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1. Grafted Nanoparticle Surface Wetting during Phase Separation in Polymer Nanocomposite Films

Author

Cherie R. Kagan, John D. Demaree, Connor Bilchak, Patrice Rannou, Christopher B. Murray, Michael J. Boyle, Nadia M. Krook, Kohji Ohno, Shawn Maguire, Austin W Keller, Russell J. Composto, School of Engineering and Applied Science [University of Pennsylvania], University of Pennsylvania [Philadelphia], U.S. Army Research Laboratory [Adelphi, MD] (ARL), United States Army (U.S. Army), DuPont Company, Institute for Chemical Research, Kyoto University (KUICR), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP ), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and University of Pennsylvania

Subjects
Materials science, Polymer nanocomposite, surface segregation, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Lower critical solution temperature, polymer nanocomposites, [CHIM]Chemical Sciences, General Materials Science, Dewetting, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, polymer surfaces, ComputingMilieux_MISCELLANEOUS, [PHYS]Physics [physics], wetting, diffusion, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Rutherford backscattering spectrometry, Surface energy, 0104 chemical sciences, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, Polymer blend, Wetting, grafted nanoparticles, 0210 nano-technology
Abstract

International audience; Wetting of polymer-grafted nanoparticles (NPs) in a polymer nanocomposite (PNC) film is driven by a difference in surface energy between components as well as bulk thermodynamics, namely, the value of the interaction parameter, χ. The interplay between these contributions is investigated in a PNC containing 25 wt % polymethyl methacrylate (PMMA)-grafted silica NPs (PMMA-NPs) in poly(styrene-ran-acrylonitrile) (SAN) upon annealing above the lower critical solution temperature (LCST, 160 °C). Atomic force microscopy (AFM) studies show that the areal density of particles increases rapidly and then approaches 80% of that expected for random close-packed hard spheres. A slightly greater areal density is observed at 190 °C compared to 170 °C. The PMMA-NPs are also shown to prevent dewetting of PNC films under conditions where the analogous polymer blend is unstable. Transmission electron microscopy (TEM) imaging shows that PMMANPs symmetrically wet both interfaces and form columns that span the free surface and substrate interface. Using grazingincidence Rutherford backscattering spectrometry (GI-RBS), the PMMA-NP surface excess (Z*) initially increases rapidly with time and then approaches a constant value at longer times. Consistent with the areal density, Z* is slightly greater at deeper quench depths, which is attributed to the more unfavorable interactions between the PMMA brush and SAN segments. The Z* values at early times are used to determine the PMMA-NP diffusion coefficients, which are significantly larger than theoretical predictions. These studies provide insights into the interplay between wetting and phase separation in PNCs and can be utilized in nanotechnology applications where surface-dependent properties, such as wettability, durability, and friction, are important.

Published
2021
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2. Interfacial Compatibilization in Ternary Polymer Nanocomposites: Comparing Theory and Experiments

Author

Patrice Rannou, Manuel Maréchal, Nadia M. Krook, Andreea-Maria Pana, Arthi Jayaraman, Arjita Kulshreshtha, Russell J. Composto, Connor Bilchak, Shawn Maguire, Robert Brosnan, Kohji Ohno, School of Engineering and Applied Science [University of Pennsylvania], University of Pennsylvania [Philadelphia], DuPont Company, Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP ), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes (UGA), Department of Chemical and Biomolecular Engineering, University of Pennsylvania, Institute for Chemical Research, Kyoto University (KUICR), Department of Chemical and Biomolecular Engineering, University of Delaware, University of Delaware [Newark], Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), University of Pennsylvania, and ANR-15-PIRE-0001,REACT,Research and Education in Active Coatings Technologies for human habitat(2015)

