X-ray Diffraction Research Articles

Chitosan-grafted Cyclodextrin via Click Chemistry as an Encapsulating Agent to Enhance the Antibacterial Activity of Thymol

Introduction: This paper aimed to investigate, for the first time, the possibility of increasing the antibacterial activities of thymol (TH) by developing an encapsulating agent based on chitosan-grafted cyclodextrin. For this purpose, β-cyclodextrin was monosubstituted at position 6 via propargyl bromide, and chitosan’s amine groups were converted to azide functions. After alkylation and diazotization reactions, the grafting of β-cyclodextrin onto the chitosan (CSβCD) was realized via click chemistry alkyne–azide cycloaddition. Methods: The incorporation of TH into chitosan-grafted β-cyclodextrin (TH/CS-βCD) was performed by the freeze-drying method, and the encapsulation efficiency was investigated based on various mass ratios (TH:CS-βCD). The optimized inclusion complex was then thoroughly examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). Results: The antibacterial activity was assessed against Escherichia coli, Staphylococcus aureus, and Bacillus subtilis using broth-microdilution assay. Fourier transform infrared spectroscopy analysis demonstrated the successful grafting of β-cyclodextrin onto chitosan since the optimum mass ratio between TH and CS-βCD was 1:8 (w:w), corresponding to 78 ± 3.42% of encapsulation efficiency, while SEM, XRD, TGA and DSC confirmed the establishment of TH/CS-βCD inclusion complexes. Conclusion: The in vitro investigation showed that TH/CS-βCD exhibited higher antibacterial properties compared to TH in free form.

Two new Mn-LMOF based on an AIEgens ligand for selective detection of Al3+ and other ions in aqueous solution

Two novel multifunctional chemical sensor Mn-LMOF, namely, [Mn2(TPPE)(ndc)2(H2O)]n (LMOF-1) and [Mn2(TPPE)(oba)2]n (LMOF-2) were solvothermally synthesized by introducing an AIE luminogens (AIEgens) ligand, 1,1,2,2-tetra[4-(pyridin-4-yl)phenyl]ethylene(TPPE), and analyzed by single crystal X-ray diffraction, thermogravimetric and powder X-ray diffraction and other methods. LMOF-1 and LMOF-2 have high stability and strong luminescence properties in solutions. The sensing experiments testify that LMOF-1 can be used as a selectively sensor for Al3+, with the limit of detection is 1.83 × 10−5 M. And LMOF-1 and LMOF-2 can identify Fe3+, CrO42− and Cr2O72− ions in aqueous solution, and LMOF-1 has a higher Ksv for all three ions than LMOF-2.

Corrosion resistance and wear behavior of CoCrFeNiMn@Gr high entropy alloy-based composite coatings prepared by laser cladding

In this study, we utilize laser cladding to apply a CoCrFeNiMn HEA with 2 wt.% few-layer graphene (Gr) coating onto the surface of Q235B mild steel. Alcohol stirring method was used for HEA and Gr preparation of composite powder. Raman spectroscopy and energy dispersion spectroscope (EDS) indicate the successful mixing of HEA and Gr powders, with Gr adhering to the surface of the HEA powder in a lamellar structure. The X-ray diffraction (XRD), scanning electron microscope (SEM), EDS, and Electron backscatter diffraction (EBSD) analyses revealed that grain refinement and the formation of fine carbide-hard phases in the HEA/Gr coating improve microhardness and wear resistance. The average Schmidt factors of the coating decreased from 0.47 to 0.45 with the addition of Gr, indicating enhanced resistance to plastic deformation and anisotropy. Nanoindentation experiments demonstrated that the HEA/Gr coatings exhibit superior resistance to plastic deformation, effectively enhancing the coating’s durability against spalling under stress and wear conditions. The microhardness of the HEA/Gr coating increased by 99.25%, and the wear rate decreased by 86.31% compared to the HEA coating alone. The open circuit potential (OCP), linear polarization curve, Tafel curves, electrochemical impedance spectroscopy (EIS), and Mott-Schottky tests all indicated that the HEA/Gr coating possesses superior corrosion resistance. X-ray Photoelectron Spectroscopy (XPS) results suggest that the passivation film of the HEA/Gr coating, which contains more oxides and less hydroxide, is more protective and denser, thereby slowing the corrosion rate.

