Efficient inductively heated shape memory polyurethane acrylate network with silane modified nanodiamond@Fe3O4 superparamagnetic nanohybrid

doi:10.1016/j.eurpolymj.2021.110735

European Polymer Journal

Volume 159, 5 October 2021, 110735

https://doi.org/10.1016/j.eurpolymj.2021.110735 Get rights and content

Highlights

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Magnetoresponsive PUA/ND-Fe₃O₄ were prepared by in situ polymerization technique.
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Silane modified ND-Fe₃O₄ (S-NDF) hybrid nanoparticle were well-dispersed in matrix.
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PUA and PUA/S-NDF nanocomposites present excellent shape memory behavior in hot water.
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PUA/9 wt% S-NDF nanocomposites exhibit excellent magnetic shape recovery rate (96%).
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The PUA and its nanocomposites are biocompatible (PrestoBlue cell viability assay).

Abstract

Multifunctional magnetic shape memory polymer (SMP) nanocomposites with high sensitivity was synthesized through inclusion of silane functionalized nanodiamond@Fe₃O₄ (S-NDF) hybrid nanoparticle into polycaprolactone (PCL) based polyurethane acrylate (PUA) matrix followed by in situ crosslinking of the matrix. Highly biocompatible and superparamagnetic nanodiamond(ND)@Fe₃O₄ nanohybrids were synthesized through in situ co-precipitation method. The morphological analysis suggested that S-NDFs filled PUAs (2 to 9 wt% loadings) well interacted with both soft and hard domains of the matrix. The base polymer and the nanocomposites presented excellent shape fixity ratio (above 97%) and shape recovery ratio (above 99.5%) in hot water. Furthermore, PUA/S-NDF nanocomposites with nanohybrid loading of 9 wt% exhibited excellent shape recovery rate (above 96%) in a very small magnetic field (H = 0.76 kA.m⁻¹) as well as faster magnetic responsiveness compared to Fe₃O₄ loaded nanocomposites. Moreover, PrestoBlue cell viability assay suggested biocompatibility of the base polymers and the nanocomposites.

Graphical abstract

Introduction

Development of novel smart materials with multifunctional properties has motivated substantial interests in terms of design and application in the past two decades. One of the important classes of these materials is shape memory polymers (SMPs) and nanocomposites based on the SMPs. SMPs are a group of smart materials that can be programmed into a stable temporary shape and then recovered their predefined permanent shape in response to an appropriate external stimulus. Most SMPs are thermo-responsive polymers whose shape is actuated by passing a specific transition temperature, T_tran [1], [2], [3], [4]. Basically, shape memory effect (SME) functions based on a network structure consisting of net points (hard segments) with physical or either chemical nature as well as molecular switches (soft segments) which serve as reversible components through molecular motion in a rubbery state. The hard segments stabilize permanent shape while the soft segments fix temporary shape and thermal transition of the soft segments (T_trans) serves as switch temperature for SME [5], [6], [7].

A fascinating approach in SMPs is the development of noncontact activation without increasing ambient temperature through remote triggering methods such as light (laser heating) and magnetic field (inductive heating) [8], [9], [10], [11]. Such noncontact triggering methods are crucial in applications where the variation of ambient temperature is detrimental for the system or when effective in vivo implementation of SMP devices without recovery in body temperature is required [11], [12], [13]. Examples of such applications can be encountered in biomedical fields as smart implants, tissue engineering [14], soft robotics, and biomedical devices [10] or other applications such as sensors [15].

Magnetically responsive SMPs, as a multifunctional system, can be obtained by incorporating magnetic particles (micrometer and/or nanometer size) into a thermo-sensitive SMP matrix. Resulting magneto-responsive SMP composites enable inductive heating in a magnetic field promoting internal heating through embedded particles. The heating mechanism is related to hysteresis loss and/or related processes originated from superparamagnetism [16]. One of the main concerns in magneto-responsive SMPs is to obtain effective heat transfer in (nano-) composites under magnetic fields which could be dominated by the uniform distribution of suitable magnetic (nano-) particles within polymeric matrix. The present research concerning magneto-responsive SMPs has mainly focused on appropriate dispersion of an effective hybrid nanoparticles (NPs) in a biocompatible polymer matrix to achieve promoted internal heating by application of magnetic fields.

Regarding the tendency of magnetic NPs to agglomeration due to magnetic and van der Waals forces, various approaches were reported for homogeneous dispersion of such NPs in polymer matrices. Surface modification of magnetic NPs with different functional groups and surfactants, through either physical or chemical coupling, as well as covalent integration of magnetic NPs in polymer matrices are essential methods to prevent agglomeration and improve dispersion of NPs in polymer nanocomposites. Oleic acid-coated magnetic NP [8], [17], [18], silica-coated magnetic NP [12], [19], and polymer or oligomer coated magnetic NPs (grafting to, grafting from) [20] are examples of applied methods for stabilization of magnetic NPs in polymer matrices. Covalent integration of magnetic NPs in polymer matrices, makes NPs as nanoscale netpoints and provides better dispersion/distribution within matrices leading to improved internal heat transfer. Another promising new strategy to have better heat transfer in magneto-responsive SMPs is the application of carbon-magnetic hybrid NPs to improve the thermal conductivity. Although studies concerning magneto-responsive SMP composites embedding hybrid carbon-magnetic NPs is rare, e.g. Graphene-Ferromagnetic (G-F) hybrid [21] and Fe₃O₄-MWCNT [22], performance of nanocomposites containing such hybrid NPs was reported to be appealing.

