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Organic-Inorganic Hybrid Materials III

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A special issue of Polymers (ISSN 2073-4360). This special issue belongs to the section "Polymer Composites and Nanocomposites".

Deadline for manuscript submissions: closed (31 March 2024) | Viewed by 14522

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Dr. Jesús-María García-Martínez

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Polymer Engineering Group (GIP), Polymer Science and Technology Institute (ICTP), Spanish Council for Scientific Research (CSIC), 28006 Madrid, Spain
Interests: polymers and environment; heterogeneous materials based on polymers; polyolefins; interfacial agents; interphase; interface; functionalization; plastic wastes; blends; composites
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Dr. Emilia P. Collar

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Dear Colleagues,

This Special Issue is devoted to one of the most attractive fields in material science and technology research. The concept of organic–inorganic hybrid materials can be applied to a wide variety of approaches at present, including those considering the matrix of inorganic or organic nature. Hence, the encapsulation of organic functionalities within inorganic matrices obtained by sol–gel processes, the polymerization of organoalkoxyxilanes, and the functionalization of inorganic substances such as micro or nanofillers with organic and/or inorganic molecules able to interact with organic matrixes to provide enhanced properties. In any case, it is the interphase between the components that becomes the critical aspect to consider in research activities with this type of advanced material, thus any effort to enhance and understand these interactions will be key to obtaining these materials with "tailor-made"organized structures at the subsequent nano, meso, micro and macro scales.

Dr. Jesús-María García-Martínez
Dr. Emilia P. Collar
Guest Editors

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Keywords

hybrid inorganic/organic polymer-based materials
heterogeneous materials based on polymers interfaces
interphase
functionalization
sol-gel
chemical modification
composites

Published Papers (12 papers)

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16 pages, 4504 KiB

Open AccessArticle

Composites of Poly(3-hydroxybutyrate) and Mesoporous SBA-15 Silica: Crystalline Characteristics, Confinement and Final Properties

by Tamara M. Díez-Rodríguez, Enrique Blázquez-Blázquez, Ernesto Pérez and María L. Cerrada

Polymers 2024, 16(8), 1037; https://doi.org/10.3390/polym16081037 - 10 Apr 2024

Viewed by 264

Abstract

Several composites based on poly(3-hydroxybutyrate) (PHB) and mesoporous SBA-15 silica were prepared by solvent-casting followed by a further stage of compression molding. The thermal stability, phase transitions and crystalline details of these composites were studied, paying special attention to the confinement of the PHB polymeric chains into the mesopores of the silica. For that, differential scanning calorimetry (DSC) and real-time variable-temperature X-ray scattering at small angles (SAXS) were performed. Confinement was stated first by the existence of a small endotherm at temperatures around 20 °C below the main melting or crystallization peak, being later confirmed by a notable discontinuity in the intensity of the main (100) diffraction from the mesoporous silica observed through SAXS experiments, which is related to the change in the scattering contrast before and after the crystallization or melting of the polymer chains. Furthermore, the usual α modification of PHB was developed in all samples. Finally, a preliminary investigation of mechanical and relaxation parameters was carried out through dynamic–mechanical thermal analysis (DMTA). The results show, in the temperature interval analyzed, two relaxations, named α and β (the latest related to the glass transition) in order of decreasing temperatures, in all specimens. The role of silica as a filler is mainly observed at temperatures higher than the glass transition. In such cases, stiffness is dependent on SBA-15 content. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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19 pages, 13353 KiB

Open AccessArticle

Effect of Water Absorption and Stacking Sequences on the Tensile Properties and Damage Mechanisms of Hybrid Polyester/Glass/Jute Composites

by Rudá Aranha, Mario A. Albuquerque Filho, Cícero de L. Santos, Tony Herbert F. de Andrade, Viviane M. Fonseca, Jose Luis Valin Rivera, Marco A. dos Santos, Antonio G. B. de Lima, Wanderley F. de Amorim, Jr. and Laura H. de Carvalho