Radiation damage in He irradiated nanolayered Zr/Nb at different temperatures

Nanolayered Zr/Nb metals are considered promising for advanced nuclear reactors due to their superior resistance to irradiation. In this study, Zr/Nb multilayers were irradiated with 50 keV He+ ions to a fluence of 1 × 1017 ions/cm2 at temperatures of room temperature, 350 °C, and 500 °C to investigate irradiation-induced structural changes. X-ray diffraction (XRD) analysis indicated low-angle shifts of 0.08-0.54° and high-angle shifts of 0.08-0.42° in the irradiated Zr and Nb layers, suggesting tensile and compressive strains, respectively. At 500 °C, the selected-area electron diffraction (SAED) observed a 9.2% lattice expansion in Zr and a 0.13% contraction in Nb. Geometric phase analysis (GPA) revealed varying strain distributions, transitioning from incoherent to coherent interfaces with increasing irradiation damage. Transmission electron microscopy (TEM) identified the presence of He bubbles in the Zr layer as one of the reasons for strain differences. Nanoindentation tests showed an increase at a depth of 150 nm hardness of 0.831 GPa at 500 °C compared to 350 °C. These results are attributed to differences in crystal structure, vacancy dynamics, interfacial effects, and lattice strain influences. Stability of Zr/Nb interfaces after He irradiation was studied. This study provides insights into the radiation behavior of Zr/Nb nanoscale metallic materials, enhancing our understanding of their potential as structural materials in nuclear energy systems.

Cathodic corrosion induced selective nano-crystallization of Nickel oxo/hydroxo complex on (NiFeCr)SiB amorphous ribbon for alkaline oxygen evolution reaction and methanol oxidation reaction

The study focuses on the development and optimization of (Ni87Fe4Cr9)78Si8B14 amorphous ribbons as self-supported electro-catalysts for oxygen evolution reaction (OER) and methanol oxidation reaction (MOR). Electro-catalytically active nano α-Ni(OH)2 phase (5–10nm) was generated in the amorphous ribbon surface through potentiostatic cathodic corrosion for different time intervals (0–120 min). The X-ray diffraction and scanning electron microscopy results shows the favourable occurrence of dense nanocrystallization of α-Ni(OH)2 between 45 and 90 min of corrosion time. For OER in 1 M KOH, the 60-min surface modified ribbon exhibits an overpotential of 295 mV at 10 mA/cm2 current density and tafel slope of 51 mV dec−1. In case of MOR in 1 M KOH +1 M MeOH, the 90-min corroded ribbon shows lowest potential of 1.38 V vs RHE, at 10 mA/cm2 and tafel slope of 34 mV dec−1. In addition to superior electro-catalytic activity, the optimal surface-modified ribbons show superior long-term stability for OER and MOR studies, indicating its potential application in hydrogen generation and direct methanol fuel cell.

Synergistic effects of liquid phase sintering and B-site substitution to enhance proton conductivity of BaZr0.1Ce0.7Y0.1Yb0.1O3-δ for protonic ceramic fuel cell

This paper is dedicated to improving the sintering and conductivity of BaZr0.1Ce0.7Y0.1Yb0.1O3-δ (BZCYYb) by adding ZnO-CuO dual-sintering aids. The synergistic effects of liquid-sintering of Zn and B-site substitution of Cu on the sinterability and proton conductivity of BZCYYb are systematically investigated. X-ray diffraction (XRD) analysis of BZCYYb after addition of ZnO-CuO (BZCYYb-Zn-Cu) confirms the complete perovskite phase formation without any secondary phase. The substitution of Ce4+ (0.87 Å) with Zn2+ (0.74 Å) or Cu2+ (0.73 Å) induces a shift in XRD diffraction peak to higher angle due to a decrease in lattice constant. Energy dispersive X-ray spectroscopy analysis indicate a distinct distribution of Zn primarily at the grain boundaries, while Cu is predominantly located within the grains of BZCYYb-Zn-Cu. The addition of ZnO-CuO into BZCYYb results in a denser microstructure with larger average grain size. Furthermore, the substitution of Ce4+ by Cu2+ increases the concentration of oxygen vacancies and reduces activation energy. For BZCYYb-Zn-Cu, the proton conductivity reaches 4.52×10-2 S/cm at 750 °C, approximately 3 times higher than that of BZCYYb. This enhancement can be attributed to the synergistic effects of larger average grain size resulting from liquid phase sintering of Zn, low active energy, and high concentration of oxygen vacancies arising from Cu B-site substitution. BZCYYb-Zn-Cu is used as the electrolyte for anode support SOFC, and the single cell exhibits remarkable electrochemical performance and excellent stability in H2 fuel. This research establishes a crucial theoretical foundation for the preparation and performance evaluation for large-size protonic ceramic cell.

