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Polymers
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Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization
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Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization

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

Deadline for manuscript submissions: closed (15 January 2024) | Viewed by 8828

Special Issue Editors

Dr. Francesca Martini

E-Mail Website
Guest Editor
Dipartimento di Chimica e Chimica Industriale, Università di Pisa, 56124 Pisa, Italy
Interests: solid-state NMR; field cycling NMR; material characterization; structure and dynamic properties
Dr. Francesca Nardelli

E-Mail Website
Guest Editor
Istituto di Chimica dei Composti Organometallici, Consiglio Nazionale delle Ricerche (CNR), 56124 Pisa, Italy
Interests: solid-state NMR; low field NMR; polymeric material characterization; structure and dynamic properties

Special Issue Information

Dear Colleagues,

The urgent need for the transition to a more sustainable and green economy is pushing scientific research toward the design and development of new eco-friendly materials for advanced technological applications in various fields. In this frame, polymer-based materials play a central role thanks to their low cost, versatility, easy processability, and tunable properties. The development of new materials with efficient performances requires achieving an in-depth comprehension of the structural and dynamic features at the molecular level. To this end, advanced spectroscopic methodologies for material characterization, able to disclose the complex structure-property relationship, are necessary. 

This Special Issue aims to gather a collection of original research articles and reviews on the characterization of polymer-based materials via advanced spectroscopic methods, including but not only limited to solid-state NMR, field cycling NMR, dielectric spectroscopy, IR spectroscopy, light and neutron scattering techniques, and optical spectroscopy.

We would like to invite you to submit works to this Special Issue to share your most recent results and methodological developments in the field of polymer analysis and characterization.

Dr. Francesca Martini
Dr. Francesca Nardelli
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Polymers is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • polymers
  • material characterization
  • spectroscopic techniques
  • solid-state NMR
  • field cycling NMR
  • dielectric spectroscopy
  • IR spectroscopy
  • light scattering
  • neutron scattering
  • optical spectroscopy

Published Papers (7 papers)