Subjects
Materials science, Polymers and Plastics, Polymer nanocomposite, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Miscibility, Inorganic Chemistry, chemistry.chemical_compound, Materials Chemistry, [CHIM]Chemical Sciences, Methyl methacrylate, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, [PHYS]Physics [physics], Nanocomposite, Organic Chemistry, Polymer, Compatibilization, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, 0210 nano-technology, Ternary operation
Abstract

International audience; In this work, we examine binary and ternary nanocomposites of poly(methyl methacrylate) grafted silica nanoparticles (PMMA-NP), in poly(styrene-ran-acrylonitrile) (SAN), and poly(methyl methacrylate) matrices as a platform to directly probe governing parameters guiding phase behavior and nanoparticle assembly in composite materials. Through the addition of PMMA matrix chains similar in molecular weight to the grafted PMMA chains and significantly smaller than the SAN matrix chains, we observe increased nanoparticle miscibility in off-critical compositions due to interfacial segregation of PMMA matrix chains. A simple interfacial model provides a general guideline for predicting the extent of compatibilization. Further insights on compatibilization behavior are provided by polymer particle pair correlation functions and structure factors obtained using polymer reference interaction site model theory calculations as well as polymer concentration profiles from molecular dynamics simulations. This study serves as a guideline to facilitate PNC processing and design of materials for a broad range of technological applications.

Published
2021
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3. Thermodynamics of Binary and Ternary Polymer Blend Nanocomposites

Author

Shawn Maguire, Krook, Nadia M., Patrice Rannou, Manuel Maréchal, Kohji Ohno, Kristen Brosnan, Composto, Russell J., Synthèse, Structure et Propriétés de Matériaux Fonctionnels (STEP), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Département Interfaces pour l'énergie, la Santé et l'Environnement (DIESE), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Institute for Chemical Research, Kyoto University (KUICR), University of Pennsylvania [Philadelphia], Maréchal, Manuel, Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and University of Pennsylvania

Subjects
[CHIM] Chemical Sciences, [CHIM]Chemical Sciences, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2019

4. Grafting of Polymer Brushes from Silica Particles Functionalized with Xanthates

Author

Ohno, Kohji, Yahata, Yoshikazu, Sakaue, Motokazu, Ladmiral, Vincent, Institute for Chemical Research, Kyoto University (KUICR), Kyoto University [Kyoto], Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC), and This work was supported in part by a Grant‐in‐Aid for Scientific Research (Grant‐in‐Aid 17685010 and 23685049) from the Ministry of Education, Culture, Sports, Science, and Technology, Japan.

Subjects
xanthates, colloids, polymerization, [CHIM]Chemical Sciences, polymer brushes, polymers
Abstract

International audience; Monodisperse silica particles (SiPs) were surface‐modified with a newly designed silane coupling agent comprising a triethoxysilane and an alkyl halide, namely, 6‐(triethoxysilyl)hexyl 2‐bromopropionate, which was further treated with potassium O‐ethyl dithiocarbonate (PEX) to immobilize xanthate molecules on the particle surfaces. Surface‐initiated macromolecular design via interchange of xanthates (MADIX) polymerization of vinyl acetate (VAc) was conducted with the xanthate‐functionalized SiPs. The polymerization was well controlled and produced SiPs coated with poly(vinyl acetate) (PVAc) with a well‐defined target molar mass and a graft density of about 0.2 chains nm−2. Dynamic light scattering and TEM measurements revealed that the hybrid particles were highly dispersible in good solvents without any aggregation. The PVAc brushes were hydrolyzed with hydrochloric acid to produce poly(vinyl alcohol) brushes on the SiP surfaces. In addition, the number of xanthate molecules introduced on the SiP surfaces could be successfully controlled by adjusting the concentration of PEX. Thus, the SiPs have two functionalities: xanthates able to act as a MADIX chain‐transfer agent and alkyl bromide initiation sites for atom transfer radical polymerization (ATRP). By using these unique bifunctional particles, mixed polymer brushes were constructed on the SiPs by MADIX of VAc followed by ATRP of styrene or methyl methacrylate.

Published
2019
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