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Due to the presence of cationic units interpolyelectrolyte complexes (IPECs) can be used as a universal basis for preparation of biocidal coatings on different surfaces. Metallopolymer nanocomposites were successfully synthesized in irradiated solutions of polyacrylic acid (PAA) and polyethylenimine (PEI), and dispersions of non-stoichiometric IPECs of PAA–PEI containing silver ions. The data from turbidimetric titration and dynamic light scattering showed that pH 6 is the optimal value for obtaining IPECs. Metal polymer complexes based on IPEC with a PAA/PEI ratio equal to 3/1 and 1/3 were selected for synthesis of nanocomposites due to their aggregative stability. Studies using methods of UV–VIS spectroscopy and TEM have demonstrated that the size and spatial organization of silver nanoparticles depend on the composition of polymer systems. The average sizes of nanoparticles are 5 nm and 20 nm for complexes with a molar ratio of PAA/PEI units equal to 3/1 and 1/3, respectively. The synthesized nanocomposites were applied to the glass surface and exhibited high antibacterial activity against both gram-positive (Staphylococcus aureus) and gram-negative bacteria (Salmonella). It is shown that IPEC-Ag coatings demonstrate significantly more pronounced biocidal activity not only in comparison with macromolecular complexes of PAA–PEI, but also coatings of PEI and PEI based nanocomposites. [ABSTRACT FROM AUTHOR]

This paper investigates the structure, morphology and antimicrobial properties of silver-containing nanocomposites based on interpolyelectrolyte complexes (IPEC) of pectin with polyethylenimine, cationic starch or chitosan as a cationic polyelectrolyte. The reduction of silver ions was carried out by thermochemical technique by heating of the interpolyelectrolyte–metal complexes, which in turn prepared by adsorption of ions on IPEC. The chemical reduction was also performed using ascorbic acid as reductant. The temperature and time needed to produce the nanocomposites at which completely reduction of silver ions occurs are 150 °C and 30 min. It is revealed that during thermochemical reduction depending on the type of cationic polyelectrolyte (PEI, cationic starch, chitosan), silver nanoparticles with an average size of 4.1, 5.3 and 4.7 nm, respectively, are formed. Various mechanisms of thermochemical reduction for interpolyelectrolyte–metal complexes containing polymers with aminogroups or polymers with the glucopyranose units are considered. It is found that the silver-containing nanocomposites, formed by thermochemical reduction, exhibited higher antimicrobial activity against strains of S. aureus and E. coli than ones obtained using ascorbic acid. [ABSTRACT FROM AUTHOR]

The structure and properties of Cu/Cu2O-containing nanocomposites formed by chemical reduction of Cu2+ ions in interpolyelectrolyte–metal complexes (IMC) at different molar ratios [NaBH4]: [Cu2+] and reduction times were studied by methods of wide- and small-angle X-ray scattering, transmission electron microscopy, thermomechanical analysis, and antimicrobial tests. Optimal conditions ([NaBH4]: [Cu2+] = 6.0, reduction time ≥ 120 min) for the formation of copper-containing nanocomposites based on interpolyelectrolyte complexes and Cu/Cu2O core–shell nanoparticles have been established by X-ray diffraction analysis. Owing to the above conditions, the structural manifestation of the metal copper phase is fully realized. Applying transmission electron microscopy, it was found that at molar ratio [NaBH4]: [Cu2+] = 6.0, and reduction time of 40 min and 180 min, accordingly, the nanocomposites with average nanoparticles size of 4.1 nm and 12.4 nm are derived from IMC, respectively, what correlates with effective size of the nanocomposites' heterogeneity regions, lp. Thermomechanical analysis has shown that raise in the amount of reducing agent or the duration of reduction of Cu2+ ions in IMC is accompanied by elevation in the glass transition temperature, which reaches a constant level, boost in the temperature of transition to the viscous state Tf and decrease in the relative deformation of nanocomposites. The antimicrobial investigations of the elaborated nanocomposites revealed they possess an antimicrobial activity against S. aureus and E. coli strains. [ABSTRACT FROM AUTHOR]

The structure and properties of silver-containing nanocomposites formed by the method of thermochemical reduction of Ag+ ions in polyelectrolyte-metal complexes pectin–Ag+–polyethyleneimine were studied using X-ray diffraction analysis, thermogravimetric analysis, pyrolysis mass spectrometry, transmission electron microscopy and antimicrobial test. The optimal parameters for the formation of nanocomposites based on interpolyelectrolyte complexes of pectin–polyethyleneimine and Ag nanoparticles (reduction temperature T = 150 °C, reduction time t = 30 min) have been found by X-ray diffraction analysis, in which the structural manifestation of the silver metal phase is fully realized. Using transmission electron microscopy, it was found that nanocomposite formed by thermochemical reduction of Ag+ ions at 150 °C for 30 min has an average nanoparticle size of 4.1 nm that less than for nanocomposite obtained at T = 120 °C during the same reduction time (average nanoparticle size is 5.8 nm). Ag nanoparticles obtained by using a typical reducing agent (NaBH4) have an average size equals 3.8 nm. It was revealed that nanocomposites obtained by thermochemical method have significantly higher antimicrobial activity compared with nanocomposites obtained by chemical reduction of Ag+ ions using NaBH4. A mechanism of thermochemical reduction of silver ions in IMC pectin–Ag+–polyethyleneimine, which is based on the transfer of electrons from the nitrogen atoms of amino groups PEI to Ag+ ions, has been investigated by destructive processes that occur at the same time. [ABSTRACT FROM AUTHOR]

