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1.
Dalton Trans ; 53(14): 6423-6435, 2024 Apr 02.
Artículo en Inglés | MEDLINE | ID: mdl-38506269

RESUMEN

Combining the experimental techniques of high-resolution X-ray diffraction, magnetometry, specific heat measurement, and X-ray photoelectron, Raman and dielectric spectroscopy techniques, we have studied the influence of La and Cr doping on the crystal structure and magnetism of the room temperature Aurivillius multiferroic Bi5Ti3FeO15 by investigating the physical properties of (Bi4La)Ti3FeO15 and Bi5Ti3 (Fe0.5Cr0.5)O15. The parent (Bi5Ti3FeO15) and the doped ((Bi4La)Ti3FeO15 and Bi5Ti3(Fe0.5Cr0.5)O15) compounds crystallize in the A21am space group, which is confirmed through our analysis of high-resolution synchrotron X-ray diffraction data obtained on phase-pure polycrystalline powders. We determined the oxidation states of the metal atoms in the studied compounds as Fe3+, Ti4+, Cr3+, and La3+ through the analysis of X-ray photoelectron spectroscopy data. The magnetic susceptibilities of the three compounds are marked by the absence of a long-range ordered ground state, but dominated by superparamagnetic clusters with dominant antiferromagnetic interactions. This signature of short-range magnetism is also seen in specific heat as a low temperature enhancement which is suppressed upon the application of external magnetic fields up to 8 T. Our dielectric spectroscopy experiments showed that the three studied compounds display similar features in the dielectric constant measured as a function of frequency. However, upon doping La at the Bi site, the width of the ferroelectric hysteresis loop increases for (Bi4La)Ti3FeO15 compared to that of the parent compound Bi5Ti3FeO15, and with Cr doping, Bi5Ti3(Fe0.5Cr0.5)O15 becomes a leaky dielectric. The resilience of the Aurivillius crystal structure towards doping of La at the Bi site and Cr at the Fe site is clearly seen in the bulk properties of magnetic susceptibility, specific heat and the average crystal structure. The relevance of changes in the local structure is evident from our Raman spectroscopy and X-ray pair distribution function studies.

2.
Polymers (Basel) ; 13(18)2021 Sep 18.
Artículo en Inglés | MEDLINE | ID: mdl-34578073

RESUMEN

In this study, chitosan was chemically modified with 2-methylpyridine. Subsequently, the modified chitosan was cross-linked to cellulose using succinic anhydride. Additionally, the capacity of cellulose derivatives to adsorb Pb(II) ions in an aqueous solution was studied through the determination of Pb(II) ions concentration in water, using microwave plasma atomic emission spectroscopy (MP-AES). A maximum adsorption capacity of 6.62, 43.14, 60.6, and 80.26 mg/g was found for cellulose, cellulose-succinic acid, cellulose-chitosan, and cellulose-chitosan-pyridine, respectively. The kinetic data analysis of the adsorption process showed a pseudo-second-order behavior. The increase in metal removal from water is possibly due to metal chelation with the carbonyl group of succinic acid, and the pyridine groups incorporated into chitosan.

3.
Polymers (Basel) ; 13(13)2021 Jun 23.
Artículo en Inglés | MEDLINE | ID: mdl-34201854

RESUMEN

Heavy metals in water are a serious environmental problem due to their accumulation and toxicity; there are several processes we can use to address this issue, but adsorption is the most popular due to its simplicity and efficiency. Polysaccharides such as cellulose have received attention as adsorbents for heavy metals, and cotton-chitosan composites (CCs) were developed here with nontoxic reagents such as carboxylic acids as crosslinkers and NaH2PO4 as a catalyst to achieve chitosan covalent crosslinkage into oxidized cotton textiles with H2O2. The composites were characterized by fourier-transform infrared spectroscopy (FTIR), elemental analysis (EA), X-ray photoelectron spectroscopy (XPS), atomic-force and scanning electron microscopy (AFM and SEM), and tensile strength; the adsorption of lead ions (Pb) was evaluated with cotton-chitosan composites and quantified by microwave plasma atomic emission spectroscopy (MP-AES). The composites showed a maximum incorporation of chitosan of 27.62 mg per gram of cotton textile. A tensile strength analysis of the composite showed a Young's modulus approximately 1 MPa higher than that of cotton textile. The adsorption of lead ions with composites in an aqueous solution at pH 5 and 25 °C was circa 74% after 6 h of contact, as determined by MP-AES. This work is an approach to demonstrate the potential of these polysaccharides, modified by "green" procedures to remove pollutants from water.

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