Physical-chemical performance of coal gasification slag with calcination activation utilized as supplementary cementitious material

The utilization of coal gasification slag to prepare supplementary cementitious materials has garnered considerable interest due to environmental friendliness. In this study, a calcination activation was carried out to enhance the pozzolanic activity of coal gasification slag, and serial sintering temperatures were conducted to activate coal gasification slag in this study. The coal gasification slags were characterized by particle size analyzer, X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). Furthermore, the pozzolanic activity of coal gasification slag was identified through dilution test and application in blended paste. Results showed that the calcination pretreatment effectively affected the particle size distribution and mineral composition. The setting time and hydration rate were prolonged by incorporating coal gasification slag. It was crucial that the coal gasification slag calcined under 400℃ performed the highest reactivity and its blend presented a 4.75% higher compressive strength than neat cement at 28 d curing. AFt and AFm were mainly generated by pozzolanic reaction, and a denser microstructure that porosity decreased by 26.76% was gained. The achievement of this study proved the feasibility of this treated coal gasification slag in building materials.

Multifunctional bacterium induced carbonate precipitation with low nitrogen effectively remediates cadmium polluted water

Microorganism Induced Carbonate Precipitation (MICP) has emerged as an efficacious approach to address the issue of cadmium (Cd) contamination in water bodies. However, the associated production of ammonium nitrogen (NH4+-N) poses a significant challenge to the MICP. To tackle this, our research has developed a novel bacterium (UN-1), with dual MICP and NH4+-N degradation capabilities. We have elucidated the biogeochemical pathways of Cd2+ precipitation and NH4+-N degradation, characterized the micromorphology, phase composition, and crystallization of the MICP products, and identified the key factors influencing the MICP reaction. Our findings indicate that The UN-1-mediated MICP effectively removes Cd2+ at concentrations below 20 mg/L, reducing NH4+-N levels to 50 mg/L within 120 h. The predominant strains in UN-1 are Sporosarcina (24.35 %), Bacillus (31.36 %), Tumebacillus (6.89 %), Nitrospira (11.09 %), and Alkaliphilus (8.16 %). The bacterium employs urea enzymes UreA, UreB, and UreC for urea hydrolysis, thereby facilitating carbonate production, while the degradation of NH4+-N is mediated by hydroxylamine oxidase (HAO), nitrite reductase (NIR), and nitrate reductase (NAR). The resultant MICP products after Cd2+ removal are irregular spherical minerals, 200–300 nm in diameter, exhibiting well-developed single-crystal structures and high crystallinity. Their X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) patterns align with the characteristics of cadmium carbonate (CdCO3) minerals. Optimal conditions for the UN-1-led MICP reaction are identified as a pH range of 5.0 to 9.0 and a temperature range of 20 to 40 °C, the dissolved oxygen (DO) concentration in the water does not significantly impact the MICP. Furthermore, the study demonstrates that NH4+-N concentrations can be maintained at low levels under most conditions. This research introduces an innovative solution to the NH4+-N by-product challenge during Cd removal via MICP, laying a solid theoretical foundation for the development of a rapid, efficient, and eco-friendly remediation technology for Cd-contaminated waters.

Bio-based composite film from konjac flour and dialdehyde starch: Development, properties and structural features

The development of environmental-friendly composite products from renewable resources has been considered as an excellent approach to address the negative impact of petroleum-based plastics on environment. Konjac flour (KF), as an excellent polysaccharide material, has a broad application in food field. It shows a promising future in the film field due to its excellent film-forming properties. In this work, KF was selected as primary film-forming matrix, and dialdehyde starch (DAS) as the reinforcing component. A series of KF/DAS composite films were prepared by adjusting the addition ratio of DAS component. Then, their physical and mechanical properties were characterized and analyzed. The results showed that KF/DAS composite film with 25 % DAS content exhibited the optimal mechanical properties, including tensile strength (TS) of 13.1 MPa and elongation at break (EAB) of 93.7 %, indicating that an excellent cross-linked system formed among KF and DAS utilizing the method described in this study. Furthermore, much evidences from the fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) confirmed that a strong chemical cross-linkages between DAS and KF via Schiff base and esterification reactions. Based on the thermogravimetry (TG) and scanning electron microscopy (SEM) results, KF/DAS composite films also had excellent thermal stability and a dense microstructure, although there are also changes with the DAS usage.

