Search Results (11)

Mesoporous hydroxyapatite (HA) is widely used in various applications, such as the biomedical field, as a catalytic, as a sensor, and many others. The aim of this work was to obtain HA powders by means of chemical precipitation in a medium containing a polymer—polyvinyl alcohol or polyvinylpyrrolidone (PVP)—with concentrations ranging from 0 to 10%. The HA powders were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, atomic emission spectroscopy with inductively coupled plasma, electron paramagnetic resonance, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The specific surface area (SSA), pore volume, and pore size distributions were determined by low-temperature nitrogen adsorption measurements, and the zeta potential was established. The formation of macropores in powder agglomerates was determined using SEM and TEM. The synthesis in 10% PVP increased the SSA from 101.3 to 158.0 m²/g, while the ripening for 7 days led to an increase from 112.3 to 195.8 m²/g, with the total pore volume rising from 0.37 to 0.71 cm³/g. These materials could be classified as meso-macroporous HA. Such materials can serve as the basis for various applications requiring improved textural properties and may lay the foundation for the creation of bulk 3D materials using a technique that allows for the preservation of their unique pore structure. Full article

This research introduces a method to enhance the biocompatibility of bioinert Al₂O₃-based ceramics by incorporating calcium phosphates (hydroxyapatite (HAp) and tricalcium phosphate (TCP)) into alumina via spark plasma sintering-reactive sintering (SPS-RS). TGA/DTG/DTA and XRD revealed phase formation of HAp and TCP and determined the main temperature points of solid-phase reactions occurring in situ during the sintering of the CaO-CaHPO₄ mixture within the volume of Al₂O₃ under SPS-RS conditions in the range of 900–1200 °C. SEM, EDX, low temperature, and nitrogen physisorption were used to monitor changes in the morphology, structure, and elemental composition of bioceramics. Structural meso- and macroporosity, with a mean mesopore size of 10 nm, were revealed in the ceramic volume, while sintering temperature was shown to play a destructive role towards the porous inorganic framework. The physico-chemical characterization demonstrated increased relative density (up to 95.1%), compressive strength (640 MPa and above), and Vickers microhardness (up to 700 HV) depending on the HAp and TCP content and sintering temperature. Four bioceramic samples with different contents of HAP (20 and 50 wt.%) were bio-tested in in vivo models. The samples were implanted into the soft tissues under the superficial fascia of the thorax of a laboratory animal (a New Zealand White rabbit, female) in the area of the trapezius muscle and the broadest muscle of the back. Based on the results of the assessment of the surrounding tissue reaction, the absence of specific inflammation, necrosis, and tumor formation in the tissues during the implantation period of 90 days was proven. Microbial tests and dynamics of Pseudomonas aeruginosa bacterial film formation on bioceramic surfaces were studied with respect to HAp content (20 and 50 wt.%) and holding time (18, 24, and 48 h) in the feed medium. Full article

The present study proposes a new process for synthesis of alkali-activated materials (AAM)-supported analcime-C foam materials (AFs), utilizing a by-product of the lithium carbonate industry. This material has great application value as a bulk-type solid adsorbent. Characterization analyses show that the alkaline activator modulus greatly affects the crystallinity of analcime-C in AFs. Furthermore, the compressive strength, zeolite yield, and microstructure of AFs are significantly affected by the saturated steam parameters, including crystallization pressure, temperature, and time. The synthesized materials comprise pores of different sizes (micro to macro). They combine the functional micro-porosity of the analcime-C, the meso-porosity of the gel matrix, and the macro-porosity of the foamed AAM. The maximum compressive strength, density, total porosity, and Pb²⁺ adsorption capacity of AFs investigated in this study are 1.15 MPa, 350 kg/m³, 76.5%, and 69.3 mg/g Pb²⁺, respectively. Unlike many granular adsorbents, the bulk AFs adsorbent produced by this process is easy to recycle. In addition, it also contributes to the comprehensive utilization of a by-product of the lithium carbonate industry. Full article

