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Iron Oxide Nanocomposite Hydrogels Synthesized Using a One-Step Gamma-Irradiation Method

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Iron Oxide Nanocomposite Hydrogels Synthesized Using a One-Step Gamma-Irradiation Method nanomaterials Article Rheological, Microstructural and Thermal Properties of Magnetic Poly(Ethylene Oxide)/Iron Oxide Nanocomposite Hydrogels Synthesized Using a One-Step Gamma-Irradiation Method Ivan Mari´c 1, Nataša Šijakovi´cVujiˇci´c 2 , Andela¯ Pustak 1, Marijan Goti´c 3, Goran Štefani´c 3, Jean-Marc Grenèche 4 , Goran Draži´c 5 and Tanja Jurkin 1,* 1 Radiation Chemistry and Dosimetry Laboratory, Division of Materials Chemistry, Ruder¯ Boškovi´cInstitute, BijeniˇckaCesta 54, 10000 Zagreb, Croatia; [email protected] (I.M.); [email protected] (A.P.) 2 Laboratory for Supramolecular Chemistry, Division of Organic Chemistry and Biochemistry, Ruder¯ Boškovi´cInstitute, BijeniˇckaCesta 54, 10000 Zagreb, Croatia; [email protected] 3 Laboratory for Molecular Physics and Synthesis of New Materials, Division of Materials Physics, Ruder¯ Boškovi´cInstitute, BijeniˇckaCesta 54, 10000 Zagreb, Croatia; [email protected] (M.G.); [email protected] (G.Š.) 4 Institut des Molécules et Matériaux du Mans (IMMM UMR CNRS 6283), Le Mans Université, Avenue Olivier Messiaen, F-72085 Le Mans CEDEX 9, France; [email protected] 5 Department of Materials Chemistry, National Institute of Chemistry, Hajdrihova 19, SI-1001 Ljubljana, Slovenia; [email protected] * Correspondence: [email protected]; Tel.: +385-1-4571-255 Received: 31 July 2020; Accepted: 10 September 2020; Published: 12 September 2020 Abstract: Magnetic polymer gels are a new promising class of nanocomposite gels. In this work, magnetic PEO/iron oxide nanocomposite hydrogels were synthesized using the one-step γ-irradiation method starting from poly(ethylene oxide) (PEO) and iron(III) precursor alkaline aqueous suspensions followed by simultaneous crosslinking of PEO chains and reduction of Fe(III) precursor. γ-irradiation dose and concentrations of Fe3+, 2-propanol and PEO in the initial suspensions were varied and optimized. With 2-propanol and at high doses magnetic gels with embedded magnetite nanoparticles were obtained, as confirmed by XRD, SEM and Mössbauer spectrometry.The quantitative determination of γ-irradiation generated Fe2+ was performed using the 1,10-phenanthroline method. The maximal Fe2+ molar fraction of 0.55 was achieved at 300 kGy, pH = 12 and initial 5% of Fe3+. The DSC and rheological measurements confirmed the formation of a well-structured network. The thermal and rheological properties of gels depended on the dose, PEO concentration and initial Fe3+ content (amount of nanoparticles synthesized inside gels). More amorphous and stronger gels were formed at higher dose and higher nanoparticle content. The properties of synthesized gels were determined by the presence of magnetic iron oxide nanoparticles, which acted as reinforcing agents and additional crosslinkers of PEO chains thus facilitating the one-step gel formation. Keywords: magnetic hydrogel; gamma-irradiation; poly(ethylene oxide); magnetite; rheological properties; thermal properties; 57Fe Mössbauer spectrometry; XRD; SEM; Fe(II) determination 1. Introduction Magnetic polymer gels (ferrogels) are a new and promising class of nanocomposite hydrogels that have the potential to be used as effective absorbents of toxic ions in water, protein immobilization, separation, in soft actuators such as artificial muscles, in tissue engineering, drug delivery and hyperthermia applications [1–7]. Ferrogels combine the elastic properties and the defined structure Nanomaterials 2020, 10, 1823; doi:10.3390/nano10091823 www.mdpi.com/journal/nanomaterials Nanomaterials 2020, 10, 1823 2 of 25 of gels with the magnetic properties of magnetic nanoparticles (usually magnetite or maghemite) andNanomaterials respond quickly 2019, 9, x FOR to the PEER external REVIEW magnetic field. Apart from their unique magnetic properties,2 of 29 nanocomposite gel scaffolds with embedded magnetite/maghemite nanoparticles have exhibited defined structure of gels with the magnetic properties of magnetic nanoparticles (usually magnetite superior mechanical, rheological and electrical properties compared to scaffold gels without nanoparticle or maghemite) and respond quickly to the external magnetic field. Apart from their unique magnetic reinforcement,properties, betternanocomposite biocompatibility, gel scaffolds low with cytotoxicity, embedded and magnetite/maghemite demonstrated antibacterial nanoparticles properties have [1–4]. Furthermore,exhibited ironsuperior oxide mechanical, nanoparticles rheological have been and shown electrical to promoteproperties osteogenic compared di tofferentiation scaffold gels of stem cellswithout [8–10] and nanoparticle can provide reinforcement, the transduction better ofbiocom