Abstract
A systematic study is presented to explore the NH4CN polymerization induced by microwave (MW) radiation, keeping in mind the recent growing interest in these polymers in material science. Thus, a first approach through two series, varying the reaction times and the temperatures between 130 and 205 °C, was conducted. As a relevant outcome, using particular reaction conditions, polymer conversions similar to those obtained by means of conventional thermal methods were achieved, with the advantage of a very significant reduction of the reaction times. The structural properties of the end products were evaluated using compositional data, spectroscopic measurements, simultaneous thermal analysis (STA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). As a result, based on the principal component analysis (PCA) from the main experimental results collected, practically only the crystallographic features and the morphologies in the nanoscale were affected by the MW-driven polymerization conditions with respect to those obtained by classical syntheses. Therefore, MW radiation allows us to tune the morphology, size and shape of the particles from the bidimensional C=N networks which are characteristic of the NH4CN polymers by an easy, fast, low-cost and green-solvent production. These new insights make these macromolecular systems attractive for exploration in current soft-matter science.
Highlights
The development of new smart and multifunctional materials is currently encouraged to be constrained toward the design of low cost and free-solvent synthetic processes, or at least green-solvents, and easy, fast, effective and robust productions
For the first series of syntheses, the reaction times were chosen with a comparative proposal in a relationship with the NH4CN polymer obtained at 80 ◦C using conventional heating and a reaction time of 144 h [1]
We focused on this temperature based on the data reported in the first part of this work, as greater yields were obtained at this temperature; 130 ◦C and 205 ◦C were ruled out to explore the production of nanoparticles/nanofibers based on the principal component analysis (PCA) results, and due to the easier dispersion of the polymer synthetized at 170 ◦C in EtOH to prepare the samples for the scanning electron microscopy (SEM) measurements compared to those synthetized at higher temperatures, i.e., 190 ◦C and 205 ◦C
Summary
The development of new smart and multifunctional materials is currently encouraged to be constrained toward the design of low cost and free-solvent synthetic processes, or at least green-solvents, and easy, fast, effective and robust productions. It has been shown that the particle morphology of the known HCN-derived polymers can be tuned by the choice of the synthetic conditions [1,2,3] Some polymers of this heterogeneous family [4] have been proposed as emergent materials with different applications, such as photocatalysts [5], semiconductors, nanowires, ferroelectric materials [6], capacitors [1], coatings with potential biomedical applications [2,7,8,9], protective films against corrosion [10,11], or for the development of antimicrobial media for passive filtration [12]
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