Preparation, Characterization, andab initioX-Ray Powder Diffraction Study of Cu2(OH)3(CH3COO)·H2O

Masciocchi, Norberto; Corradi, Eleonora; Sironi, Angelo; Moretti, Giuliano; Minelli, G.; Porta, P.

doi:10.1006/jssc.1997.7372

Cited by 88 publications

(110 citation statements)

References 35 publications

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“…38 FTIR spectra suggest that the bonding of the acetate to the metal centers in the gallery spacing is pseudo-bridging in ZCA with one acetate oxygen bound to Cu 2+ and the other acetate oxygen forming a hydrogen bond with an adjacent OH group from the metal hydroxide layer, similar to that reported 37 for Cu2(OH)3(CH3CO2)·H2O. ZHA and ZNA spectra were more consistent with unidentate binding; 38 however, the possibility of hydrogen-bonding interaction of the "free" carbonyl oxygen cannot be precluded on the basis of the FTIR data.…”

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confidence: 81%

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Thermal Degradation of Acetate-Intercalated Hydroxy Double and Layered Hydroxy Salts

Kandare

Hossenlopp

2006

Inorg. Chem.

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Synopsis:The gas-phase products from thermal degradation of zinccontaining layered metal hydroxides with intercalated acetate anions depend on the identity of metals in the hydroxide layers. Zinc hydroxy acetate and zinc/nickel hydroxy acetate precursors promote ketonization to produce acetone while this channel is suppressed in zinc copper hydroxy acetate. Growth of ZnO crystallites is also precursor dependent.NOT THE PUBLISHED VERSION; this is the author's final, peer-reviewed manuscript. The published version may be accessed by following the link in the citation at the bottom of the page.Inorganic Chemistry, Vol 45, No. 9 (April 2006): pg. 3766-3773. DOI. This article is © American Chemical Society and permission has been granted for this version to appear in e-Publications@Marquette. American Chemical Society does not grant permission for this article to be further copied/distributed or hosted elsewhere without the express permission from American Chemical Society. 2 AbstractTwo hydroxy double salts (HDSs), zinc copper hydroxy acetate (ZCA) and zinc nickel hydroxy acetate (ZNA), and an analogous layered compound, zinc hydroxy acetate (ZHA), have been prepared by a coprecipitation method. The thermal degradation of these materials was characterized via thermogravimetric analysis (TGA), differential thermal analysis (DTA), and TGA coupled with Fourier transform infrared spectroscopy of gas-phase products, TGA-FTIR. Loss of physisorbed and interlayer H2O was observed between 50 and 150 °C for all compounds. Acetic acid, acetone, water, and CO2 were released at high temperatures with relative acetone yields found to be dependent on precursor identity, with very little formed from ZCA compared with ZHA and ZNA. Combined FTIR and XRD analysis of solid residues extracted at different points in the heating profile suggests that ketonization occurs via dissociative adsorption of acetic acid on ZnO surfaces. Nanometer-sized ZnO particles were formed from ZHA, showing slight preferential growth in the ZnO (002) lattice direction, while the presence of a second metal, Ni or Cu, served to retard ZnO crystallite growth at temperatures below 600 °C and eliminate preferential growth. ZCA leads to the formation of reduced copper species (metallic copper and Cu2O) when heated to 250 °C.

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“…8-88) 33 as extensively described by Masciocchi and co-workers. 37 ZHA, ZCA, and ZNA were accessed by following the link in the citation at the bottom of the page.…”

Section: Resultsmentioning

confidence: 99%

Thermal Degradation of Acetate-Intercalated Hydroxy Double and Layered Hydroxy Salts

Kandare

Hossenlopp

2006

Inorg. Chem.

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“…25 Elemental analysis is consistent with at least some of the acetate groups binding to Cu 2+ ; we also note that DRS data (Supporting Information) for ZCA and selected anionexchanged HDSs are also consistent with anion interaction with Cu 2+ sites based on shifts in visible wavelength bands assignable to Cu 2+ d−d transitions.…”

supporting

confidence: 72%

Hydroxy Double Salt Anion Exchange Kinetics: Effects of Precursor Structure and Anion Size

