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Bioactive glass is currently considered a material with a high biocompatibility and has been used both in the field of bone regeneration and in the preparation of cosmetic products with the controlled release of active compounds. The present work involved a study on the synthesis of bioglass using the sol–gel process. The study aims to evaluate the influence of the treatment of bioglass with Polyethylene glycol 4000 (PEG 4000) on its main characteristics. The surface characteristics of this material were obtained by nitrogen adsorption/desorption analysis, using the standard BET (Brunauer–Emmett–Teller) equation, the crystallinity by XRD (X-ray diffraction) analysis, the surface structure by SEM (Scanning Electron Microscope), thermal stability by TGA (ThermoGravimetric Analyses), and chemical bonds changes by FTIR (Fourier transform infrared) spectroscopy. After treatment with PEG 4000, the average diameter of the pores increased insignificantly, the crystallinity peak disappeared, and the SEM analysis highlighted several clusters of very small sizes. [ABSTRACT FROM AUTHOR]

Diatomite deposits in Poland are located in the Podkarpackie Voivodeship, and the only active deposit is in Jawornik Ruski. Therefore, it is a unique material. Improved rock processing methods are constantly in demand. In the research presented here, we have used research methods such as X-ray diffraction (XRD), scanning electron microscope (SEM), particle shape analysis, and appropriate sets of crushing machines. Diatomite comminution tests were carried out on test stands in different crushers (jaw crusher, hammer crusher, high-pressure roller press, ball mill) using different elementary crushing force actions: crushing, abrasion, and impact, occurring separately or in combination. The machines were tested with selected variable parameters to obtain products with a wide range of grain sizes ranging from 0 to 10 mm. The ball mill (yield 87%, system C3) and the hammer crusher with HPGR (high-pressure grinding roller) (yield 79%, system D2 + D3) have the greatest impact on diatom shell release and accumulation in the finest 0–5 μm and 5–10 μm fractions. For commercial purposes, it is important to obtain very fine fractions while keeping the shells undisturbed. [ABSTRACT FROM AUTHOR]

The perovskite-structured materials P b 0.75 B a 0.25 1 − x C a x (Z r 0.7 T i 0.3) O 3 for x = 1 and 2 at.% were synthesized using the conventional mixed-oxide method and carbonates. Microstructural analysis, performed using a scanning electron microscope, revealed rounded grains with relatively inhomogeneous sizes and distinct grain boundaries. X-ray diffraction confirmed that the materials exhibit a rhombohedral structure with an R3c space group at room temperature. Piezoelectric resonance measurements were conducted to determine the piezoelectric and elastic properties of the samples. The results indicated that a small amount of calcium doping significantly enhanced the piezoelectric coefficient d31. The calcium-doped ceramics exhibited higher electrical permittivity across the entire temperature range compared to the pure material, as well as a significant value of remanent polarization. These findings indicate that the performance parameters of the base material have been significantly improved, making these ceramics promising candidates for various applications. [ABSTRACT FROM AUTHOR]

Considering the high demand for innovative solutions in medicine, a major increase in interest in biomaterials research has been noticed, with the most significant advancements in metals and their alloys. Titanium-based alloys are one of the most recognised in the scientific community but do not represent the only way to achieve optimal results. Zirconium alloys for medical applications are a novelty with significant research potential based on their outstanding properties, which may be of value for medicine. The aim of the present study was to obtain new biomedical Zr-Nb-Mo alloys with varying ratios of their respective elements—Zr and Mo—using combined powder metallurgy (PM) and arc melting (VAM) methods. The obtained samples underwent microstructure analysis using an optical microscope (OM) and a scanning electron microscope (SEM). The study of element distribution was conducted with energy dispersive spectroscopy (EDS), whereas the phase composition was determined using X-ray diffraction (XRD). Mechanical properties were examined with a Micro Combi Tester MCT3, whereas tribological properties were assessed with a TRN Tribometer, and Ringer's solution was used as a lubricant. Additionally, the wear tracks of the studied samples were observed using the SEM. The research results indicated that increased Mo content conduced to microstructure refinement and homogeneity. Furthermore, the higher content of this element contributed to the growth of the HVIT, HIT, and EIT parameters, together with the improvement in the tribological performance of the alloys. XRD analysis revealed that the obtained samples were multiphase, and raising the Mo addition promoted the formation of new phases, including a ternary phase—Zr0.9Nb0.66Mo1.44 (Fd 3 ¯ m). The chemical composition study showed uneven distribution of niobium and areas of uneven mutual distribution of zirconium and molybdenum. [ABSTRACT FROM AUTHOR]