Plasma synthesis and characteristics of nanocomposite coatings based on PVA and chitosan with incorporated nanoparticles for the healing of skin wounds

This study investigated the impact of new composites based on PVA and chitosan on wound healing in mice. Metal or metal oxide nanoparticles were synthesized without reagents by creating an impulse discharge between metal electrodes in a polymer dispersion. Polymer composites and coatings were then prepared using these nanoparticles. The composites were analyzed using various techniques, including UV spectroscopy, X-ray diffraction, scanning and transmittance electron microscopy, and infrared spectroscopy. The maximum concentration of nanoparticles in the composite was 3.5%. The average diameter of the nanoparticles was approximately 50-60 nm. The inclusion of Ag and ZnO nanoparticles accelerated the healing process by approximately 25%.

Hydrogen resistance of reduced graphene oxide coatings prepared by electrophoretic deposition on duplex stainless steel

In this study, reduced graphene oxide (rGO) coatings were fabricated on duplex stainless steel (DSS) substrates using the electrophoretic deposition (EPD) method to evaluate their hydrogen resistance performance. The successful fabrication of rGO coatings was confirmed using Fourier Transform Infrared Spectroscopy (FT-IR) and X-ray Photoelectron Spectroscopy (XPS). The structural characteristics were characterized using Raman spectroscopy and X-ray Diffraction (XRD). The results indicate that the EPD voltage is a crucial factor affecting the surface quality of and hydrogen resistance performance of rGO. Lower voltages resulted in lower degrees of rGO reduction and higher surface wrinkle density, while higher voltages caused bubble formation, significantly degrading the coating quality and hydrogen resistance performance. The optimal hydrogen resistance was achieved at an EPD voltage of 7.5V and a deposition time of 6 minutes. Electrochemical hydrogen charging tests and thermal desorption analysis (TDA) demonstrated that rGO coatings prepared under optimal conditions exhibited excellent hydrogen resistance efficiency, significantly reducing hydrogen atom penetration in hydrogen environments. The study further revealed that bubble formation significantly reduces the hydrogen resistance of rGO, which is attributed to increased interlayer spacing and the loss of the “labyrinth effect”.

Chromatic tuning of upconversion emission upon dual infrared wavelength co-excitation in Er3+ doped Ba3Lu4O9 phosphor

Emission color change of the upconversion luminescence materials is often required for applications in optical anti-counterfeiting, laser lighting, and 3D displays. In this work, we developed a new route for chromatic tuning of upconversion emission upon two wavelength co-excitation by changing excitation power density. The proposed route was used for Er3+ single-doped Ba3Lu4O9 phosphor which was derived from a traditional solid-state reaction. The crystal structure of the obtained Ba3Lu4O9:Er3+ phosphor was characterized by X-ray diffraction and Rietveld refinement modeling. Under individual excitation of 980 or 1550 nm, it was found that the luminescence intensity ratio of red to green changes slightly with respectively increasing excitation power density (working current of the laser) of 980 or 1550 nm laser. However, upon both 980 and 1550 nm co-excitation at the same time and by adjusting the excitation power density of one laser amongst the two lasers, the luminescence intensity ratio of red to green changes greatly with increasing excitation power density. The change of luminescence intensity ratio of red to green implies the upconversion emission color tuning. The mechanism for the color tuning was discovered. It was found that with changing excitation power density the ratio of red to green changed greatly when the phosphor was irradiated by 980 and 1550 together, but the ratio of red to green changed slightly when the phosphor was irradiated individually by 980 or 1550. It is proved that it is feasible to turn color by the method of two infrared wavelengths excitation.

