Dataset Information

Aggregation of Gold Nanoparticles in Presence of the Thermoresponsive Cationic Diblock Copolymer PNIPAAM48-b-PAMPTMA6.

ABSTRACT: The adsorption of the thermoresponsive positively charged copolymer poly(N-isopropylacrylamide)-block-poly(3-acrylamidopropyl)trimethylammonium chloride, PNIPAAM48-b-PAMPTMA6(+), onto negatively charged gold nanoparticles can provide stability to the nanoparticles and make the emerging structure tunable by temperature. In this work, we characterize the nanocomposite formed by gold nanoparticles and copolymer chains and study the influence of the copolymer on the expected aggregation process that undergoes those nanoparticles at high ionic strength. We also determine the lower critical solution temperature (LCST) of the copolymer (around 42 °C) and evaluate the influence of the temperature on the nanocomposite. For those purposes, we use dynamic light scattering, UV-vis spectroscopy and transmission electron microscopy. At the working PNIPAAM48-b-PAMPTMA6(+) concentration, we observe the existence of copolymer structures that trap the gold nanoparticles and avoid the formation of nanoparticles aggregates. Finally, we discuss how these structures can be useful in catalysis and nanoparticles recovery.

SUBMITTER: Robalino DH

PROVIDER: S-EPMC8658865 | biostudies-literature | 2021 Nov

REPOSITORIES: biostudies-literature

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Aggregation of Gold Nanoparticles in Presence of the Thermoresponsive Cationic Diblock Copolymer PNIPAAM48-b-PAMPTMA6.

Robalino David Herrera DH Durán Del Amor María Del Mar MDM Almagro Gómez Carmen María CM Hernández Cifre José Ginés JG

Polymers 20211123 23

The adsorption of the thermoresponsive positively charged copolymer poly(N-isopropylacrylamide)-block-poly(3-acrylamidopropyl)trimethylammonium chloride, PNIPAAM48-b-PAMPTMA6(+), onto negatively charged gold nanoparticles can provide stability to the nanoparticles and make the emerging structure tunable by temperature. In this work, we characterize the nanocomposite formed by gold nanoparticles and copolymer chains and study the influence of the copolymer on the expe ...[more]

PMID: 34883571

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Project description:A series of linear cationic diblock copolymer nanoparticles are prepared by polymerization-induced self-assembly (PISA) via reversible addition-fragmentation chain transfer (RAFT) aqueous dispersion polymerization of 2-hydroxypropyl methacrylate (HPMA) using a binary mixture of non-ionic and cationic macromolecular RAFT agents, namely poly(ethylene oxide) (PEO113, Mn = 4400 g mol-1; Mw/Mn = 1.08) and poly([2-(methacryloyloxy)ethyl]trimethylammonium chloride) (PQDMA125, Mn = 31 800 g mol-1, Mw/Mn = 1.19). A detailed phase diagram was constructed to determine the maximum amount of PQDMA125 stabilizer block that could be incorporated while still allowing access to a pure worm copolymer morphology. Aqueous electrophoresis studies indicated that zeta potentials of +35 mV could be achieved for such cationic worms over a wide pH range. Core cross-linked worms were prepared via statistical copolymerization of glycidyl methacrylate (GlyMA) with HPMA using a slightly modified PISA formulation, followed by reacting the epoxy groups of the GlyMA residues located within the worm cores with 3-aminopropyl triethoxysilane (APTES), and concomitant hydrolysis/condensation of the pendent silanol groups with the secondary alcohol on the HPMA residues. TEM and DLS studies confirmed that such core cross-linked cationic worms remained colloidally stable when challenged with either excess methanol or a cationic surfactant. These cross-linked cationic worms are shown to be much more effective bridging flocculants for 1.0 μm silica particles at pH 9 than the corresponding linear cationic worms (and also various commercial high molecular weight water-soluble polymers.). Laser diffraction studies indicated silica aggregates of around 25-28 μm diameter when using the former worms but only 3-5 μm diameter when employing the latter worms. Moreover, SEM studies confirmed that the cross-linked worms remained intact after their adsorption onto the silica particles, whereas the much more delicate linear worms underwent fragmentation under the same conditions. Similar results were obtained with 4 μm silica particles.

Project description:Reversible addition-fragmentation chain transfer (RAFT) aqueous dispersion polymerization of 2-hydroxypropyl methacrylate was used to prepare three poly(glycerol monomethacrylate) x -poly(2-hydroxypropyl methacrylate) y (denoted G x -H y or PGMA-PHPMA) diblock copolymers, namely G37-H80, G54-H140, and G71-H200. A master phase diagram was used to select each copolymer composition to ensure that a pure worm phase was obtained in each case, as confirmed by transmission electron microscopy (TEM) and small-angle x-ray scattering (SAXS) studies. The latter technique indicated a mean worm cross-sectional diameter (or worm width) ranging from 11 to 20 nm as the mean degree of polymerization (DP) of the hydrophobic PHPMA block was increased from 80 to 200. These copolymer worms form soft hydrogels at 20 °C that undergo degelation on cooling. This thermoresponsive behavior was examined using variable temperature DLS, oscillatory rheology, and SAXS. A 10% w/w G37-H80 worm dispersion dissociated to afford an aqueous solution of molecularly dissolved copolymer chains at 2 °C; on returning to ambient temperature, these chains aggregated to form first spheres and then worms, with the original gel strength being recovered. In contrast, the G54-H140 and G71-H200 worms each only formed spheres on cooling to 2 °C, with thermoreversible (de)gelation being observed in the former case. The sphere-to-worm transition for G54-H140 was monitored by variable temperature SAXS: these experiments indicated the gradual formation of longer worms at higher temperature, with a concomitant reduction in the number of spheres, suggesting worm growth via multiple 1D sphere-sphere fusion events. DLS studies indicated that a 0.1% w/w aqueous dispersion of G71-H200 worms underwent an irreversible worm-to-sphere transition on cooling to 2 °C. Furthermore, irreversible degelation over the time scale of the experiment was also observed during rheological studies of a 10% w/w G71-H200 worm dispersion. Shear-induced polarized light imaging (SIPLI) studies revealed qualitatively different thermoreversible behavior for these three copolymer worm dispersions, although worm alignment was observed at a shear rate of 10 s-1 in each case. Subsequently conducting this technique at a lower shear rate of 1 s-1 combined with ultra small-angle x-ray scattering (USAXS) also indicated that worm branching occurred at a certain critical temperature since an upturn in viscosity, distortion in the birefringence, and a characteristic feature in the USAXS pattern were observed. Finally, SIPLI studies indicated that the characteristic relaxation times required for loss of worm alignment after cessation of shear depended markedly on the copolymer molecular weight.

Dataset Information

Aggregation of Gold Nanoparticles in Presence of the Thermoresponsive Cationic Diblock Copolymer PNIPAAM48-b-PAMPTMA6.

Publications

Aggregation of Gold Nanoparticles in Presence of the Thermoresponsive Cationic Diblock Copolymer PNIPAAM<sub>48</sub>-b-PAMPTMA<sub>6</sub>.

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