Residual melon by-products were explored for the first time as a bioresource of microcrystalline cellulose (MCC) obtention. Two alkaline extraction methods were employed, the traditional (4.5% NaOH, 2 h, 80 °C) and a thermo-alkaline in the autoclave (2% NaOH, 1 h, 100 °C), obtaining a yield of MCC ranging from 4.76 to 9.15% and 2.32 to 3.29%, respectively. The final MCCs were characterized for their chemical groups by Fourier-transform infrared spectroscopy (FTIR), crystallinity with X-ray diffraction, and morphology analyzed by scanning electron microscope (SEM). FTIR spectra showed that the traditional protocol allows for a more effective hemicellulose and lignin removal from the melon residues than the thermo-alkaline process. The degree of crystallinity of MCC ranged from 51.51 to 61.94% and 54.80 to 55.07% for the thermo-alkaline and traditional processes, respectively. The peaks detected in X-ray diffraction patterns indicated the presence of Type I cellulose. SEM analysis revealed microcrystals with rough surfaces and great porosity, which could remark their high-water absorption capacity and drug-carrier capacities. Thus, these findings could respond to the need to valorize industrial melon by-products as raw materials for MCC obtention with potential applications as biodegradable materials. [ABSTRACT FROM AUTHOR]

This study aimed to uncover the chronology and production technologies of ancient bricks unearthed from various locations in Upper Assam, Northeast India. To achieve this goal, complementary spectroscopic techniques such as Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), Scanning Electron Microscope (SEM) coupled with Energy Dispersive Spectrometer (EDS), as well as Thermoluminescence (TL) and Optically Stimulated Luminescence (OSL/IRSL) dating, were applied. FTIR and XRD analyses revealed the presence of quartz, feldspar (microcline, orthoclase, albite), kaolinite, chlorite, cerussite, palygorskite, magnetite, hematite, and organic carbon. The mineralogical composition indicates two distinct groups with firing temperatures below 650 °C and above ~800 °C. These two groups could be the first indication of the presence of two civilizations or at least two different production technologies involving different firing temperatures and kiln atmospheric conditions. Further, the SEM-EDS study suggests that both calcareous and non-calcareous clays were used in brick making, which have low and high refractory properties, respectively. The internal morphology of the samples shows the existence of micropores and microfractures, indicating the influence of higher-temperature firing. Absolute dating techniques associate the two brick groups with different age ranges: a firing temperature above ~800 °C indicates a superior technology corresponding to a production period between the 7th and 10th centuries CE. In contrast, a temperature below 650 °C indicates a technologically less advanced group of people, with the age group dated between the 11th and 14th centuries CE. [ABSTRACT FROM AUTHOR]

The existence of lead-zinc tailings threatens the social and ecological environment. The recycling of lead–zinc tailings is important for the all-round green transformation of economic society. In this study, the possibility of fabricating sintered ordinary bricks with lead–zinc tailings was studied based on orthogonal experimentation, and the phase composition and micromorphology of sintered products were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM). With lead–zinc tailings as the main material, and clay and fly ash as additives, the effect of clay content, forming pressure, sintering temperature, and holding time on physical properties of sintered bricks was analyzed. The results show that clay content and sintering temperature have a major effect on compressive strength, while sintering temperature and holding time play an important role in water absorption. During sintering, mica, chlorite, and other components in lead–zinc tailings are decomposed to form albite, hematite, maghemite, and anhydrite, which play a role in the strength of bricks. The optimal process parameters were found to be a ratio of lead–zinc tailings:clay:fly ash = 6:3:1, forming pressure of 20 MPa, firing temperature of 1080 °C, and holding time of 60 min. The corresponding compressive strength and water absorption were 34.94 MPa and 16.02%, which meets the Chinese sintered ordinary bricks standard (GB/T 5101-2017). [ABSTRACT FROM AUTHOR]

