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1.
Dalton Trans ; 53(2): 525-534, 2024 Jan 02.
Article in English | MEDLINE | ID: mdl-38051257

ABSTRACT

In this study, several methods were employed to investigate the electrical characteristics of ß-Ag2MoO4 systems, both Eu-doped and undoped, synthesized using the microwave-assisted hydrothermal method. The focus extended to understanding how synthesis time influences material defects, with doping fixed at 1%. A systematic shift in the silver vacancy (VAg) concentration was observed within the doped ß-Ag2MoO4 system. Specifically, this study demonstrated that the incorporation of Eu3+ into polycrystalline ß-Ag2MoO4 initially increases the VAg concentration. However, as the synthesis time progresses, the VAg concentration decreases, resulting in alterations in the resulting electrical properties, arising from the intricate interplay between the number of grain boundaries and carrier density. By combining information obtained from photoluminescence, positron annihilation lifetime spectroscopy, and impedance spectroscopy, a comprehensive conduction mechanism was formulated, shedding light on both doped and undoped ß-Ag2MoO4 systems.

2.
Carbohydr Polym ; 310: 120739, 2023 Jun 15.
Article in English | MEDLINE | ID: mdl-36925254

ABSTRACT

The effect of citric acid (CA) concentration and water content on the free hole volume of thermoplastic cassava starch films (TPS) was studied. To this aim, continuous in situ positron annihilation lifetime spectroscopy measurements were performed at fixed moisture content and during water desorption. The results show that the increase in CA concentration leads to wider free hole volume distributions with lower mean values. During water desorption, the mean values and width of such distributions systematically decrease with the exposure time, and the evolution of the hole volumes was well-described using the Kohlrausch-Williams-Watts function. The water vapour permeability was significantly higher in films incorporating 5 % (w/w) of CA, in line with the more open network of this material that was revealed in the hole volumes distribution. The Young's modulus of all the developed films increased significantly after partial water desorption, which was attributed to the plasticizer loss reflected in a decrease in the mean hole volume value (between 4 % and 13 %). This work evidences that the control and report of the relative humidity are essential when testing TPS-based films, as their nanostructures are strongly dependent on external conditions.

3.
Carbohydr Polym ; 297: 120026, 2022 Dec 01.
Article in English | MEDLINE | ID: mdl-36184174

ABSTRACT

An experimental study on the evolution of the physicochemical, thermal and nanostructural properties of chitosan samples obtained from squid pens as the deacetylation treatment proceeds is presented. To this aim, potentiometric titration, capillary viscosimetry, infrared spectroscopy, differential scanning calorimetry and positron annihilation lifetime spectroscopy were used. The results obtained are discussed in terms of the influence of the deacetylation time on the deacetylation degree, average molecular weight, thermal parameters and average free nanohole size of the different samples. A way of preparing chitosan matrices with tailored nanostructural characteristics for specific applications through the deacetylation process is explored.


Subject(s)
Chitosan , Animals , Calorimetry, Differential Scanning , Chitin/chemistry , Chitosan/chemistry , Decapodiformes/chemistry , Molecular Weight , Powders
4.
Carbohydr Polym ; 222: 114987, 2019 Oct 15.
Article in English | MEDLINE | ID: mdl-31320046

ABSTRACT

A study of the structural changes at micro- and nano-scale in a chitosan matrix after the adsorption of different metal ions is presented. Toward this aim, samples of chitosan films soaked in different concentrations of copper(II) and chromium(VI) aqueous solutions were prepared. Cu and Cr ions were selected as sorbates since they have different ionic properties. The effect of the adsorbed metal ions on the microstructure of the chitosan matrices were studied using Fourier transformed infrared spectroscopy, UV-vis spectroscopy, differential scanning calorimetry and thermogravimetric analysis. To go further into the study of the samples at the molecular level, the nuclear technique positron annihilation lifetime spectroscopy was used. Results are discussed in terms of the interaction between the metal ions and the chitosan functional groups.

5.
Carbohydr Polym ; 145: 86-94, 2016 07 10.
Article in English | MEDLINE | ID: mdl-27106155

ABSTRACT

Two chitosan polymers with different deacetylation degree and molecular weight were subjected to grafting reactions with the aim to enhance the properties of these bio-based materials. Specifically, n-butyl acrylate in different proportions was grafted onto two different deacetylation degree (DD%) chitosan using radical initiation in a surfactant free emulsion system. Infrared spectroscopy was used to confirm grafting and products grafting percentage and efficiency were evaluated against acrylate/chitosan ratio and DD%. Thermal and structural properties and the behavior against water of the raw and grafted biopolymers were studied using several experimental techniques: differential scanning calorimetry, transmission electron microscopy, dynamic light scattering, water swelling, contact angle and positron annihilation lifetime spectroscopy. The influence of the grafting process on the morphological and physicochemical properties of the prepared natural/synthetic hybrid materials is discussed.


Subject(s)
Acrylates/chemistry , Chitosan/chemistry , Polymers/chemistry , Microscopy, Electron, Transmission , Molecular Weight , Particle Size , Spectroscopy, Fourier Transform Infrared , Water/chemistry , X-Ray Diffraction
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