Effects of Synthesis Parameters on Structure and Antimicrobial Properties of Bacterial Cellulose/Hydroxyapatite/TiO2 Polymer-Ceramic Composite Material.

Bacterial cellulose (BC) is a highly pure polysaccharide biopolymer that can be produced by various bacterial genera. Even though BC lacks functional properties, its porosity, three-dimensional network, and high specific surface area make it a suitable carrier for functional composite materials. In the present study, BC-producing bacteria were isolated from kombucha beverage and identified using a molecular method. Two sets of the BC hydrogels were produced in static conditions after four and seven days. Afterwards, two different synthesis pathways were applied for BC functionalization. The first method implied the incorporation of previously synthesized HAp/TiO2 nanocomposite using an immersion technique, while the second method included the functionalization of BC during the synthesis of HAp/TiO2 nanocomposite in the reaction mixture. The primary goal was to find the best method to obtain the functionalized material. Physicochemical and microstructural properties were analyzed by SEM, EDS, FTIR, and XRD methods. Further properties were examined by tensile test and thermogravimetric analysis, and antimicrobial activity was assessed by a total plate count assay. The results showed that HAp/TiO2 was successfully incorporated into the produced BC hydrogels using both methods. The applied methods of incorporation influenced the differences in morphology, phase distribution, mechanical and thermal properties, and antimicrobial activity against Staphylococcus aureus (ATCC 25923), Escherichia coli (ATCC 25922), Proteus mirabilis (ATCC 12453), and Candida albicans (ATCC 10231). Composite material can be recommended for further development and application in environments that are suitable for diseases spreading.

Dielectric and Structural Properties of the Hybrid Material Polyvinylidene Fluoride-Bacterial Nanocellulose-Based Composite.

In the search for environmentally friendly materials with a wide range of properties, polymer composites have emerged as a promising alternative due to their multifunctional properties. This study focuses on the synthesis of composite materials consisting of four components: bacterial nanocellulose (BNC) modified with magnetic Fe3O4, and a mixture of BaTiO3 (BT) and polyvinylidene fluoride (PVDF). The BT powder was mechanically activated prior to mixing with PVDF. The influence of BT mechanical activation and BNC with magnetic particles on the PVDF matrix was investigated. The obtained composite films' structural characteristics, morphology, and dielectric properties are presented. This research provides insights into the relationship between mechanical activation of the filler and structural and dielectric properties in the PVDF/BT/BNC/Fe3O4 system, creating the way for the development of materials with a wide range of diverse properties that support the concept of green technologies.

Design of PEI and Amine Modified Metakaolin-Brushite Hybrid Polymeric Composite Materials for CO2 Capturing.

In this paper, the properties of organic-inorganic hybrid polymer materials, which were synthesized from an aluminosilicate inorganic matrix with the addition of brushite and aminosilane grafted on one side and PEI covalently bonded composites on the other side, were examined. The synthesized organic-inorganic hybrid polymers were examined in terms of a structural, morphological, thermo-gravimetric, and adsorption-desorption analysis and also as potential CO2 capturers. The structural and phase properties as well as the percentage contents of the crystalline and amorphous phase were determined by the X-ray diffraction method. The higher content of the amorphous phase in the structure of hybrid polymers was proven in metakaolin and metakaolin-brushite hybrid samples with the addition of amino silane and with 1,000,000 PEI in a structure. The DRIFT method showed the main band changes with the addition of an organic phase and inorganic matrix. Microstructural studies with the EDS analysis showed a uniform distribution of organic and inorganic phases in the hybrid geopolymers. The thermo-gravimetric analysis showed that organic compounds are successfully bonded to inorganic polymer matrix, while adsorption-desorption analysis confirmed that the organic phase completely covered the surface of the inorganic matrix. The CO2 adsorption experiments showed that the amine-modified composites have the higher capture capacity, which is 0.685 mmol·g-1 for the GM10 sample and 0.581 mmol·g-1 for the BGM10 sample, with 1,000,000 PEI in the structure.

Processability evaluation of multiparticulate units prepared by selective laser sintering using the SeDeM Expert System approach.