Structural organization, morphology and thermomechanical properties of nanocomposites based on pectin, polyethyleneimine and Cu nanoparticles, formed by the thermal reduction method from interpolyelectrolyte–metal complexes (IMC) pectin–Cu 2+ –polyethyleneimine have been investigated using WAXS (wide-angle X-ray scattering), SAXS (small-angle X-ray scattering) methods as well as TEM (transmission electron microscopy) and thermomechanical analysis. It is defined that thermal reduction of Cu 2+ ions in IMC bulk (while films are heated to the temperature around 170 °C and higher temperatures) results in nanocomposites based on interpolyelectrolyte complexes “pectin–polyethyleneimine” and Cu nanoparticles being formed. In its turn, thermal reduction of copper ions is found out to take place owing to polyethyleneimine (namely, on account of electrons transfer from the amino groups’ nitrogen atoms of polyethyleneimine to Cu 2+ ions). It has been shown by thermomechanical analysis that the optimal time for complete thermal reduction of Cu 2+ ions to metallic copper at T = 170 °C is 30 min. The antimicrobial investigations of the elaborated nanocomposites revealed they possess a high antimicrobial activity against S. aureus and E. coli strains. [ABSTRACT FROM AUTHOR]

The structural organization and thermomechanical properties of nanocomposites prepared from interpolyelectrolyte-metal complex (IMC) involving anionic polyelectrolyte, pectin and AgNO, and cationic polyelectrolyte, poly(4-vinylpyridine), have been investigated using the methods of wide- and small-angle X-ray scattering and thermomechanical analysis. It is established that chemical reduction of Ag ions in the IMC by sodium borohydride results in formation of the nanocomposite based on the 'pectin-poly(4-vinylpyridine)' interpolyelectrolyte complex (IPEC) and Ag nanoparticles as well. At the same time, the level of nanocomposites' structural heterogeneity is substantially enhancing, while effective size of the heterogeneity regions decreases. The nanocomposites IPEC-Ag prepared are shown much bigger T value and enhanced ability for deformation than those for IMC. [ABSTRACT FROM AUTHOR]

The morphology, structural, thermomechanical and electric properties of nanocomposites prepared from interpolyelectrolyte–metal complex being formed involving anionic polyelectrolyte – pectin, CuSO 4 and cationic polyelectrolyte – polyethyleneimine have been investigated using the methods of wide-angle X-ray scattering, transmission electronic microscopy, thermomechanical analysis and dielectric spectroscopy. Such type of nanocomposites with Cu/Cu 2 O core–shell nanoparticles incorporated into polymer matrix is obtained due to the chemical reduction of Cu 2+ cations by NaBH 4 in the interpolyelectrolyte complex, and appearance of the copper’s metallic phase is observed in full extent while BH 4 − :Cu 2+ molar ratio is equal to 6.0. Applying thermomechanical analysis and dielectric spectroscopy, it was observed that transformation of interpolyelectrolyte–metal complexes into nanocomposites results in decreasing of their glass-transition temperature and increasing of the electric conductivity. [ABSTRACT FROM AUTHOR]

Applying wide-angle X-ray scattering method, thermomechanical analysis, and differential scanning calorimetry, the structural organization and properties of nanocomposites formed by chemical reduction of Сu cations in the interpolyelectrolyte-metal complex (pectin-Cu-polyethyleneimine) under the influence of a constant magnetic and electric fields have been studied. It has been found that the chemical reduction of Cu cations in the interpolyelectrolyte-metal complex bulk under constant electric and magnetic fields leads to formation of nanocomposite consisting of interpolyelectrolyte complex, including pectin-polyethyleneimine and nanoparticles of the metal Cu phase, whereas nanocomposite with Cu/CuO nanoparticles is formed in original state (without any field). It was observed that, under constant field, nanocomposites obtained have higher structural glass-transition temperatures and thermal stability. [ABSTRACT FROM AUTHOR]

• Nanocomposites were obtained by thermochemical reduction of Ag+ at 150 °C for 30 min. • The least average size of silver nanoparticles is 4.7 nm for pectin––Ag–chitosan+. • The greatest average size of silver nanoparticles is 9 nm for starch––Ag–starch+. • The greatest antimicrobial activity is the pectin––Ag–chitosan+, and the least starch––Ag–starch+. The effect of the chemical structure of interpolyelectrolyte complexes (IPEC) based on polymers of natural origin (pectin––chitosan+, pectin––cationic starch (starch+), carboxymethylcellulose (CMC–)–cationic β-cyclodextrin (β-CD+), anionic starch (starch–)–cationic starch (starch+) on the structure, morphology, thermomechanical and antimicrobial properties of silver-containing nanocomposites obtained by thermochemical reduction of Ag+ ions in interpolyelectrolyte-metal complexes (IMC) was studied. Thermochemical reduction of Ag+ ions in the IMC bulk for 30 min at 150 °C led to formation of silver-containing nanocomposites and this fact was confirmed by wide-angle X-ray scattering method. Transmission electron microscopy showed that different sized of silver nanoparticles were formed depending on the chemical structure of IPEC. The average size of silver nanoparticles was found to be 4.7 nm for pectin––Ag–chitosan+; 5.3 nm for pectin––Ag–starch+; 6.3 for CMC––Ag–β-CD+ and 9 nm for starch––Ag–starch+, correspondingly. The nanocomposites having smaller average nanoparticle size exhibited higher antimicrobial activity against S. aureus and E. coli strains. Pectin––Ag–chitosan+ nanocomposites formed by thermochemical reduction of Ag+ ions showed that the diameter of the inhibition zone against S. aureus and E. coli strains was 19.7 and 32.6 mm, respectively, whereas these values were 15.6 and 14 mm, respectively, for the same nanocomposites obtained by chemical reduction using ascorbic acid. [ABSTRACT FROM AUTHOR]