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Title: Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase

Abstract

A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2{sub 1}/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D), was also isolated and the crystal structure was determined (monoclinic P2{sub 1}/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D) a metastable phase during the hydrothermal synthesis, was also determined.more » The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal structure of 1D metastable phase was also determined. • Thermal behavior of 2D compound is strongly dependent on the selected heating rate. • Magnetic measurements show no magnetic ordering down to 4 K.« less

Authors:
;  [1];  [2];  [2];  [2]; ;  [3]; ;  [1]
  1. Departamentos de Química Física y Analítica y Química Orgánica e Inorgánica, Universidad de Oviedo-CINN, 33006 Oviedo (Spain)
  2. Servicios Científico Técnicos, Universidad de Oviedo, 33006 Oviedo (Spain)
  3. Departamento de Física, Universidad de Oviedo, 33007 Oviedo (Spain)
Publication Date:
OSTI Identifier:
22475614
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 225; Other Information: Copyright (c) 2015 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ACTIVATION ENERGY; COBALT COMPOUNDS; HEATING RATE; HYDRATES; HYDROGEN; HYDROTHERMAL SYNTHESIS; MAGNETIC SUSCEPTIBILITY; MAGNETIZATION; MONOCLINIC LATTICES; MONOCRYSTALS; PIPERAZINES; POWDERS; PYROLYSIS; THERMAL ANALYSIS; TRANSMISSION ELECTRON MICROSCOPY; TWO-DIMENSIONAL SYSTEMS; WATER; X-RAY DIFFRACTION; ZINC PHOSPHATES

Citation Formats

Torre-Fernández, Laura, Khainakova, Olena A., Espina, Aránzazu, Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es, Khainakov, Sergei A., Alfonso, Belén F., Blanco, Jesús A., García, José R., and García-Granda, Santiago. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase. United States: N. p., 2015. Web. doi:10.1016/J.JSSC.2015.01.010.
Torre-Fernández, Laura, Khainakova, Olena A., Espina, Aránzazu, Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es, Khainakov, Sergei A., Alfonso, Belén F., Blanco, Jesús A., García, José R., & García-Granda, Santiago. Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase. United States. doi:10.1016/J.JSSC.2015.01.010.
Torre-Fernández, Laura, Khainakova, Olena A., Espina, Aránzazu, Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es, Khainakov, Sergei A., Alfonso, Belén F., Blanco, Jesús A., García, José R., and García-Granda, Santiago. Fri . "Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase". United States. doi:10.1016/J.JSSC.2015.01.010.
@article{osti_22475614,
title = {Hydrothermal synthesis and characterization of a two-dimensional piperazinium cobalt–zinc phosphate via a metastable one-dimensional phase},
author = {Torre-Fernández, Laura and Khainakova, Olena A. and Espina, Aránzazu and Amghouz, Zakariae, E-mail: amghouz.uo@uniovi.es and Khainakov, Sergei A. and Alfonso, Belén F. and Blanco, Jesús A. and García, José R. and García-Granda, Santiago},
abstractNote = {A two-dimensional piperazinium cobalt–zinc phosphate, formulated as (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), was synthesized under hydrothermal conditions. The crystal structure was determined using single-crystal X-ray diffraction data (monoclinic P2{sub 1}/c, a=8.1165(3) Å, b=26.2301(10) Å, c=8.3595(4) Å, and β=110.930(5)°) and the hydrogen atom positions were optimized by DFT calculations. A single-crystal corresponding to one-dimensional metastable phase, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D), was also isolated and the crystal structure was determined (monoclinic P2{sub 1}/c, a=8.9120(6) Å, b=14.0290(1) Å, c=12.2494(5) Å, and β=130.884(6)°). The bulk was characterized by chemical (C–H–N) analysis, powder X-ray diffraction (PXRD), powder X-ray thermodiffractometry (HT-XRD), transmission electron microscopy (STEM(DF)-EDX and EFTEM), and thermal analysis (TG/SDTA-MS), including activation energy data of its thermal decomposition. The magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Graphical abstract: Hydrothermal synthesis and structural characterization of a two-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12}){sub 1.5}(Co{sub 0.6}Zn{sub 0.4}){sub 2}(HPO{sub 4}){sub 2}(PO{sub 4})·H{sub 2}O (2D), have been reported. The crystal structure of a one-dimensional piperazinium cobalt–zinc phosphate, (C{sub 4}N{sub 2}H{sub 12})Co{sub 0.3}Zn{sub 0.7}(HPO{sub 4}){sub 2}·H{sub 2}O (1D) a metastable phase during the hydrothermal synthesis, was also determined. The thermal behavior of 2D compound is strongly dependent on the selected heating rate and the magnetic susceptibility and magnetization measurements show no magnetic ordering down to 4 K. - Highlights: • A 2D piperazinium cobalt–zinc phosphate has been synthesized and characterized. • Crystal structure of 1D metastable phase was also determined. • Thermal behavior of 2D compound is strongly dependent on the selected heating rate. • Magnetic measurements show no magnetic ordering down to 4 K.},
doi = {10.1016/J.JSSC.2015.01.010},
journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = ,
volume = 225,
place = {United States},
year = {2015},
month = {5}
}