To explore and deal with the difficulty in curing cement-stabilized bases in desert environments, curing agents were prepared to enhance the curing effect on the base in this research. The composite curing agent was prepared through orthogonal experiments and the durability of the curing agent coating were studied by simulating a desert environment. Subsequently, the curing effect on the performance of bases was analyzed. Finally, the hydration degree of cement was studied via scanning electron microscope (SEM), thermogravimetric analysis (TG), and X-ray diffraction analysis (XRD), and the curing mechanism of the curing agent was explored. The results show that the composite (paraffin emulsion is the main component of the film, vinyl acetate-ethylene copolymer dosage is 20%, ethanol ester-12 dosage is 10%, and sodium silicate dosage is 18%) could effectively improve the water-retention performance (water-loss ratio: 2.36%) and mechanical properties of the specimen (7 d compressive strength: 7.48 MPa; 7 d indirect tensile strength: 0.70 MPa). The dry shrinkage coefficient of the specimen with composite curing agent was reduced by 116.26% at 28 days. The compressive strength of dry and wet freeze could reach 7.48 MPa and 6.88 MPa, respectively. The durability of the curing agent-coated base met the requirements of pavement performance in desert areas. The results of XRD, TG, and SEM indicated that the curing agent promoted hydration. In addition, the number of C-S-H gel and AFt crystals significantly increased. The curing difficulty of road bases in desert areas could be reduced effectively through the application presented in this study, which contributes to the conservation of natural and human resources. [ABSTRACT FROM AUTHOR]

Shale is composed of a rock matrix and bedding planes with a layered structure, resulting in significant anisotropy in its mechanical properties. In order to study the anisotropic mechanical properties of shale, the shale samples were prepared in different orientations with respect to the bedding planes, and the composition and microstructure of shale were first analyzed by X-ray diffractometer (XRD) and scanning electron microscope (SEM), and then the uniaxial and triaxial compression experiment on shale samples with five different bedding angles (the angle between the loading direction and the normal direction of the bedding planes, 0°, 30°, 45°, 60°, and 90°) were conducted under five confining pressures (0, 10, 20, 30, and 40 MPa), respectively; meanwhile, the acoustic emission (AE) test was carried out in the uniaxial test. The results indicate that the mechanical properties and parameters of shale have obvious anisotropy, and the AE characteristics of shale samples with different bedding angles are significantly different during uniaxial loading. Furthermore, the compressive strength and elastic modulus of the shale samples first decrease and then increase with the increase in the bedding angle under different confining pressures. Moreover, according to the anisotropic grade of compressive strength, the shale has moderate anisotropy. In addition, the failure mode of the shale samples is also anisotropic, and varies with the bedding angle and confining pressure. [ABSTRACT FROM AUTHOR]

Manganese slag (MS) containing a certain amount of active hydration substances may be used as a kind of cementitious material. In the present study, we measured the mass, the relative dynamic modulus of elasticity (RDME), and the flexural and compressive strengths of MS high-performance concrete (MS-HPC) with added basalt fibers exposed to NaCl freeze–thaw cycles (N-FCs), NaCl dry–wet alternations (N-DAs), and Na2SO4 dry–wet alternations (NS-DAs). Scanning electron microscope energy-dispersive spectrometer (SEM-EDS) spectra, thermogravimetric analysis (TG) curves, and X-ray diffraction spectroscopy (XRD) curves were obtained. The mass ratio of MS ranged from 0% to 40%. The volume ratio of basalt fibers varied from 0% to 2%. We found that, as a result of salt action, the mass loss rate (MLR) exhibited linear functions which were inversely correlated with the mass ratio of MS and the volume ratio of basalt fibers. After salt action, MLR increased by rates of 0~56.3%, but this increase was attenuated by the addition of MS and basalt fibers. Corresponding increases in RDME exhibited a linear function which was positively correlated with MS mass ratios in a range of 0~55.1%. The addition of MS and basalt fibers also led to decreased attenuation of mechanical strength, while the addition of MS led to increased levels of flocculent hydration products and the elements Mn, Mg, and Fe. CaClOH and CaSO4 crystals were observed in XRD curves after N-DA and NS-DA actions, respectively. Finally, the addition of MS resulted in increased variation in TG values. However, the opposite result was obtained when dry–wet actions were exerted. [ABSTRACT FROM AUTHOR]

In the Al-Fe binary system, the Al13Fe3 phase as well as the Al13Fe4 phase has similar icosahedral building blocks like those appearing in quasicrystals. Therefore, it is of vital importance to clarify the formation process of these two phases. Coexistence of the Al13Fe3 and Al13Fe4 phases was discovered from the educts obtained with a nominal atomic ratio of Al/Fe of 9:2 by high-pressure sintering for the first time. Firstly, single crystal X-ray diffraction (SXRD) combined with a scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX) measurement capabilities were adopted to determine the detailed crystal structures of both phases, which were sharply refined with regard to Al13Fe3 and Al13Fe4. Secondly, the orientation relationship between Al13Fe3 and Al13Fe4 was directly deduced from the SXRD datasets and the coexistence structure model was consequently constructed. Finally, seven pairs of parallel atomic planes and their unique orientation relations were determined from the reconstructed reciprocal space precession images. In addition, the real space structure model of the intergrowth crystal along with one kind of interfacial atomic structure were constructed from the determined orientation relations between two phases. [ABSTRACT FROM AUTHOR]

