F.

Authors:
; ; ; ; ;
Publication Date:
Research Org.:
Univ. de Versailles-St.Quentin en Yvelines (FR)
OSTI Identifier:
20080267
Resource Type:
Journal Article
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 12; Journal Issue: 5; Other Information: PBD: May 2000; Journal ID: ISSN 0897-4756
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; GALLIUM PHOSPHATES; ORGANIC FLUORINE COMPOUNDS; HYDROTHERMAL SYNTHESIS; CRYSTAL STRUCTURE

Citation Formats

Loiseau, T., Paulet, C., Simon, N., Munch, V., Taulelle, F., and Ferey, G. Hydrothermal synthesis and structural characterization of (NH{sub 4})GaPO{sub 4}F, KTP-type and (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4}) (HPO{sub 4})F{sub 3}, pseudo-KTP-type materials. United States: N. p., 2000. Web. doi:10.1021/cm991177z.
Loiseau, T., Paulet, C., Simon, N., Munch, V., Taulelle, F., & Ferey, G. Hydrothermal synthesis and structural characterization of (NH{sub 4})GaPO{sub 4}F, KTP-type and (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4}) (HPO{sub 4})F{sub 3}, pseudo-KTP-type materials. United States. doi:10.1021/cm991177z.
Loiseau, T., Paulet, C., Simon, N., Munch, V., Taulelle, F., and Ferey, G. Mon . "Hydrothermal synthesis and structural characterization of (NH{sub 4})GaPO{sub 4}F, KTP-type and (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4}) (HPO{sub 4})F{sub 3}, pseudo-KTP-type materials". United States. doi:10.1021/cm991177z.
@article{osti_20080267,
title = {Hydrothermal synthesis and structural characterization of (NH{sub 4})GaPO{sub 4}F, KTP-type and (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4}) (HPO{sub 4})F{sub 3}, pseudo-KTP-type materials},
author = {Loiseau, T. and Paulet, C. and Simon, N. and Munch, V. and Taulelle, F. and Ferey, G.},
abstractNote = {Two new fluorinated gallium phosphates have been hydrothermally synthesized in the system GaOOH/H{sub 2}O/H{sub 3}PO{sub 4}/HF/guanidine or NH{sub 4}F (180 C, autogenous pressure, 4 days). The structures of both compounds have been characterized by single-crystal X-ray diffraction. The (NH{sub 4})GaPO{sub 4}F phase is isostructural with the KTiOPO{sub 4} (KTP) structural type. The structure of the second phase (NH{sub 4}){sub 2}Ga{sub 2}(PO{sub 4})(HPO{sub 4})F{sub 3}, named pseudo-KTP or p-KTP, is closely related to that of KTP. In the latter, the existence of terminal P-OH and Ga-F bond along the b axis prevents the full connection by corner-sharing of the PO{sub 4} and Ga(O,F){sub 6} units as it occurs in KTP structure. It results in a more distorted framework in which the occluded ammonium cations interact mainly with the P-OH and Ga-F terminal bonds. The structure of p-KTP was examined by {sup 19}F and {sup 31}P solid-state nuclear magnetic resonance spectroscopy using high-speed MAS experiments (30 kHz). {sup 19}F NMR indicates a full occupancy by fluorine for the atomic sites bridging the gallium atoms. Crystal data is given for (NH{sub 4})GaPO{sub 4}F.},
doi = {10.1021/cm991177z},
journal = {Chemistry of Materials},
issn = {0897-4756},
number = 5,
volume = 12,
place = {United States},
year = {2000},
month = {5}
}