The Synthesis of Ammonium Fluorometallates in Methanol<sup>1a</sup>

Haendler, Helmut M.; Johnson, Frederic A.; Crocket, David S.

doi:10.1021/ja01544a017

Cited by 60 publications

(6 citation statements)

References 2 publications

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“…However, from the observation of etching of glass beakers used for the synthesis, we concluded that in the aqueous medium one cannot avoid the generation of hydrofluoric acid. The generation of HF might be one of the main reasons for the non-stoichiometry observed in the total fluoride content and also for the presence of hydroxyl groups in the final products as observed in earlier reports (Haendler et al 1958;Crocket and Haendler 1960). We have chosen non-aqueous medium for the synthesis of these ternary fluorides mainly for two reasons viz.…”

Section: Resultsmentioning

confidence: 97%

“…In the case of KCuF 3 prepared from aqueous solutions, replacement of one fluoride ion by one hydroxyl ion resulting in a composition of KCu (OH)F 2 has been observed (Machin et al 1963;Li et al 2000). The oxygen content in the complex fluorides synthesized by solid state reaction was higher than that of the corresponding complex fluorides synthesized by hydrothermal technique (Haendler et al 1958). The earliest work on the synthesis of these fluorometallates in non-aqueous medium was carried out by Crocket and Haendler (1960), for the synthesis of NH 4 MF 3 (M = Cd, Co, Cu, Mn, Zn, Mg, Fe) in methanol in the year 1958.…”

Section: Introductionmentioning

confidence: 95%

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Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

et al. 2009

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Synthesis of mixed metal fluorides of the general formula, KMF 3 (M = Mg, Mn, Co, Ni, Cu and Zn), possessing perovskite structure was investigated in non-aqueous medium. The fluorides were characterized by powder X-ray diffraction, FT-IR spectroscopy, thermal analysis, SEM and TEM. Monophasic cubic phases were obtained for the central metal ions such as Mg, Mn, Co, Ni, and Zn and a tetragonally distorted phase was observed for Cu. The usage of non-aqueous medium is advantageous for the bulk synthesis of these fluorides, since it eliminated the generation and handling of the hazardous HF that has usually been encountered during aqueous preparations. The average crystallite size of the fluorides obtained by this approach was estimated to be in the range of 9-30 nm. SEM micrographs of KZnF 3 showed cubic morphology of perovskite phases. TEM studies on KCuF 3 confirmed the presence of tetragonal distortion. The fluoride content was determined by titrimetry and found to be nearly stoichiometric. Some of these fluorides were found to be thermally stable up to 225°C in air. These fluorides were employed as fluorinating agents in organic fluorination reactions, thereby suggesting their possible utilization for selective fluorination of aliphatic and aromatic hydrofluorocarbons (HFCs) that are industrially relevant.

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Section: Resultsmentioning

confidence: 97%

Section: Introductionmentioning

confidence: 95%

Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

et al. 2009

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“…On the basis of the XRD results obtained investigating as-grown anodic films in glycerol solutions, it can be concluded that, except for Fe, Cr, and Ni fluorides, the formation of complex ammonium fluorometallates also takes place. However, in the solutions containing additional water, (NH 4 ) 3 CrF 6 and (NH 4 ) 3 FeF 6 tend to dissolve owing to their higher solubility in aqueous environments. − …”

Section: Results and Discussionmentioning

confidence: 99%

Fabrication and Characterization of Anodic Films onto the Type-304 Stainless Steel in Glycerol Electrolyte

et al. 2013

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Porous films without periodic structuration were formed by direct current anodizing the surface of type-304 stainless steel in glycerol solution containing NH4F and H2O at elevated temperatures. Formed in the solutions containing both NH4F and H2O at the constant voltage mode of up to 50 V, these films are thin (∼1.0–1.2 μm) and yellow, whereas those formed at higher voltages, ca. 60–70 V, are thicker (up to 15 μm) and greenish. Note that these porous films are composed of both amorphous and crystalline species. X-ray diffraction (XRD), energy-dispersive X-ray (EDX), and X-ray photoemission spectroscopy (XPS) investigations and the detailed chemical analysis of incorporated elements revealed the complex nature of these films varied depending on the anodizing solution composition and voltage value applied. On the basis of the obtained data, the possible mechanism of formation of the glycerol anodic films on the SS304 substrate is presented. Compositional and structural transitions of as-grown films to material composed of crystalline Cr1.3Fe0.7O3 and spinel-type species were achieved via calcination procedure of anodized samples in air at 700 °C.

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“…A better way to do so is using structure field diagrams in which the stability of perovskites and related structures are mapped according to their ionic radii quotients. This was already done by Beck et al and Schilling and Meyer, who gave a comprehensive overview of several ABX 3 − and A I B 2 II X 5 / B I A 2 II X 5 ,,,,− halides and showed the correlation of the different structure types with the ratio of the ionic radii quotients r ( A )/ r ( X ) and r ( B )/ r ( X ), as depicte...…”

Section: Introductionmentioning

confidence: 84%

Structures and Ionic Transport Properties of Perovskite-Related B^IA^IIX₃ and B^IA₂^IIX₅ Halides

Plass,

Bette,

Schneider

et al. 2024

Chem. Mater.

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The structure family of perovskites and related phases contains a large variety of compounds with versatile properties and applications. While perovskite structures of the A I B II X 3 type usually are categorized based on geometrical considerations like the Goldschmidt tolerance factor, perovskiterelated and distorted structure types need to be classified by the more general approach of structure field diagrams. By synthesizing LiSr 2 X 5 with X

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The Synthesis of Ammonium Fluorometallates in Methanol^1a

Cited by 60 publications

References 2 publications

Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

Fabrication and Characterization of Anodic Films onto the Type-304 Stainless Steel in Glycerol Electrolyte

Structures and Ionic Transport Properties of Perovskite-Related B^IA^IIX₃ and B^IA₂^IIX₅ Halides

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The Synthesis of Ammonium Fluorometallates in Methanol1a

Cited by 60 publications

References 2 publications

Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

Synthesis of nanocrystalline mixed metal fluorides in nonaqueous medium

Fabrication and Characterization of Anodic Films onto the Type-304 Stainless Steel in Glycerol Electrolyte

Structures and Ionic Transport Properties of Perovskite-Related BIAIIX3 and BIA2IIX5 Halides

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Product

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The Synthesis of Ammonium Fluorometallates in Methanol^1a

Structures and Ionic Transport Properties of Perovskite-Related B^IA^IIX₃ and B^IA₂^IIX₅ Halides