3D printing in dosage forms fabrication is in the focus of researchers, however, the attempts in multiparticulate units (MPUs) preparation are scarce. The aim of this study was to fabricate different size MPUs by selective laser sintering (SLS), using different polymers, and investigate their processability based on the SeDeM Expert System approach. MPUs (1- or 2-mm size) were prepared with model drug (ibuprofen or caffeine), polymer (poly(ethylene)oxide (PEO), ethyl cellulose (EC) or methacrylic acid-ethyl acrylate copolymer (MA-EA)) and printing aid. Comprehensive sample characterization was performed and experimentally obtained parameters were mathematically transformed and evaluated using the SeDeM Expert System framework. The obtained samples exhibited irregular shape, despite the spherical printing object design. Polymer incorporated notably affected MPUs properties. The obtained samples exhibited low bulk density, good flowability-, as well as stability-related parameters, which indicated their suitability for filling into capsules or sachets. Low density values implied that compressibility enhancing excipients may be required for MPUs incorporation in tablets. Samples containing EC and MA-EA were found suitable for compression, due to high compacts tensile strength. The obtained results indicate that SeDeM Expert System may extended from powder compressibility evaluation tool to framework facilitating powders/multiparticulate units processing.

Heat Treatment of Geopolymer Samples Obtained by Varying Concentration of Sodium Hydroxide as Constituent of Alkali Activator.

In this paper, raw natural metakaolin (MK, Serbia) clay was used as a starting material for the synthesis of geopolymers for thermal treatment. Metakaolin was obtained by calcination of kaolin at 750 °C for 1 h while geopolymer samples were calcined at 900 °C, which is the key transition temperature. Metakaolin was activated by a solution of NaOH of various concentrations and sodium silicate. During the controlled heat treatment, the geopolymer samples began to melt slightly and coagulate locally. The high-temperature exposure of geopolymer samples (900 °C) caused a significant reduction in oxygen, and even more sodium, which led to the formation of a complex porous structure. As the concentration of NaOH (6 mol dm-3 and 8 mol dm-3) increased, new semi-crystalline phases of nepheline and sanidine were formed. Thermal properties were increasingly used to better understand and improve the properties of geopolymers at high temperatures. Temperature changes were monitored by simultaneous use of thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The loss of mass of the investigated samples at 900 °C was in the range of 8-16%. Thermal treatment of geopolymers at 900 °C did not have much effect on the change in compressive strength of investigated samples. The results of thermal treatment of geopolymers at 900 °C showed that this is approximately the temperature at which the structure of the geopolymer turns into a ceramic-like structure. All investigated properties of the geopolymers are closely connected to the precursors and the constituents of the geopolymers.

Hydroxyapatite/TiO2 Nanomaterial with Defined Microstructural and Good Antimicrobial Properties.

Due to the growing number of people infected with the new coronavirus globally, which weakens immunity, there has been an increase in bacterial infections. Hence, knowledge about simple and low-cost synthesis methods of materials with good structural and antimicrobial properties is of great importance. A material obtained through the combination of a nanoscale hydroxyapatite material (with good biocompatibility) and titanium dioxide (with good degradation properties of organic molecules) can absorb and decompose bacteria. In this investigation, three different synthesis routes used to prepare hydroxyapatite/titanium dioxide nanomaterials are examined. The morphology and semiquantitative chemical composition are characterized by scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX). The obtained materials' phase and structural characterization are determined using the X-ray powder diffraction method (XRD). The crystallite sizes of the obtained materials are in the range of 8 nm to 15 nm. Based on XRD peak positions, the hexagonal hydroxyapatite phases are formed in all samples along with TiO2 anatase and rutile phases. According to SEM and TEM analyses, the morphology of the prepared samples differs depending on the synthesis route. The EDX analysis confirmed the presence of Ti, Ca, P, and O in the obtained materials. The IR spectroscopy verified the vibration bands characteristic for HAp and titanium. The investigated materials show excellent antimicrobial and photocatalytic properties.

Potential Usage of Hybrid Polymers Binders Based on Fly Ash with the Addition of PVA with Satisfying Mechanical and Radiological Properties.

Since recycled technologies usage is mandatory for environmental safety, and in this regard, it is important to examine new materials that can be used in construction and are primarily produced from fly ash. In addition to characteristics such as hardness and compressive strength, the given materials must also be radiologically and environmentally safe. The main concept of engineered geopolymer gel composites based on fly ash residues is focused on developing binder materials via gel formation processes that can replace ordinary cement materials. This study is unique in researching the potential use of fly ash from the Nikola Tesla thermal power plant in Serbia, where the hybrid geopolymeric materials synthesized from fly ash are experimentally examined with the addition 1 wt% and 2 wt% of polyvinyl alcohol (PVA). This paper aims to investigate the structural, morphological, mechanical, and radiological properties of hybrid materials with the addition of PVA and without additive in the period of ageing for 28 days at room temperature. The phase composition was investigated using X-ray powder diffraction (XRPD) analysis, while morphological characteristics of these materials were examined using scanning electron microscopy and energy dispersive X-ray analysis (SEM-EDS). Vibrational spectra of obtained samples are investigated using diffuse reflectance infrared Fourier transform (DRIFT) and Fourier transform infrared (FTIR) techniques. The hardness and compressive strength are also examined, indicating that the 1 wt% addition in geopolymeric matrix results in the best mechanical properties. Radiological measurements of investigated all geopolymer samples show decreasing activity concentrations of radionuclides for 50% compared to fly ash.