Although the Al2Fe phase has similar decagonal-like atomic arrangements as that of the orthorhombic Al5Fe2 phase, no evidence for intergrowth samples of Al2Fe and Al5Fe2 has been reported. In the present work, the co-existence of Al2Fe and Al5Fe2 phases has been discovered from the educts obtained with a nominal atomic ratio of Al:Fe of 2:1 by arc melting. First, single-crystal X-ray diffraction (SXRD) as well as scanning electron microscope (SEM) equipped with energy-dispersive X-ray spectroscopy (EDX) measurements have been utilized to determine the exact crystal structures of both phases, which are refined to be Al12.48Fe6.52 and Al5.72Fe2, respectively. Second, the orientation relationship between Al2Fe and Al5Fe2 has been directly deduced from the SXRD data sets, and the co-existence structure model has been constructed. Finally, four pairs of parallel atomic planes and their unique orientation relations have been determined from the reconstructed reciprocal-space precession images of (0kl), (h0l), and (hk0) layers. In addition, one kind of interface atomic structure model is constructed by the orientation relations between two phases, correspondingly. [ABSTRACT FROM AUTHOR]

In the present work, we studied the impact of excess Na addition on the structure of the standard NASICON ion conductor along with Na ion transport mechanisms. In this sense, NASICON ceramic membranes (NZSP) were prepared by a simple chemical synthesis method, the solid state reaction (SSR), using an excess of 5% Na (Na3.15Zr2Si2PO12) and an excess of 10% Na (Na3.3Zr2Si2PO12), in order to improve the conduction properties of the ceramic membrane. The characterization of the NZSP nanoparticles was performed by measuring the particle size by dynamic light scattering (DLS), the morphology of the NASICON samples pre-sintered at 1100 °C was analyzed by the SEM method (scanning electron microscope), and X-ray diffraction (XRD) analysis was used to investigate the crystal structure of samples, while the surface area was measured using the BET technique. The electrical properties (i.e., ionic conductivity) were evaluated by impedance spectroscopic methods at room temperature (RT). Following the experiments for NASICON membranes without Na excess, with 5% Na excess, and with 10% Na excess synthesized at different pressing forces and sintering temperatures, it was found that membranes with a 10% Na excess, sintered at 1175 °C for 10 h, presented a good ionic conductivity (4.72 × 10−4 S/cm). [ABSTRACT FROM AUTHOR]

Despite numerous studies focused on the hydrothermal (HT) synthesis of fly ash zeolites (FAZs), this method still has many limitations, the main of which is the low yield of zeolites. Hydrothermally synthesized zeolites are typically multiphase and exhibit low purity, which limits their applicability. Pure-phase zeolites have been primarily prepared from filtrates after alkaline mineralization of fly ashes, not directly in suspension. In addition, the published methodologies have not been tested in a wider set of samples, and thus their reproducibility is not confirmed. The aim of the study is to propose a reproducible methodology that overcomes the mentioned limitations. The influence of the Si/Al ratio (1.3:1–1:2), the type and concentration of the activator (2/4 M NaOH/KOH/LiOH), the reagent (30% LiCl), the duration (24–168 h), and the temperature (50–180 °C) of the synthesis phases were studied. The sequence of the synthesis phases was also optimized, depending on the type of heat transfer. The fly ashes were analyzed by wavelength-dispersive X-ray fluorescence (WD XRF), flame atomic absorption spectrometry (F-AAS), and X-ray diffraction (XRD). The energy intensity of the synthesis was reduced through the application of unique microwave digestion technology. Both microwave and combined (microwave and convection) syntheses were conducted. FAZs were identified and quantified by XRD analysis. This study presents a three-stage (TS) hydrothermal synthesis of pure-phase sodalite in suspension. Sodalite (>99 wt.%) was prepared from nine fly ashes under the following conditions: I. microwave phase: 120 °C, 150 min, solid-to-liquid ratio (S/L) 1:5, Si/Al ratio 1:1.5, and 4 M NaOH; II. convection phase: 120 °C, 24 h, S/L 1:40, and the addition of 30 mL of 30% LiCl; and III. crystallization: 70 °C for 24 h. The formation of rhombododecahedral sodalite crystals was confirmed by scanning electron microscope (SEM) images. [ABSTRACT FROM AUTHOR]