Polymers 2024, 16(7), 925; https://doi.org/10.3390/polym16070925 - 28 Mar 2024

Viewed by 461

Abstract

The aim of this work is to analyze the effect of water absorption on the mechanical properties and damage mechanisms of polyester/glass fiber/jute fiber hybrid composites obtained using the compression molding and vacuum-assisted resin transfer molding (VARTM) techniques with different stacking sequences. For this purpose, the mechanical behavior under tensile stress of the samples was evaluated before and after hygrothermal aging at different temperatures: TA, 50 °C, and 70 °C for a period of 696 h. The damage mechanism after the mechanical tests was evaluated using SEM analysis. The results showed a tendency for the mechanical properties of the composites to decrease with exposure to an aqueous ambient, regardless of the molding technique used to conform the composites. It was also observed that the stacking sequence had no significant influence on the dry composites. However, exposure to the aqueous ambient led to a reduction in mechanical properties, both for the molding technique and the stacking sequence. Damage such as delamination, fiber pull-out, fiber/matrix detachment, voids, and matrix removal were observed in the composites in the SEM analyses. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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29 pages, 31999 KiB

Open AccessArticle

Mechanochemical Encapsulation of Caffeine in UiO-66 and UiO-66-NH₂ to Obtain Polymeric Composites by Extrusion with Recycled Polyamide 6 or Polylactic Acid Biopolymer

by Cristina Pina-Vidal, Víctor Berned-Samatán, Elena Piera, Miguel Ángel Caballero and Carlos Téllez

Polymers 2024, 16(5), 637; https://doi.org/10.3390/polym16050637 - 27 Feb 2024

Viewed by 658

Abstract

The development of capsules with additives that can be added to polymers during extrusion processing can lead to advances in the manufacturing of textile fabrics with improved and durable properties. In this work, caffeine (CAF), which has anti-cellulite properties, has been encapsulated by liquid-assisted milling in zirconium-based metal–organic frameworks (MOFs) with different textural properties and chemical functionalization: commercial UiO-66, UiO-66 synthesized without solvents, and UiO-66-NH₂ synthesized in ethanol. The CAF@MOF capsules obtained through the grinding procedure have been added during the extrusion process to recycled polyamide 6 (PA6) and to a biopolymer based on polylactic acid (PLA) to obtain a load of approximately 2.5 wt% of caffeine. The materials have been characterized by various techniques (XRD, NMR, TGA, FTIR, nitrogen sorption, UV–vis, SEM, and TEM) that confirm the caffeine encapsulation, the preservation of caffeine during the extrusion process, and the good contact between the polymer and the MOF. Studies of the capsules and PA6 polymer+capsules composites have shown that release is slower when caffeine is encapsulated than when it is free, and the textural properties of UiO-66 influence the release more prominently than the NH₂ group. However, an interaction is established between the biopolymer PLA and caffeine that delays the release of the additive. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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17 pages, 5349 KiB

Open AccessArticle

Water Sorption in Hybrid Polyester/Glass/Jute Composites Processed via Compression Molding and Vacuum-Assisted Resin Transfer Molding

by Rudá Aranha, Mario A. Albuquerque Filho, Cícero de Lima Santos, Viviane M. Fonseca, José L. V. Rivera, Antonio G. B. de Lima, Wanderley F. de Amorim, Jr. and Laura H. Carvalho

Polymers 2023, 15(22), 4438; https://doi.org/10.3390/polym15224438 - 16 Nov 2023

Cited by 1 | Viewed by 738

Abstract

The aim of this work is to analyze water sorption in hybrid polyester/glass fabric/jute fabric composites molded via compression and VARTM (Vacuum-Assisted Resin Transfer Molding). The laminates were produced with five different stacking sequences and subjected to water sorption testing at room temperature, 50 °C and 70 °C. This study consisted of two stages: experimental and theoretical stages. The composites had a fiber volume content ranging from 30% to 40%. Water absorption and diffusion coefficient in the hybrid composites were intermediate to those reinforced with a single type of fiber. There were no significant differences in these properties based on fiber arrangement once the composites reached saturation. Diffusion coefficient values were higher for specimens with jute fiber on at least one of the outer surfaces. Water sorption rates increased with higher immersion temperatures. The water sorption at saturation point was not affected by the manufacturing process. Among the hybrid composites, those with jute on the surfaces showed the highest diffusion coefficient, while those with glass on the surface had the lowest values. Higher diffusion coefficient values were observed at temperatures of 50 °C and 70 °C. The main influencing factors on the absorbed moisture content for composites are the presence and content of jute fibers in the system and the immersion temperature. The manufacturing process does not affect the water sorption at saturation point. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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16 pages, 7894 KiB

