Τhis work describes the synthesis of PLA-grafted M-alginate (g-M-alginate; M: Ca²⁺, Co²⁺, Ni²⁺, Cu²⁺) aerogels. DL-lactide (LA) was attached on the surface of preformed M-alginate beads and was polymerized, using stannous octoate as catalyst and the –OH groups of the alginate backbone as initiators/points of attachment. The material properties of g-M-alginate aerogels were not affected much by grafting, because the linear PLA chains grew on the M-alginate framework like a brush and did not bridge their points of attachment as in polyurea-crosslinked M-alginate aerogels. Thus, all g-M-alginate aerogels retained the fibrous morphology of their parent M-alginate aerogels, and they were lightweight (bulk densities up to 0.24 g cm⁻³), macroporous/mesoporous materials with high porosities (up to 96% v/v). The BET surface areas were in the range of 154–542 m² g⁻¹, depending on the metal, the nature of the alginate framework and the PLA content. The latter was found at about 15% w/w for Ca- and Ni-based materials and at about 29% w/w for Co- and Cu-based materials. Overall, we have demonstrated a new methodology for the functionalization of alginate aerogels that opens the way to the synthesis of polylactide-crosslinked alginate aerogels with the use of multifunctional monomers. Full article

The fabrication of bioactive three-dimensional (3D) hydrogel scaffolds from biocompatible materials with a complex inner structure (mesoporous and macroporous) and highly interconnected porosity is crucial for bone tissue engineering (BTE). 3D-printing technology combined with aerogel processing allows the fabrication of functional nanostructured scaffolds from polysaccharides for BTE with personalized geometry, porosity and composition. However, these aerogels are usually fragile, with fast biodegradation rates in biological aqueous fluids, and they lack the sterility required for clinical practice. In this work, reinforced alginate-hydroxyapatite (HA) aerogel scaffolds for BTE applications were obtained by a dual strategy that combines extrusion-based 3D-printing and supercritical CO₂ gel drying with an extra crosslinking step. Gel ageing in CaCl₂ solutions and glutaraldehyde (GA) chemical crosslinking of aerogels were performed as intermediate and post-processing reinforcement strategies to achieve highly crosslinked aerogel scaffolds. Nitrogen adsorption–desorption (BET) and SEM analyses were performed to assess the textural parameters of the resulting alginate-HA aerogel scaffolds. The biological evaluation of the aerogel scaffolds was performed regarding cell viability, hemolytic activity and bioactivity for BTE. The impact of scCO₂-based post-sterilization treatment on scaffold properties was also assessed. The obtained aerogels were dual porous, bio- and hemocompatible, as well as endowed with high bioactivity that is dependent on the HA content. This work is a step forward towards the optimization of the physicochemical performance of advanced biomaterials and their sterilization. Full article

Medical implants are routinely tracked and monitored using different techniques, such as MRI, X-ray, and ultrasound. Due to the need for ionizing radiation, the two former methods pose a significant risk to tissue. Ultrasound imaging, however, is non-invasive and presents no known risk to human tissue. Aerogels are an emerging material with great potential in biomedical implants. While qualitative observation of ultrasound images by experts can already provide a lot of information about the implants and the surrounding structures, this paper describes the development and study of two simple B-Mode image analysis techniques based on attenuation measurements and echogenicity comparisons, which can further enhance the study of the biological tissues and implants, especially of different types of biocompatible aerogels. Full article

Organic aerogels in the form of powder, microgranules and microsized particles receive considerable attention due to their easy fabrication, low process time and costs compared to their monolithic form. Here, we developed resorcinol-formaldehyde (RF) aerogel microparticles by using an emulsion-gelation method. The main objective of this study is to investigate the influence of curing time, stirring rate, RF sol:oil ratio and initial pH of the sol in order to control the size and properties of the microparticles produced. The emulsion-gelation of RF sol prepared with sodium carbonate catalyst in an oil phase at 60 °C was explored. RF microparticles were washed with ethanol to remove the oil phase followed by supercritical and ambient pressure drying. The properties of the dried RF microparticles were analyzed using FT-IR, N₂ adsorption isotherm, gas pycnometry, wide angle X-ray scattering and scanning electron microscope. RF microparticles with high surface area up to 543 m²/g and large pore volume of 1.75 cm³/g with particle sizes ranging from 50–425 µm were obtained. Full article

The presented study shows the possibility of using bioaerogels, namely neat alginate, pectin, chitosan aerogels, and alginate and pectin aerogels coated with chitosan, as drug delivery systems for esomeprazole. Two different techniques were used for the impregnation of esomeprazole: Supercritical impregnation, and diffusion via ethanol during the sol-gel synthesis. The prepared samples were characterized by employing N₂ adsorption-desorption analysis, TGA/DSC, and FTIR. The achieved loadings were satisfactory for all the tested samples and showed to be dependent on the technique used for impregnation. In all cases, higher loadings were achieved when impregnation via diffusion from ethanol was used. Extensive release studies were performed for all impregnated samples. The in vitro dissolution profiles were found to be dependent on the carrier and impregnation method used. Most importantly, in all cases more controlled and delayed release was achieved with the bioaerogels compared to using pure esomeprazole. Full article

The imaging of non-conducting materials by scanning electron microscopy (SEM) is most often performed after depositing few nanometers thick conductive layers on the samples. It is shown in this work, that even a 5 nm thick sputtered gold layer can dramatically alter the morphology and the surface structure of many different types of aerogels. Silica, polyimide, polyamide, calcium-alginate and cellulose aerogels were imaged in their pristine forms and after gold sputtering utilizing low voltage scanning electron microscopy (LVSEM) in order to reduce charging effects. The morphological features seen in the SEM images of the pristine samples are in excellent agreement with the structural parameters of the aerogels measured by nitrogen adsorption-desorption porosimetry. In contrast, the morphologies of the sputter coated samples are significantly distorted and feature nanostructured gold. These findings point out that extra care should be taken in order to ensure that gold sputtering does not cause morphological artifacts. Otherwise, the application of low voltage scanning electron microscopy even yields high resolution images of pristine non-conducting aerogels. Full article

Polyurea is an isocyanate derivative, and comprises the basis for a well-established class of polymeric aerogels. Polyurea aerogels are prepared either via reaction of multifunctional isocyanates with multifunctional amines, via reaction of multifunctional isocyanates and water, or via reaction of multifunctional isocyanates and mineral acids. The first method is the established one for the synthesis of polyurea, the third is a relatively new method that yields polyurea doped with metal oxides in one step, while the reaction of isocyanates with water has become the most popular route to polyurea aerogels. The intense interest in polyurea aerogels can be attributed in part to the low cost of the starting materials—especially via the water method—in part to the extremely broad array of nanostructural morphologies that allow study of the nanostructure of gels as a function of synthetic conditions, and in part to the broad array of functional properties that can be achieved even within a single chemical composition by simply adjusting the synthetic parameters. In addition, polyurea aerogels based on aromatic isocyanates are typically carbonizable materials, making them highly competitive alternatives to phenolic aerogels as precursors of carbon aerogels. Several types of polyurea aerogels are already at different stages of commercialization. This article is a comprehensive review of all polyurea-based aerogels, including polyurea-crosslinked oxide and biopolymer aerogels, from a fundamental nanostructure–material properties perspective, as well as from an application perspective in thermal and acoustic insulation, oil adsorption, ballistic protection, and environmental cleanup. Full article