Recently, application of spherical NPs in biomedical fields has shown a rapid growth due to their unique size, better dispersion, and size-dependent properties. [23], [24]. Therefore, present research focuses on a carbon-magnetic hybrid NP for the implementation of remote magnetic triggering. Applied carbon-magnetic hybrid NPs are composed of two spherical NPs including nanodiamond (ND) and Fe₃O₄, to get higher thermal conductivity as well as biocompatibility. Regarding biocompatibility and superparamagnetic characteristics, Fe₃O₄ is known as a prominently promising candidate and most commonly employed in the clinical and biomedical fields compared to other iron oxides and magnetic nanomaterials. On the other hand, ND is a promising candidate to develop multifunctional NPs due to its unique morphology, interesting surface chemistry and proven biocompatibility [24], [25]. Other appealing characteristics of ND which is essential for magento-active stimuli of SMPs is its great thermal conductivity with inherently high electrical resistance [24], [25]. In the previous research [26] decoration of oxidized-ND (Ox-ND) by in situ synthesized Fe₃O₄ through the one-shot co-precipitation method, and subsequently covalent surface functionalization of the synthesized ND-Fe₃O₄ hybrid NPs were reported in details. To the best of our knowledge, there have been no studies on SMP/ND-Fe₃O₄ nanocomposite for remotely controlled SME. For covalent incorporation of ND-Fe₃O₄ nanohybrid in SMP matrix, vinyl-containing silane was used for surface modification of hybrid NPs.

A prominent class of SMPs is segmented polyurethanes (PUs). Shape memory polyurethane (SMPU) is known as a promising SMP with tunable actuation temperatures and adjustable mechanical properties due to a diversity of species of soft and hard segment molecules. Recently, few pieces of research have reported very good shape memory behavior for polyurethane acrylates (PUAs) [27], [28], [29], [30], [31], which are indeed chemically crosslinked PUs with attractive characteristics and thermo- and photo-curing potentials. In this class of PUs, hard segments possess chemical crosslinks with improved mechanical properties. Furthermore, recent literature demonstrates excellent potential of PUAs in biomedical applications, for example soft [32] and hard [33], [34] tissue engineering. In SMPUs for biomedical applications, principal components (polyols and diisocyanates) must be selected based on biocompatible and bio-based resources [8], [35], [36]. Polycaprolactone diol (PCL-diol) with a crystalline structure, good mechanical properties, and excellent biocompatibility is one of the most attractive soft segments in the synthesis of SMPU that have extensively studied in biomedical applications [37], [38].

In this research, we present magnetically induced SMP nanocomposites by in-situ crosslinking of polycaprolactone-based PUAs in presence of magnetic hybrid NPs (ND-Fe₃O₄). The structures, thermal, mechanical and magnetic properties, viability and shape memory behaviors of PUA/ND-Fe₃O₄ are then investigated systematically.

Section snippets

Materials

Polycaprolactone-diol of M_n = 4000 g/mol was kindly provided by Perstorp (Capa^TM 2402). Hexamethylene diisocyanate (HDI) and 2-hydroxyethyl methacrylate (HEMA) were provided from Merck. 2,2- azobisisobutyronitrile (AIBN) was purchased from Sigma-Aldrich. PCL-diol was vacuum dried at 80 °C for 24 h before use. HEMA was dried applying 4 Å molecular sieves prior to use. Other reagents were employed as received with no extra purification.

Detonation ND was purchased from NaBond Technologies Co.,

Characterization of S-NDF nanohybrid

The successful in situ formation and attachment of crystalline Fe₃O₄ NPs onto the surface of thermally oxidized NDs (Ox-ND) through electrostatic interaction as well as silane functionalization of NDF nanohybrid through the formation of covalent bond with VTMS was characterized and confirmed by XRD, FTIR, XPS, TGA and TEM techniques which were described in details in our previous study[26]. The prepared NDF and S-NDF were further analyzed by BET surface analyzer, photoluminescence (PL)

Conclusions

In this study, bio-based polyurethane acrylate nanocomposites (PUA/ND-Fe₃O₄) with thermo- and magneto-responsive shape memory effects as well as high sensitivity were introduced. Silane-modified ND-Fe₃O₄ hybrid nanoparticle (S-NDF) having unique spherical geometry with strong superparamagnetic properties and great thermal conductivity could be an attractive candidate to add magnetic responsiveness to shape memory PUA. For the purpose of homogeneous dispersion of magnetic hybrid NPs and

CRediT authorship contribution statement

Samaneh Salkhi Khasraghi: Investigation, Methodology, Visualization, Writing - original draft. Akbar Shojaei: Conceptualization, Resources, Supervision, Writing - review & editing. Mohsen Janmaleki: Formal analysis. Uttandaraman Sundararaj: Resources, Supervision.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgements

The authors are thankful for the financial support provided by Iran National Science Foundation (INSF) for this work. The supports received from Sharif University of Technology and University of Calgary are also appreciated. In addition, we thank PERSTORP for providing Capa^TM 2402.

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Efficient inductively heated shape memory polyurethane acrylate network with silane modified nanodiamond@Fe3O4 superparamagnetic nanohybrid

Highlights

Abstract

Graphical abstract

Introduction

Section snippets

Materials

Characterization of S-NDF nanohybrid

Conclusions

CRediT authorship contribution statement

Declaration of Competing Interest

Acknowledgements

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Efficient inductively heated shape memory polyurethane acrylate network with silane modified nanodiamond@Fe₃O₄ superparamagnetic nanohybrid