Open AccessArticle

Dry Friction and Wear Behavior of Laser-Sintered Graphite/Carbon Fiber/Polyamide 12 Composite

by Abdelrasoul Gadelmoula and Saleh Ahmed Aldahash

Polymers 2023, 15(19), 3916; https://doi.org/10.3390/polym15193916 - 28 Sep 2023

Cited by 2 | Viewed by 856

Abstract

Carbon fiber-reinforced polymers (CFRPs) are being used extensively in modern industries that require a high strength-to-weight ratio, such as aerospace, automotive, motorsport, and sports equipment. However, although reinforcement with carbon fibers improves the mechanical properties of polymers, this comes at the expense of abrasive wear resistance. Therefore, to efficiently utilize CFRPs in dry sliding contacts, solid lubricant is used as a filler. Further, to facilitate the fabrication of objects with complex geometries, selective laser sintering (SLS) can be employed. Accordingly, in the present work, graphite-filled carbon fiber-reinforced polyamide 12 (CFR-PA12) specimens were prepared using the SLS process to explore the dry sliding friction and wear characteristics of the composite. The test specimens were aligned along four different orientations in the build chamber of the SLS machine to determine the orientation-dependent tribological properties. The experiments were conducted using a pin-on-disc tribometer to measure the coefficient of friction (COF), interface temperature, friction-induced noise, and specific wear rate. In addition, scanning electron microscopy (SEM) of tribo-surfaces was conducted to specify the dominant wear pattern. The results indicated that the steady-state COF, contact temperature, and wear pattern of graphite-filled CFR-PA12 are orientation-independent and that the contact temperature is likely to approach an asymptote far below the glass transition temperature of amorphous PA12 zones, thus eliminating the possibility of matrix softening. Additionally, the results showed that the Z-oriented specimen exhibits the lowest level of friction-induced noise along with the highest wear resistance. Moreover, SEM of tribo-surfaces determined that abrasive wear is the dominant wear pattern. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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13 pages, 6527 KiB

Open AccessArticle

Cohesive Zone Modeling of Pull-Out Test for Dental Fiber–Silicone Polymer

by Ayman M. Maqableh and Muhanad M. Hatamleh

Polymers 2023, 15(18), 3668; https://doi.org/10.3390/polym15183668 - 06 Sep 2023

Viewed by 879

Abstract

Background: Several analytical methods for the fiber pull-out test have been developed to evaluate the bond strength of fiber–matrix systems. We aimed to investigate the debonding mechanism of a fiber–silicone pull-out specimen and validate the experimental data using 3D-FEM and a cohesive element approach. Methods: A 3D model of a fiber–silicone pull-out testing specimen was established by pre-processing CT images of the typical specimen. The materials on the scans were posted in three different cross-sectional views using ScanIP and imported to ScanFE in which 3D generation was implemented for all of the image slices. This file was exported in FEA format and was imported in the FEA software (PATRAN/ABAQUS, version r2) for generating solid mesh, boundary conditions, and material properties attribution, as well as load case creation and data processing. Results: The FEM cohesive zone pull-out force versus displacement curve showed an initial linear response. The Von Mises stress concentration was distributed along the fiber–silicone interface. The damage in the principal stresses’ directions S11, S22, and S33, which represented the maximum possible magnitude of tensile and compressive stress at the fiber–silicone interface, showed that the stress is higher in the direction S33 (stress acting in the Z-direction) in which the lower damage criterion was higher as well when compared to S11 (stress acting in the XY plane) and S23 (stress acting in the YZ plane). Conclusions: The comparison between the experimental values and the results from the finite element simulations show that the proposed cohesive zone model accurately reproduces the experimental results. These results are considered almost identical to the experimental observations about the interface. The cohesive element approach is a potential function that takes into account the shear effects with many advantages related to its ability to predict the initiation and progress of the fiber–silicone debonding during pull-out tests. A disadvantage of this approach is the computational effort required for the simulation and analysis process. A good understanding of the parameters related to the cohesive laws is responsible for a successful simulation. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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15 pages, 5512 KiB

Open AccessArticle

Thermal Properties and In Vitro Biodegradation of PLA-Mg Filaments for Fused Deposition Modeling

by Adrián Leonés, Valentina Salaris, Ignacio Ramos Aranda, Marcela Lieblich, Daniel López and Laura Peponi

Polymers 2023, 15(8), 1907; https://doi.org/10.3390/polym15081907 - 16 Apr 2023

Cited by 4 | Viewed by 1289

Abstract

Additive manufacturing, in particular the fused deposition method, is a quite new interesting technique used to obtain specific 3D objects by depositing layer after layer of material. Generally, commercial filaments can be used in 3D printing. However, the obtention of functional filaments is not so easy to reach. In this work, we obtain filaments based on poly(lactic acid), PLA, reinforced with different amounts of magnesium, Mg, microparticles, using a two-step extrusion process, in order to study how processing can affect the thermal degradation of the filaments; we additionally study their in vitro degradation, with a complete release of Mg microparticles after 84 days in phosphate buffer saline media. Therefore, considering that we want to obtain a functional filament for further 3D printing, the simpler the processing, the better the result in terms of a scalable approach. In our case, we obtain micro-composites via the double-extrusion process without degrading the materials, with good dispersion of the microparticles into the PLA matrix without any chemical or physical modification of the microparticles. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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13 pages, 6785 KiB