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Research

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18 pages, 3842 KiB  
Article
Exploring the Effect of Resins of Different Origin on the Structure, Dynamics and Curing Characteristics of SBR Compounds
by Michele Pierigé, Francesca Nardelli, Lucia Calucci, Mattia Cettolin, Luca Giannini, Andrea Causa, Francesca Martini and Marco Geppi
Polymers 2024, 16(6), 834; https://doi.org/10.3390/polym16060834 - 18 Mar 2024
Viewed by 582
Abstract
The replacement of synthetic and petroleum-based ingredients with greener alternatives of natural origin is an imperative issue in rubber technology for the tire industry. In this study, a glycerin-esterified maleated rosin resin, derived from natural resources, is examined as a potential tackifier in [...] Read more.
The replacement of synthetic and petroleum-based ingredients with greener alternatives of natural origin is an imperative issue in rubber technology for the tire industry. In this study, a glycerin-esterified maleated rosin resin, derived from natural resources, is examined as a potential tackifier in styrene–butadiene rubber (SBR) formulations. A comparison is made with two synthetic resins commonly used as tackifiers in tire manufacturing: a petroleum-derived aromatic resin and a phenolic resin. Specifically, this research investigates how these resins affect the structure, dynamics, and curing characteristics of SBR compounds, which are strictly related to the mechanical and technological properties of the final products. Moving die rheometer and equilibrium swelling experiments are employed to analyze vulcanization kinetics and crosslink density, which are differently influenced by the different resins. Information on the polymer–resin compatibility is gained by differential scanning calorimetry and dynamo-mechanical analysis, while solid-state NMR methods offer insights into the structure and dynamics of both cured and uncured SBR compounds at the molecular level. Overall, our analysis shows that the resin of vegetal origin has a comparable impact on the SBR compound to that observed for the synthetic resins and could be further tested for industrial applications. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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12 pages, 1821 KiB  
Article
Effect of Polymer Composition on the Optical Properties of a New Aggregation-Induced Emission Fluorophore: A Combined Experimental and Computational Approach
by Alberto Picchi, Qinfan Wang, Francesco Ventura, Cosimo Micheletti, Jesse Heijkoop, Francesco Picchioni, Ilaria Ciofini, Carlo Adamo and Andrea Pucci
Polymers 2023, 15(17), 3530; https://doi.org/10.3390/polym15173530 - 24 Aug 2023
Viewed by 1184
Abstract
Nowadays, fluorophores with a tetraphenylethylene (TPE) core are considered interesting due to the aggregation-induced emission (AIE) behavior that enables their effective use in polymer films. We propose a novel TPE fluorophore (TPE-BPAN) bearing two dimethylamino push and a 4-biphenylacetonitrile pull moieties [...] Read more.
Nowadays, fluorophores with a tetraphenylethylene (TPE) core are considered interesting due to the aggregation-induced emission (AIE) behavior that enables their effective use in polymer films. We propose a novel TPE fluorophore (TPE-BPAN) bearing two dimethylamino push and a 4-biphenylacetonitrile pull moieties with the typical AIE characteristics in solution and in the solid state, as rationalized by DFT calculations. Five different host polymer matrices with different polarity have been selected: two homopolymers of poly(methylmethacrylate) (PMMA) and poly(cyclohexyl methacrylate) (PCHMA) and three copolymers at different compositions (P(MMA-co-CHMA) 75:25, 50:50, and 25:75 mol%). The less polar comonomer of CHMA appeared to enhance TPE-BPAN emission with the highest quantum yield (QY) of about 40% measured in P(MMA-co-CHMA) 75:25. Further reduction in polymer polarity lowered QY and decreased the film stability and adhesion to the glass surface. LSC performances were not significantly affected by the matrix’s polarity and resulted in around one-third of the state-of-the-art due to the reduced QY of TPE-BPAN. The theoretical investigation based on density functional theory (DFT) calculations clarified the origin of the observed AIE and the role played by the environment in modulating the photophysical behavior. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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7 pages, 1966 KiB  
Communication
Assessing the Quality of Oxygen Plasma Focused Ion Beam (O-PFIB) Etching on Polypropylene Surfaces Using Secondary Electron Hyperspectral Imaging
by Nicholas T. H. Farr, Maciej Pasniewski and Alex de Marco
Polymers 2023, 15(15), 3247; https://doi.org/10.3390/polym15153247 - 30 Jul 2023
Viewed by 846
Abstract
The development of Focused Ion Beam–Scanning Electron Microscopy (FIB-SEM) systems has provided significant advances in the processing and characterization of polymers. A fundamental understanding of ion–sample interactions is still missing despite FIB-SEM being routinely applied in microstructural analyses of polymers. This study applies [...] Read more.
The development of Focused Ion Beam–Scanning Electron Microscopy (FIB-SEM) systems has provided significant advances in the processing and characterization of polymers. A fundamental understanding of ion–sample interactions is still missing despite FIB-SEM being routinely applied in microstructural analyses of polymers. This study applies Secondary Electron Hyperspectral Imaging to reveal oxygen and xenon plasma FIB interactions on the surface of a polymer (in this instance, polypropylene). Secondary Electron Hyperspectral Imaging (SEHI) is a technique housed within the SEM chamber that exhibits multiscale surface sensitivity with a high spatial resolution and the ability to identify carbon bonding present using low beam energies without requiring an Ultra High Vacuum (UHV). SEHI is made possible through the use of through-the-lens detectors (TLDs) to provide a low-pass SE collection of low primary electron beam energies and currents. SE images acquired over the same region of interest from different energy ranges are plotted to produce an SE spectrum. The data provided in this study provide evidence of SEHI’s ability to be a valuable tool in the characterization of polymer surfaces post-PFIB etching, allowing for insights into both tailoring polymer processing FIB parameters and SEHI’s ability to be used to monitor serial FIB polymer surfaces in situ. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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17 pages, 3475 KiB  
Article
Advanced Particle Size Analysis in High-Solid-Content Polymer Dispersions Using Photon Density Wave Spectroscopy