Kandare

Hossenlopp

2005

J. Phys. Chem. B

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1 H NMR spectroscopy and powder X-ray diffraction have been used to explore the details of anion exchange reactions of two layered hydroxy double salts (HDSs), zinc copper hydroxy acetate (ZCA), nickel zinc hydroxy acetate (NZA), and a related layered material, zinc hydroxy acetate (ZHA), at room temperature (21−22 °C). Reactions that followed Avrami−Erofe'ev kinetics with respect to temporal profiles for acetate release, ZCA with butyrate (k = 1.7 × 10 -3 s -1 ), and octanoate (k = 0.79 × 10 -3 s -1 ) anions, as well as ZHA with octanoate (k = 2.6 × 10 -3 s -1 ), demonstrate that rate constants for acetate release are influenced by the exchange anion relative size as well as by the solid precursor structure/composition. The reaction of NZA with octanoate deviated from expected Avrami−Erofe'ev behavior, with

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“…The acetate anion is coordinated to cobalt(II) ion by the oxygen atom, and occupies the interlayer spacing with a head to tail arrangement. Such a structural model for the inorganic layer is also found for the copper(II) hydroxyacetate [11,18].…”

Section: X-ray Diffraction Studymentioning

confidence: 54%

Structural and spectroscopic study of organic-inorganic transition metal based layered magnets

Rabu¹,

Drillon²,

Hornick³

2000

Analusis

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IntroductionRecently, a novel trend of investigation has been the combination of both molecular and solid state chemistry to build hybrid organic-inorganic materials [1]. Clearly, the research on hybrid compounds is very appealing for the design of novel 3d networks in which the physical properties of both assemblies, that are normally found in distinct materials, are in close conjunction [2][3][4][5].Smectite clay minerals (montmorillonite for instance), in which silicate layers are negatively charged by substituting divalent metal ions for trivalent ones, constitute versatile host layer structures for organic or inorganic species. A large number of such cation exchangeable layer compounds are known in which the intercalated species favor pillared structures.Anion exchangeable layered compounds are less common, probably because the anions are usually strongly bound to the metal ions, and form the framework of the crystal. Exchange of interlamellar anions by organic species (dicarboxylic acid anions) was first reported by Miyata and Kumura [6]. Then, the interlayer arrangement of anionic surfactants has been extensively studied in layered double-consisting of positively charged hydroxide layers, separated by A -anions counter-balancing the positive charge of the hydroxy layers [3,4,7,8]. In such compounds, the counterion A -is located in between the hydroxy layers, and no real chemical bond exists usually between the guest and host sub-networks. The cohesion is basically due to electrostatic interactions, and when available to weak hydrogen bond couplings.On the other hand, new hybrid magnetic materials have been prepared by anion exchange reaction, in which the exchangeable anion A -is coordinated to the divalent metal ion. The layered compounds M 2 (OH) 3 A (M = Co, Cu, and A = NO 3 -or OAc -) are shown to be well adapted for substitution reactions [9][10][11][12]. The exchange for large organic species (i.e. aliphatic chain anions) coordinating the metal ion enables to tune the basal spacing, and accordingly to modify drastically the magnetic properties [11,12]. Thus, nalkyl chain molecules involving a single anionic function (carboxylate or sulfate anion), have been used to separate basic layers (Fig. 1a).In that case, the organic spacers exhibit a saturated carbon chain, whose length is mediated by the number of carbon atoms, up to 40 Å [10]. The magnetic interaction within layers is highly dependent on the nature of the anionic function and the chain stacking, so that ferro-, ferri-or antiferromagnetic behavior may be stabilized. Clearly, the n-alkyl chains do not participate directly to interlayer interactionthey may be viewed as "neutral'' pillars -but they modulate the distance between magnetic sheets, and as a result influence through-space magnetic interactions. We have shown that, due to dipolar coupling [13], ferromagnetic 3d order is stabilized when basal spacing becomes large enough (> 10 Å). The interaction mechanism between ferromagnetic layers is then mainly driven by the divergence of the inpl...

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Preparation, Characterization, andab initioX-Ray Powder Diffraction Study of Cu2(OH)3(CH3COO)·H2O

Cited by 88 publications

References 35 publications

Thermal Degradation of Acetate-Intercalated Hydroxy Double and Layered Hydroxy Salts

Thermal Degradation of Acetate-Intercalated Hydroxy Double and Layered Hydroxy Salts

Hydroxy Double Salt Anion Exchange Kinetics: Effects of Precursor Structure and Anion Size

Structural and spectroscopic study of organic-inorganic transition metal based layered magnets

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