Open AccessCommunication

One-Step Low Temperature Synthesis of CeO₂ Nanoparticles Stabilized by Carboxymethylcellulose

by Vasily V. Spiridonov, Andrey V. Sybachin, Vladislava A. Pigareva, Mikhail I. Afanasov, Sharifjon A. Musoev, Alexander V. Knotko and Sergey B. Zezin

Polymers 2023, 15(6), 1437; https://doi.org/10.3390/polym15061437 - 14 Mar 2023

Cited by 2 | Viewed by 1608

Abstract

An elegant method of one-pot reaction at room temperature for the synthesis of nanocomposites consisting of cerium containing nanoparticles stabilized by carboxymethyl cellulose (CMC) macromolecules was introduced. The characterization of the nanocomposites was carried out with a combination of microscopy, XRD, and IR spectroscopy analysis. The type of crystal structure of inorganic nanoparticles corresponding to CeO₂ was determined and the mechanism of nanoparticle formation was suggested. It was demonstrated that the size and shape of the nanoparticles in the resulting nanocomposites does not depend on the ratio of the initial reagents. Spherical particles with a mean diameter 2–3 nm of were obtained in different reaction mixtures with a mass fraction of cerium from 6.4 to 14.1%. The scheme of the dual stabilization of CeO₂ nanoparticles with carboxylate and hydroxyl groups of CMC was proposed. These findings demonstrate that the suggested easily reproducible technique is promising for the large-scale development of nanoceria-containing materials. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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17 pages, 6197 KiB

Open AccessArticle

Centrifugal Force-Spinning to Obtain Multifunctional Fibers of PLA Reinforced with Functionalized Silver Nanoparticles

by María Dolores Martín-Alonso, Valentina Salaris, Adrián Leonés, Víctor Hevilla, Alexandra Muñoz-Bonilla, Coro Echeverría, Marta Fernández-García, Laura Peponi and Daniel López

Polymers 2023, 15(5), 1240; https://doi.org/10.3390/polym15051240 - 28 Feb 2023

Cited by 3 | Viewed by 1460

Abstract

The design and development of multifunctional fibers awakened great interest in biomaterials and food packaging materials. One way to achieve these materials is by incorporating functionalized nanoparticles into matrices obtained by spinning techniques. Here, a procedure for obtaining functionalized silver nanoparticles through a green protocol, using chitosan as a reducing agent, was implemented. These nanoparticles were incorporated into PLA solutions to study the production of multifunctional polymeric fibers by centrifugal force-spinning. Multifunctional PLA-based microfibers were obtained with nanoparticle concentrations varying from 0 to 3.5 wt%. The effect of the incorporation of nanoparticles and the method of preparation of the fibers on the morphology, thermomechanical properties, biodisintegration, and antimicrobial behavior, was investigated. The best balance in terms of thermomechanical behavior was obtained for the lowest amount of nanoparticles, that is 1 wt%. Furthermore, functionalized silver nanoparticles confer antibacterial activity to the PLA fibers, with a percentage of killing bacteria between 65 and 90%. All the samples turned out to be disintegrable under composting conditions. Additionally, the suitability of the centrifugal force-spinning technique for producing shape-memory fiber mats was tested. Results demonstrate that with 2 wt% of nanoparticles a good thermally activated shape-memory effect, with high values of fixity and recovery ratios, is obtained. The results obtained show interesting properties of the nanocomposites to be applied as biomaterials. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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17 pages, 2623 KiB

Open AccessArticle

Characterization of PLA/PCL/Nano-Hydroxyapatite (nHA) Biocomposites Prepared via Cold Isostatic Pressing

by Solechan Solechan, Agus Suprihanto, Susilo Adi Widyanto, Joko Triyono, Deni Fajar Fitriyana, Januar Parlaungan Siregar and Tezara Cionita