A simple and inexpensive method for the preparation of porous SiC microspheres is presented. Polysiloxane microspheres derived from polyhydromethylsiloxane (PHMS) cross-linked with divinylbenzene (DVB) were ceramized under conditions leading to the removal of oxygen from the material. The content of free carbon (C_f) in highly crystalline silicon carbide (SiC) particles can be controlled by using various proportions of DVB in the synthesis of the pre-ceramic material. The chemical structure of the ceramic microspheres was studied by elemental analysis for carbon and oxygen, ²⁹Si MAS NMR, ¹³C MAS NMR, SEM/EDS, XRD and Raman spectroscopies, and their morphology by SEM, nitrogen adsorption and mercury intrusion porosimetries. The gaseous products of the thermal reduction processes formed during ceramization created a porous structure of the microspheres. In the SiC/C_f microspheres, meso/micro pores were formed, while in carbon-free SiC, microspheres macroporosity dominated. Full article

Silica aerogels are known to be materials with exceptional characteristics, such as ultra-low density, high surface area, high porosity, high adsorption, and low-thermal conductivity. In addition, these unique properties are mainly related to their specific processing. Depending on the aerogel synthesis procedure, the aerogels texture can be tailored with meso and/or macroporosity. Fractal geometry has been observed and used to describe silica aerogels at nanoscales in certain conditions. In this review paper, we describe the fractal structure of silica aerogels that can develop depending on the synthesis conditions. X-ray and neutron scattering measurements allow to show that silica aerogels can exhibit a fractal structure over one or even more than two orders of magnitude in length. The fractal dimension does not depend directly on the material density but can vary with the synthesis conditions. It ranges typically between 1.6 and 2.4. The effect of the introduction of silica particles or of further thermal treatment or compression of the silica aerogels on their microstructure and their fractal characteristics is also resumed. Full article

In the search of a new biomaterial for the treatment of bone defects resulting from traumatic events, an osteoporosis scenario with bone fractures, tumor removal, congenital pathologies or implant revisions for infection, we developed 3D scaffolds based on mesoporous bioactive glasses (MBGs) (85 − x)SiO₂–5P₂O₅–10CaO–xSrO (x = 0, 2.5 and 5 mol.%). The scaffolds with meso-macroporosity were fabricated by pouring a suspension of MBG powders in polyvinyl alcohol (PVA) into a negative template of polylactic acid (PLA), followed by removal of the template by extraction at low temperature. SrO-containing MBGs exhibited excellent properties for bone substitution including ordered mesoporous structure, high textural properties, quick in vitro bioactive response in simulated body fluid (SBF) and the ability of releasing concentrations of strontium ions able to stimulate expression of early markers of osteoblastic differentiation. Moreover, the direct contact of MC3T3-E1 pre-osteoblastic cells with the scaffolds confirmed the cytocompatibility of the three compositions investigated. Nevertheless, the scaffold containing 2.5% of SrO induced the best cellular proliferation showing the potential of this scaffold as a candidate to be further investigated in vitro and in vivo, aiming to be clinically used for bone regeneration applications in non-load bearing sites. Full article

In this report, we explore the use of supercritical CO₂ (scCO₂) in the synthesis of well-known metal-organic frameworks (MOFs) including Zn-MOF-74 and UiO-66, as well as on the preparation of [Cu₂₄(OH-mBDC)₂₄]_n metal-organic polyhedra (MOPs) and two new MOF structures {[Zn₂(L¹)(DPE)]∙4H₂O}_n and {[Zn₃(L¹)₃(4,4′-azopy)]∙7.5H₂O}_n, where BTC = benzene-1,3,5-tricarboxylate, BDC = benzene-1,4-dicarboxylate, L¹ = 4-carboxy-phenylene-methyleneamino-4-benzoate, DPE = 1,2-di(4-pyridyl)ethylene, 4.4′-azopy = 4,4′- azopyridine, and compare the results versus traditional solvothermal preparations at low temperatures (i.e., 40 °C). The objective of the work was to see if the same or different products would result from the scCO₂ route versus the solvothermal method. We were interested to see which method produced the highest yield, the cleanest product and what types of morphology resulted. While there was no evidence of additional meso- or macroporosity in these MOFs/MOPs nor any significant improvements in product yields through the addition of scCO₂ to these systems, it was shown that the use of scCO₂ can have an effect on crystallinity, crystal size and morphology. Full article