Structural and Chemical Properties of Geopolymer Gels Incorporated with Neodymium and Samarium.

The present work was focused on doping of 1% and 5% both of Nd2O3 and Sm2O3 in geopolymer gels. One of the main goals was to determine the influence of the behavior of Nd and Sm as dopants and structural nanoparticles changes of the final geopolymer formed. It is shown that the disorder formed by alkali activation of metakaolin can accommodate the rare earth cations Nd3+ and Sm3+ into their aluminosilicate framework structure. The main geopolymerization product identified in gels is Al-rich (Na)-AS-H gel comprising Al and Si in tetrahedral coordination. Na+ ions were balancing the negative charge resulting from Al3+ in tetrahedral coordination. The changes in the structures of the final product (geopolymer/Nd2O3; Sm2O3), has been characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) analysis with energy dispersive spectrometry (EDS). Nucleation at the seed surfaces leads to the formation of phase-separated gels from rare earth phase early in the reaction process. It is confirmed that Nd and Sm have been shown to form unstable hydroxides Nd(OH)3 and Sm(OH)3 that are in equilibrium with the corresponding oxides.

Investigation into liquisolid system processability based on the SeDeM Expert System approach.

Liquisolid systems are emerging formulation approach for poorly soluble drugs, based on adsorption/absorption of drug dispersion and obtaining free-flowing powder with good compressibility. SeDeM Expert System represents a powder processability evaluation method. It may provide additional insight into liquisolid systems critical quality attributes, but the contribution of this approach remains to be explored. The aims of this study were: pellet preparation by combination of liquisolid technology and water granulation/extrusion, evaluation of liquisolid based systems (pellets/admixtures) and investigation into the applicability of SeDeM Expert System in liquisolid systems characterization. Pellets/admixtures were prepared with microcrystalline cellulose as carrier and crospovidone/silicon dioxide as coating agent. Ibuprofen solution in polyethylene glycol 400 was used as liquid phase. After comprehensive sample characterization, experimentally obtained parameters were mathematically transformed and evaluated in the SeDeM Expert System framework. Pellets exhibited low aspect ratio and excellent flowability, despite liquid load up to 52.2%. The investigated liquisolid admixtures exhibited good flowability and faster drug dissolution than pellets. Single pellet crushing test results exhibited strong correlation with compact indentation hardness and may be used as indentation hardness predictor. SeDeM Expert System provides useful insight into liquisolid system processability and comparative evaluation and it may facilitate final solid dosage form development.

Geopolymer/CeO2 as Solid Electrolyte For IT-SOFC.

As a material for application in the life sciences, a new composite material, geopolymer/CeO2 (GP_CeO2), was synthesized as a potential low-cost solid electrolyte for application in solid oxide fuel cells operating in intermediate temperature (IT-SOFC). The new materials were obtained from alkali-activated metakaolin (calcined clay) in the presence of CeO2 powders (x = 10%). Besides the commercial CeO2 powder, as a source of ceria, two differently synthesized CeO2 powders also were used: CeO2 synthesized by modified glycine nitrate procedure (MGNP) and self-propagating reaction at room temperature (SPRT). The structural, morphological, and electrical properties of pure and GP_CeO2-type samples were investigated by X-ray powder diffraction (XRPD), Fourier transform infrared (FTIR), BET, differential thermal and thermogravimetric analysis (DTA/TGA), scanning electron microscopy (FE-SEM), energy dispersive spectrometer (EDS), and method complex impedance (EIS). XRPD and matrix-assisted laser desorption and ionization time-of-flight (MALDI-TOF) analysis confirmed the formation of solid phase CeO2. The BET, DTA/TGA, FE-SEM, and EDS results indicated that particles of CeO2 were stabile interconnected and form a continuous conductive path, which was confirmed by the EIS method. The highest conductivity of 1.86 × 10-2 Ω-1 cm-1 was obtained for the sample GP_CeO2_MGNP at 700 °C. The corresponding value of activation energy for conductivity was 0.26 eV in the temperature range 500-700 °C.