Polymers 2023, 15(3), 559; https://doi.org/10.3390/polym15030559 - 21 Jan 2023

Cited by 12 | Viewed by 2368

Abstract

Hydroxyapatite has the closest chemical composition to human bone. Despite this, the use of nano-hydroxyapatite (nHA) to produce biocomposite scaffolds from a mixture of polylactic acid (PLA) and polycaprolactone (PCL) using cold isostatic pressing has not been studied intensively. In this study, biocomposites were created employing nHA as an osteoconductive filler and a polymeric blend of PLA and PCL as a polymer matrix for prospective usage in the medical field. Cold isostatic pressing and subsequent sintering were used to create composites with different nHA concentrations that ranged from 0 to 30 weight percent. Using physical and mechanical characterization techniques such as Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and density, porosity, tensile, and flexural standard tests, it was determined how the nHA concentrations affected the biocomposite’s general properties. In this study, the presence of PLA, PCL, and nHA was well identified using FTIR, XRD, and SEM methods. The biocomposites with high nHA content showed intense bands for symmetric stretching and the asymmetric bending vibration of PO₄³⁻. The incorporation of nHA into the polymeric blend matrix resulted in a rather irregular structure and the crystallization became more difficult. The addition of nHA improved the density and tensile and flexural strength of the PLA/PCL matrix (0% nHA). However, with increasing nHA content, the PLA/PCL/nHA biocomposites became more porous. In addition, the density, flexural strength, and tensile strength of the PLA/PCL/nHA biocomposites decreased with increasing nHA concentration. The PLA/PCL/nHA biocomposites with 10% nHA had the highest mechanical properties with a density of 1.39 g/cm³, a porosity of 1.93%, a flexural strength of 55.35 MPa, and a tensile strength of 30.68 MPa. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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8 pages, 2644 KiB

Open AccessArticle

Polyzwitterion–SiO₂ Double-Network Polymer Electrolyte with High Strength and High Ionic Conductivity

by Lei Zhang, Haiqi Gao, Lixiang Guan, Yuchao Li and Qian Wang

Polymers 2023, 15(2), 466; https://doi.org/10.3390/polym15020466 - 16 Jan 2023

Cited by 2 | Viewed by 1488

Abstract

The key to developing high-performance polymer electrolytes (PEs) is to achieve their high strength and high ionic conductivity, but this is still challenging. Herein, we designed a new double-network PE based on the nonhydrolytic sol–gel reaction of tetraethyl orthosilicate and in situ polymerization of zwitterions. The as-prepared PE possesses high strength (0.75 Mpa) and high stretchability (560%) due to the efficient dissipation energy of the inorganic network and elastic characteristics of the polymer network. In addition, the highest ionic conductivity of the PE reaches 0.44 mS cm⁻¹ at 30 °C owning to the construction of dynamic ion channels between the polyzwitterion segments and between the polyzwitterion segments and ionic liquids. Furthermore, the inorganic network can act as Lewis acid to adsorb trace impurities, resulting in a prepared electrolyte with a high electrochemical window over 5 V. The excellent interface compatibility of the as-prepared PE with a Li metal electrode is also confirmed. Our work provides new insights into the design and preparation of high-performance polymer-based electrolytes for solid-state energy storage devices. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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Review

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20 pages, 2473 KiB

Open AccessReview

A Review of Electrospun Nanofiber Interleaves for Interlaminar Toughening of Composite Laminates

by Biltu Mahato, Stepan V. Lomov, Aleksei Shiverskii, Mohammad Owais and Sergey G. Abaimov

Polymers 2023, 15(6), 1380; https://doi.org/10.3390/polym15061380 - 10 Mar 2023

Cited by 7 | Viewed by 1725

Abstract

Recently, polymeric nanofiber veils have gained lot of interest for various industrial and research applications. Embedding polymeric veils has proven to be one of the most effective ways to prevent delamination caused by the poor out-of-plane properties of composite laminates. The polymeric veils are introduced between plies of a composite laminate, and their targeted effects on delamination initiation and propagation have been widely studied. This paper presents an overview of the application of nanofiber polymeric veils as toughening interleaves in fiber-reinforced composite laminates. It presents a systematic comparative analysis and summary of attainable fracture toughness improvements based on electrospun veil materials. Both Mode I and Mode II tests are covered. Various popular veil materials and their modifications are considered. The toughening mechanisms introduced by polymeric veils are identified, listed, and analyzed. The numerical modeling of failure in Mode I and Mode II delamination is also discussed. This analytical review can be used as guidance for veil material selection, for estimation of the achievable toughening effect, for understanding the toughening mechanism introduced by veils, and for the numerical modeling of delamination. Full article

(This article belongs to the Special Issue Organic-Inorganic Hybrid Materials III)

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