the dynamicpatibility, mechanical low cytotoxicity, stimulation and demonstrated required for bone formationantibacterial [11]. properties [1–4]. Furthermore, iron oxide nanoparticles have been shown to promote osteogenicNanocomposite differentiation gels can of be st synthesizedem cells [8–10] by aand variety can provide of methods, the transduction including the of radiolyticthe dynamic method. γ-irradiationmechanical (radiolytic stimulation method) required has for the bone advantage formation of [11]. a pure and homogeneous initiation of the polymer crosslinkingNanocomposite reaction and gels reduction can be of synthesized metal cations, by asa variety well as theof methods, sterility ofincluding the final product.the radiolytic Typically, method. γ-irradiation (radiolytic method) has the advantage of a pure and homogeneous initiation nanocomposite gels are synthesized by two-step methods: (i) γ-irradiation induced crosslinking of of the polymer crosslinking reaction and reduction of metal cations, as well as the sterility of the final the polymerproduct. Typically, in solution nanocomposite in the presence gels ofar pre-preparede synthesized by nanoparticles two-step methods: (NPs) [(i)12 ,γ13-irradiation] or (ii) in situ γ-irradiationinduced crosslinking synthesis of of nanoparticles the polymer in within solution the in already the presence prepared of pre-prepared polymer gel nanoparticles [14–17]. Of (NPs) particular interest[12,13] is the or (ii) one-step in situ γ-irradiation-irradiation synthesis synthesis of ofnanoparticles nanocomposite within gels. the already However, prepared the one-step polymer synthesis gel has the[14–17]. advantage Of particular of simultaneous interest is the crosslinking one-step γ-irradiation of polymer synthesis chains of with nanocomposite the formation gels. of However, network and reductionthe one-step of metal synthesis salts and has thethe formationadvantage of of simult NPs.aneous The one-step crosslinking synthesis of polymer is faster chains and with simpler the and resultsformation in a small of network NPs size and and reduction narrow of size metal distribution salts and the as formation well as homogeneous of NPs. The one-step distribution synthesis of NPs throughoutis faster the and polymer simpler matrix.and results On thein a other small hand, NPs thesize one-step and narrow synthesis size distribution of nanocomposite as well gelsas has beenhomogeneous poorly studied, distribution as it is di offfi NPscult throughout to find favorable the polymer conditions matrix. for On boththe other nanoparticle hand, the synthesisone-step and synthesis of nanocomposite gels has been poorly studied, as it is difficult to find favorable conditions polymer crosslinking. for both nanoparticle synthesis and polymer crosslinking. γ The The-irradiation γ-irradiation method method is is highly highly suitablesuitable for for th thee synthesis synthesis of ofNPs NPs of controlled of controlled size and size shape and shape in ain solution a solution and and in in heterogeneous heterogeneous media media such such as hy asdrogels. hydrogels. It is also It suit is alsoable for suitable forming for the forming three- the three-dimensionaldimensional polymer polymer network. network. However, However, the thestudies studies are mostly are mostly oriented oriented toward toward the synthesis the synthesis of of metalmetal NPs NPs and and gels gels containing containing metal metal NPs. NPs. The radi radiolyticolytic synthesis synthesis of ofiron iron oxide oxide nanoparticles nanoparticles and and nanocompositenanocomposite gels gels is rarelyis rarely studied studied [ 18[18–28].–28]. One of of the the reasons reasons for for this this is a is very a very complex complex iron oxide iron oxide chemistry,chemistry, which which generates generates numerous numerous iron iron oxideoxide and oxyhydroxide oxyhydroxide polymorphs. polymorphs. Another Another difficulty diffi culty is theis highthe high susceptibility susceptibility of of magnetic magnetic iron iron oxideoxide NPs to to (re)oxidation (re)oxidation of offerrous ferrous ions ions (Fe2+ (Fe) to2 +ferric) to ferric 3+ ionsions (Fe3 +(Fe) under) under atmospheric atmospheric conditions, conditions, especially when when they they are are in inthe the nano-size nano-size range. range. The main The main principle of formation of metal and metal oxide nanoparticles by gamma-irradiation of an aqueous principle of formation of metal and metal oxide nanoparticles by gamma-irradiationn+ of an aqueous solution of a metal salt or within a hydrogel is the reduction of metal cations (M ) byn+ hydrated solution of a metal− salt or− within a hydrogel is the reduction of metal cations (M ) by hydrated electrons (e ) (Eo(H2O/ e ) = −2.87 VSHE) and proton radicals (H·) (Eo(H+/H•) = −2.30 VSHE) which are electrons (e )(aqEo(H O/e )aq= 2.87 V ) and proton
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