Li-O₂ batteries can offer large discharge capacities, but this depends on the morphology of the discharged Li₂O₂, which in turn is strongly affected by the nanostructured carbon used as support in the air cathode. However, the relation with the textural parameters is complex. To investigate the combined effect of channels of different sizes, meso-macroporous carbons with similar mesopore volume but different pore size distribution were prepared from the polymerization of resorcinol-formaldehyde (RF) in the presence of surfactants and micro-CaCO₃ particles. The carbon materials were used as active materials of air cathodes flooded by ionic liquid-based electrolytes in Li-O₂ cells with two different configurations, one with a static electrolyte and the other with a stirred electrolyte, which favor a film-like and large particle deposition, respectively. The presence of large pores enhances the discharge capacity with both mechanisms. Conversely, with respect to the reversible capacity, the trend depends on the cell configuration, with macroporosity favoring better performance with static, but poorer with stirred electrolytes. However, all mesoporous carbons demonstrated larger reversible capacity than a purely macroporous electrode made of carbon black. These results indicate that in addition to pore volume, a proper arrangement of large and small pores is important for discharge capacity, while an extended interface can enhance reversibility in Li–O₂ battery cathodes. Full article

Aerogels from natural polymers are endowed with attractive textural and biological properties for biomedical applications due to their high open mesoporosity, low density, and reduced toxicity. Nevertheless, the lack of macroporosity in the aerogel structure and of a sterilization method suitable for these materials restrict their use for regenerative medicine purposes and prompt the research on getting ready-to-implant dual (macro + meso)porous aerogels. In this work, zein, a family of proteins present in materials for tissue engineering, was evaluated as a sacrificial porogen to obtain macroporous starch aerogels. This approach was particularly advantageous since it could be integrated in the conventional aerogel processing method without extra leaching steps. Physicochemical, morphological, and mechanical characterization were performed to study the effect of porogen zein at various proportions (0:1, 1:2, and 1:1 zein:starch weight ratio) on the properties of the obtained starch-based aerogels. From a forward-looking perspective for its clinical application, a supercritical CO₂ sterilization treatment was implemented for these aerogels. The sterilization efficacy and the influence of the treatment on the aerogel final properties were evaluated mainly in terms of absence of microbial growth, cytocompatibility, as well as physicochemical, structural, and mechanical modifications. Full article

Zeolites are promising catalysts that are widely used in petrochemical, oil, and gas industries due to their unique characteristics, such as ordered microporous networks, good hydrothermal stability, large surface area, tunable acidity, and shape-selectivity. Nevertheless, the sole presence of microporous channels in zeolites inevitably restricts the diffusion of bulky reactants and products into and out of the microporous networks, leading to retarded reaction rates or catalyst deactivation. This problem can be overcome by developing hierarchical zeolites which involve mesoporous and macroporous networks. The meso- and macro-porosities can enhance the mass transport of molecules and simultaneously maintain the intrinsic shape selectivity of zeolite microporosity. Hierarchical zeolites are mainly developed through post-synthesis and pre-synthesis or in situ modification of zeolites. In this review, we evaluated both pre-synthesis and post-synthesis modification strategies with more focus on post-synthesis modification strategies. The role of various synthesis strategies on the intrinsic properties of hierarchical zeolites is discussed. The catalytic performance of hierarchical zeolites in important biomass reactions, such as catalytic pyrolysis of biomass feedstock and upgradation of bio-oil, has been summarized. The utilization of hierarchical zeolites tends to give a higher aromatic yield than conventional zeolites with microporosity solely. Full article

The functionalization of multi-walled carbon nanotubes (MW-CNTs) was obtained by generating reactive perfluoropolyether (PFPE) radicals that can covalently bond to MW-CNTs’ surface. Branched and linear PFPE peroxides with equivalent molecular weights of 1275 and 1200 amu, respectively, have been thermally decomposed for the production of PFPE radicals. The functionalization with PFPE chains has changed the wettability of MW-CNTs, which switched their behavior from hydrophilic to super-hydrophobic. The low surface energy properties of PFPEs have been transferred to MW-CNTs surface and branched units with trifluoromethyl groups, CF₃, have conferred higher hydrophobicity than linear units. Porosimetry discriminated the effects of PFPE functionalization on meso-porosity and macro-porosity. It has been observed that reactive sites located in MW-CNTs mesopores have been intensively functionalized by branched PFPE peroxide due to its low average molecular weight. Conductivity measurements at different applied pressures have showed that the covalent linkage of PFPE chains, branched as well as linear, weakly modified the electrical conductivity of MW-CNTs. The decomposed portions of PFPE residues, the PFPE chains bonded on carbon nanotubes, and the PFPE fluids obtained by homo-coupling side-reactions were evaluated by mass balances. PFPE-modified MW-CNTs have been characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), static contact angle (SCA), surface area, and porosity measurements. Full article