by Stephanie Schlappa, Lena Bressel, Oliver Reich and Marvin Münzberg
Polymers 2023, 15(15), 3181; https://doi.org/10.3390/polym15153181 - 26 Jul 2023
Cited by 2 | Viewed by 985
Abstract
High-solid-content polystyrene and polyvinyl acetate dispersions of polymer particles with a 50 nm to 500 nm mean particle diameter and 12–55% (w/w) solid content have been produced via emulsion polymerization and characterized regarding their optical and physical properties. Both [...] Read more.
High-solid-content polystyrene and polyvinyl acetate dispersions of polymer particles with a 50 nm to 500 nm mean particle diameter and 12–55% (w/w) solid content have been produced via emulsion polymerization and characterized regarding their optical and physical properties. Both systems have been analyzed with common particle-size-measuring techniques like dynamic light scattering (DLS) and static light scattering (SLS) and compared to inline particle size distribution (PSD) measurements via photon density wave (PDW) spectroscopy in undiluted samples. It is shown that particle size measurements of undiluted polystyrene dispersions are in good agreement between analysis methods. However, for polyvinyl acetate particles, size determination is challenging due to bound water in the produced polymer. For the first time, water-swelling factors were determined via an iterative approach of PDW spectroscopy error (Χ2) minimization. It is shown that water-swollen particles can be analyzed in high-solid-content solutions and their physical properties can be assumed to determine the refractive index, density, and volume fraction in dispersion. It was found that assumed water swelling improved the reduced scattering coefficient fit by PDW spectroscopy by up to ten times and particle size determination was refined and enabled. Particle size analysis of the water-swollen particles agreed well with offline-based state-of-the-art techniques. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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21 pages, 5124 KiB  
Article
Multi-Spectroscopic Characterization of MgO/Nylon (6/6) Polymer: Evaluating the Potential of LIBS and Statistical Methods
by Amir Fayyaz, Haroon Asghar, Muhammad Waqas, Asif Kamal, Wedad A. Al-Onazi and Amal M. Al-Mohaimeed
Polymers 2023, 15(15), 3156; https://doi.org/10.3390/polym15153156 - 25 Jul 2023
Cited by 1 | Viewed by 2063
Abstract
The potential of using laser-induced breakdown spectroscopy (LIBS) in combination with various other spectroscopic and statistical methods was assessed for characterizing pure and MgO-doped nylon (6/6) organic polymer samples. The pure samples, obtained through a polycondensation chemical technique, were artificially doped with MgO [...] Read more.
The potential of using laser-induced breakdown spectroscopy (LIBS) in combination with various other spectroscopic and statistical methods was assessed for characterizing pure and MgO-doped nylon (6/6) organic polymer samples. The pure samples, obtained through a polycondensation chemical technique, were artificially doped with MgO prior to analysis for comparative purposes. These artificially doped samples served as crucial reference materials for comparative analysis and reference purposes. The LIBS studies were performed under local thermodynamic equilibrium (LTE) and optically thin plasma conditions. To assess the structural crystallinity of the nylon (6/6) polymer samples, X-ray diffraction (XRD) analysis, and Fourier transform infrared (FTIR) spectroscopy were employed to detect functional groups such as N-H, C-H, and C-N in the adsorbent polyamide nylon sample. Additionally, diffuse reflectance spectroscopy (DRS) analysis was conducted to investigate the effects of doping and temperature on the band gap and material reflectance across different sample temperatures. Chemical compositional analysis was performed using X-ray photoelectron spectroscopy (XPS) with the carbon C1s peak at 248.8 eV serving as a reference for spectrum calibration, along with energy-dispersive X-ray (EDX) analysis, which demonstrated good agreement between the techniques. To validate the different methodologies, the results obtained from CF-LIBS and EDX were compared with those from the standard inductively coupled plasma mass spectrometry (ICP-MS) technique. Finally, for classification analysis, principal component analysis (PCA) was applied to the LIBS spectral data at different sample temperatures (25 °C, 125 °C, 225 °C, and 325 °C). The analyses demonstrated that the combination of LIBS with PCA, along with other methods, presents a robust technique for polymer characterization. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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17 pages, 976 KiB  
Article
Combining Experimental and Theoretical Tools to Probe Radio-Oxidation Products in Polyethylene
by Muriel Ferry, Yunho Ahn, Florian Le Dantec, Yvette Ngono and Guido Roma
Polymers 2023, 15(6), 1537; https://doi.org/10.3390/polym15061537 - 20 Mar 2023
Cited by 1 | Viewed by 957
Abstract
Polyethylene is one of the most used polymers in a variety of sectors. A typical technique used to assess aging is infrared spectroscopy. Under oxidation, the region of the spectrum that is most studied is the one containing the carbonyl signature. However, various [...] Read more.
Polyethylene is one of the most used polymers in a variety of sectors. A typical technique used to assess aging is infrared spectroscopy. Under oxidation, the region of the spectrum that is most studied is the one containing the carbonyl signature. However, various carbonyl groups contribute to the carbonyl peak: ketones, aldehydes, esters, lactones, carboxylic acids, and more. A usual procedure to quantify each of them is the deconvolution of experimental peaks based on experimental assignments of infrared bands. In this paper, we complement this procedure, applied to two polyethylene types, with extended density functional theory (DFT) calculations of infrared spectra, using a polyethylene model mimicking the main features of a semicrystalline polymer. We compare theoretical frequencies and infrared intensities with parameters extracted from the literature that are used to, eventually, estimate concentrations. We provide an alternative estimation entirely based on theoretical data, showing that DFT can be a valuable tool to analyze, or at least complement, experimental data to assess polymer aging. The comparison of different deconvolution procedures raises the question of the contribution of conjugated ketones in the global carbonyl buildup, as well as that of ketones/alcohols pairs, or the relative concentration of esters and aldehydes. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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Review

