Supported Ionic Liquid-Phase Materials (SILP) as a Multifunctional Group of Highly Stable Modifiers and Hardeners for Carbon and Flax Epoxy Composites.

This paper introduces a novel approach to enhance epoxy resin formulations by using SILP materials as multifunctional hardeners and fillers in composite structures reinforced with carbon and flax fibers. This study explores the integration of ionic liquids (ILs) onto a silica support structure, presenting various permutations involving silica selection, ionic liquid choice, and concentration. The focus of this study was to elucidate the influence of SILP on resin curing ability and the mechanical properties of the resulting composites. Detailed research was conducted, including Brunauer-Emmett-Teller analysis (BET) for SILP materials and curing characterization for epoxy resin formulations with different SILP materials. Furthermore, the mechanical properties of the obtained composites were determined by Scanning Electron Microscopy analysis (SEM) (the force at break, the maximum elongation at break, tensile strength, and modulus of elasticity). Through SILP incorporation, the mechanical properties of composites, including the modulus of elasticity and tensile strength, are substantially improved, a phenomenon akin to traditional filler effects. The findings highlight SILP materials as prospective candidates for concurrent hardening and filling roles within composites (through a single-step procedure, with prolonged storage stability and controlled processing conditions), particularly pertinent as the composite industry veers toward epoxy bioresins necessitating liquefaction via temperature application.

Grism fabricated on the end-face of an optical fiber.

We designed and fabricated grism structures on the end-face of an optical fiber and experimentally characterized them. A UV-curable ionic-liquid polymer resin, well-suited for nanoimprinting, was used to fabricate the grism structures with grating pitches of 1.8-3 µm and prism apex angle reaching 30-40°. The structures can propagate 1st order of diffraction peaks along the fiber axis at 520, 660, and 830 nm wavelengths. The experimental and numerically simulated results of far-field intensity distribution revealed high agreement. Hence, based on the numerical simulation, we proposed grism structure designs for in-line propagation of first-order diffraction at wavelengths of λ = 1300 - 2000 nm utilizing chalcogenide glass fibers.

Thermal and Electrochemical Properties of Ionic Liquids Bearing Allyl Group with Sulfonate-Based Anions-Application Potential in Epoxy Resin Curing Process.

Sulfonate-based ionic liquids (ILs) with allyl-containing cations have been previously obtained by us, however, the present study aims to investigate the thermal, electrochemical and curing properties of these ILs. To determine the temperature range in which ionic liquid maintains a liquid state, thermal properties must be examined using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). Melting, cold crystallization and glass transition temperatures are discussed, as well as decomposition temperatures for imidazolium- and pyridinium-based ionic liquids. The conductivity and electrochemical stability ranges were studied in order to investigate their potential applicability as electrolytes. Finally, the potential of triflate-based ILs as polymerization initiators for epoxy resins was proven.

Synthesis and Behavior of Hexamethylenetetramine-Based Ionic Liquids as an Active Ingredient in Latent Curing Formulations with Ethylene Glycol for DGEBA.

The paper presents the preparation of new ionic liquids based on hexamethylenetetramine with bis(trifluoromethanesulfonyl)imide and dicyanamide anion, which were characterized in detail in terms of their purity (Ion Chromatography) and thermal properties (Differential Scanning Calorimetry), as well as stability. The obtained substances were used to develop curing systems with ethylene glycol, which were successfully tested for their application with bisphenol A diglycidyl ether molecule. In addition, the curing process and its relationship to the structure of the ionic liquid are characterized in detail. The research showed that hexamethylenetetramine-based new ionic liquids can be successfully designed using well-known and simple synthetic methods-the Delepine reaction. Moreover, attention was paid to their stability, related limitations, and the application of hexamethylenetetramine-based ionic liquids in epoxy-curing systems.

Optical Fiber Grating-Prism Fabrication by Imprint Patterning of Ionic-Liquid-Based Resist.