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24 pages, 4222 KiB  
Review
Probing the Free Volume in Polymers by Means of Positron Annihilation Lifetime Spectroscopy
by Giovanni Consolati, Dario Nichetti and Fiorenza Quasso
Polymers 2023, 15(14), 3128; https://doi.org/10.3390/polym15143128 - 23 Jul 2023
Cited by 5 | Viewed by 1590
Abstract
Positron annihilation lifetime spectroscopy (PALS) is a valuable technique to investigate defects in solids, such as vacancy clusters and grain boundaries in metals and alloys, as well as lattice imperfections in semiconductors. Positron spectroscopy is able to reveal the size, structure and concentration [...] Read more.
Positron annihilation lifetime spectroscopy (PALS) is a valuable technique to investigate defects in solids, such as vacancy clusters and grain boundaries in metals and alloys, as well as lattice imperfections in semiconductors. Positron spectroscopy is able to reveal the size, structure and concentration of vacancies with a sensitivity of 10−7. In the field of porous and amorphous systems, PALS can probe cavities in the range from a few tenths up to several tens of nm. In the case of polymers, PALS is one of the few techniques able to give information on the holes forming the free volume. This quantity, which cannot be measured with macroscopic techniques, is correlated to important mechanical, thermal, and transport properties of polymers. It can be deduced theoretically by applying suitable equations of state derived by cell models, and PALS supplies a quantitative measure of the free volume by probing the corresponding sub-nanometric holes. The system used is positronium (Ps), an unstable atom formed by a positron and an electron, whose lifetime can be related to the typical size of the holes. When analyzed in terms of continuous lifetimes, the positron annihilation spectrum allows one to gain insight into the distribution of the free volume holes, an almost unique feature of this technique. The present paper is an overview of PALS, addressed in particular to readers not familiar with this technique, with emphasis on the experimental aspects. After a general introduction on free volume, positronium, and the experimental apparatus needed to acquire the corresponding lifetime, some of the recent results obtained by various groups will be shown, highlighting the connections between the free volume as probed by PALS and structural properties of the investigated materials. Full article
(This article belongs to the Special Issue Advanced Spectroscopy Methods in Polymer-Based Materials Analysis and Characterization)
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