We present a method of microstructure fabrication on the tip of the optical fiber using a UV soft-imprint process of polymerizable ionic liquid-based optical resist. Ionic liquid with two UV-sensitive vinylbenzyl groups in the structure was diluted in non-hazardous propylene glycol (PG) to obtain liquid material for imprinting. No additional organic solvent was required. The impact of propylene glycol amount and exposure dose on optical and mechanical properties was investigated. The final procedure of the UV imprint on the optical fiber tip was developed, including the mold preparation, setup building, UV exposure and post-laser cure. As the IL-containing vinylbenzyl groups can also be polymerized by the radical rearrangement of double bonds through thermal heating, the influence of the addition of 1-2% BHT polymerization inhibitor was verified. As a result, we present the fabricated diffraction gratings and the optical fiber spectrometer component-grism (grating-prism), which allows obtaining a dispersion spectrum at the output of an optical in line with the optical fiber long axis, as the main component in an optical fiber spectrometer. The process is very simple due to the fact that its optimization already starts in the process of molecule design, which is part of the trend of sustainable technologies. The final material can be designed by the tailoring of the anion and/or cation molecule, which in turn can lead to a more efficient fabrication procedure and additional functionalities of the final structure.

Halide-Free Continuous Synthesis of Hydrophobic Ionic Liquids.

Herein, we present a novel approach for the halide-free, continuous-flow preparation of hydrophobic ionic liquids (ILs) relying on the bis(trifluoromethanesulfonyl)imide (bistriflimide, NTf2 -) anion. The simple yet fast two-step synthetic route, which involves the formation of different alkyl bistriflimides (R4NTf2), followed by the quaternization with an amine nucleophile, led to the desired ILs in high yields and excellent purities without any byproduct formation. The variable alkyl chain (R4) length and the broad range of the applicable nucleophiles (R1R2R3N) offer considerable flexibility to the synthetic protocol. The quaternization can be performed under solvent-free conditions; moreover, the homogeneous nature of these reactions allows the application of modern continuous-flow technologies. Given these advantages, the methodology can afford not just a fast and efficient alternative for the conventional synthesis of such compounds with reduced waste water production but their negligible halide content might provide a significantly broader application range of the IL products, especially for the field of materials science.

Electron Beam Patterning of Polymerizable Ionic Liquid Films for Application in Photonics.

Planar photonic components can be fabricated with high resolution by electron beam patterning of polymer thin films on solid substrates such as silicon and glass. However, polymer films are normally formed by spin-coating lithographic resists containing not only polymers but also volatile solvents, which is a serious environmental and health issue. Therefore, we investigate a new type of material for planar structure fabrication (i.e., room-temperature ionic liquids (RTILs) with a polymerizable allyl group) that is electron-beam-curable, solvent-free, and thus potentially interesting for processing materials with weak resistance to solvents. We fabricate planar polymer microstructures by electron beam patterning of RTIL thin films in vacuum, which is possible because of the negligible volatility of ionic liquids. Three different polymerizable ionic liquids {i.e., [Allmim][Cl] (1-allyl-3-methylimidazolium chloride), [Allmim][NTf2] (1-allyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide), and [Allmmim][NTf2] (1-allyl-2,3-dimethylimidazolium bis(trifluoromethylsulfonyl)imide)} are compared in terms of the quality of the fabricated microstructures. We demonstrate that the shape of the more viscous RTIL with the Cl- anion is less distorted during electron-beam-activated polymerization than the shape of the less viscous RTILs with a large NTf2- anion. Furthermore, the surface tension of the NTf2-based ionic liquid decreases significantly with temperature as compared to that of the Cl-based ionic liquid. Thus, we suggest that the thermocapillary effect, that is, the Marangoni flow caused by a temperature gradient, might be responsible for the differences in the shape of the RTIL-derived microstructures. Also, we analyze the chemistry of the electron-beam-activated polymerization of RTIL by the use of Fourier-transform infrared spectroscopy (FTIR) and conclude that because of the disappearance of C═C bonds the free radical polymerization is a probable reaction mechanism. Finally, we show that polymerized microstructures are potentially attractive as planar photonic components because of good optical properties such as a high refractive index.

Versatile Method for the Simultaneous Synthesis of Two Ionic Liquids, Otherwise Difficult to Obtain, with High Atom Economy.

A new synthetic approach and full spectral (NMR, IR, MS) and ion chromatographic characterization (IC) of nitrogen-based ionic liquids bearing allyl- or ethyl- substituent and triflate, tosylate, methyl sulfate or methanesulfonate anion has been presented. On a sample of 16 new ionic liquids, the versatility of the anion exchange method has been proven. In the metathesis reactions that have been carried out, the halide anion was exchanged in ionic liquid with an alkyl sulfonate based anion using alkylating agents. The results obtained using ion chromatographic analysis on the newly synthesized compounds have been discussed. Also, the utilization of a gaseous methyl halide by-product, obtained in the metathesis reaction and otherwise difficult to synthesize, has been presented. This approach ensured high atom economy of the overall process, which makes the proposed methodology sustainable and eco-friendly.