Enhancement of luminescence and thermal stability in Eu3+-doped K3Y(BO2)6 with Li+ and Na+ co-doping

Eu3+-doped and Li+/Na+ co-doped K3Y(BO2)6 (KYBO) phosphors were synthesized through a microwave-assisted sol–gel method, and their structural and photoluminescent (PL) characteristics were examined. X-ray diffraction (XRD) and Rietveld refinement confirm effective dopant incorporation and preservation of the crystalline structure. Fourier Transform Infrared (FTIR) spectroscopy indicates the maintenance of the borate structure, confirming the structural integrity of the phosphors upon doping. The addition of Li+ and Na+ co-dopants notably enhances luminescent efficiency and thermal stability, making these phosphors promising candidates for solid-state lighting (SSL) applications. PL analysis reveals strong red emission peaks at 612 nm, attributed to the 5Do → 7F2 transition of Eu3+ ions. The study indicates that electric dipole-quadrupole interactions are the primary mechanism for energy migration, with a critical distance of approximately 22.68 Å. This mechanism contributes to concentration quenching at higher doping levels. High temperature PL measurements indicated an activation energy of 0.1389 eV for thermal quenching in the Li+ co-doped sample. Additionally, the Na+ co-doped sample exhibited an abnormal thermal stability behavior, with an even higher activation energy of 0.2536 eV. This suggests that Na+ co-doping significantly enhances the thermal resilience of the phosphor, making it more suitable for high-power light-emitting applications that operate under extreme conditions. CIE chromaticity diagrams highlight the potential for optimizing Eu3+ doping levels, combined with Li+ and Na+ co-doping, to improve luminescent performance and thermal stability for advanced SSL applications.

Unveiling the untapped potential of Hibiscus Rosa-sinensis lignocellulosic fiber: A multifaceted characterization for advancing sustainable biocomposite applications

In the pursuit of sustainable advancements in bio-inspired fiber reinforced polymer composite materials, the exploration of novel natural fibers has become a focal point of research. This experimental study aims to elucidate the unexplored potential of Hibiscus Rosa-sinensis fiber (HRF) as a versatile reinforcement material for high-performance composites. Through an integrated approach, this research offers a meticulous analysis of the HRF's physico-chemical properties, and single fiber tensile strength. The crystalline structure are revealed by X-ray diffraction (XRD), thermal behavior are characterized through thermo-gravimetric analysis (TGA), and surface morphology has been visualized using field emission scanning electron microscopy (FESEM) studies. From the results, it is found that the HRF contains a cellulose content of 79.50 %, positioning it as a prime bast fiber among its counterparts. This composition is complemented by hemicellulose (10.36 %), lignin (4.62 %), wax (0.84 %), and ash (2.96 %). The Fourier-transform infrared spectroscopy (FTIR) spectra unveils the intricate functional groups present in the fibers. XRD analysis highlights a crystallinity index (CI) of 66.93 %, confirming a well-organized and structured crystalline arrangement. The thermal stability established through TGA underscores HRF's resilience up to 284 °C, presenting it is an optimal reinforcement material for bio-inspired green composites operating within 280 °C. The surface morphology of HRF is examined through FESEM and three-dimensional profiling, showcasing its inherent morphological intricacies. The multidimensional characterization provided herein contributes significantly to the evolving landscape of biocomposite research, fostering a platform for future advancements and innovations in HRF-based composite materials.

Jet cavitation-enhanced hydration method for the preparation of magnesium hydroxide

During the preparation of magnesium hydroxide via the hydration method, in-situ growth and agglomeration often inhibit the reaction. This study used active magnesium oxide as the raw material and employed jet cavitation technology to enhance the hydration process. Based on the growth process of magnesium hydroxide, the mechanism of jet-enhanced hydration was analyzed. The effects of reaction temperature (T), reaction time (t), solid-liquid ratio (s), and cavitation number (σ) on the hydration rate were investigated. An L25(54) orthogonal experiment explored the significance of each factor's impact on the hydration rate. The hydration products were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), and a specific surface area analyzer. Results indicate that the factors affecting the hydration rate, in order of significance, are cavitation number > reaction temperature > solid-liquid ratio > reaction time. The optimal process parameters were determined to be a reaction temperature of 70 °C, reaction time of 80 min, solid-liquid ratio of 1:12, and cavitation number of 0.42. Under these conditions, the hydration rate reached 94.87 %, producing well-dispersed lamellar magnesium hydroxide with a narrow particle size distribution (median particle size D50 = 4.511 μm) and a BET specific surface area of 11.345 m²/g.

Investigation of Ceria based Heterostructure Composite Mixed Matrix Membrane with Polybenzimidazole for Polymer Electrolyte Fuel Cell Application at High Temperature

In recent years Ceria based heterostructure composites are considered as one of the highest performing solid state ionic conductors, therefore we wanted to leverage the benefits of using these materials for high temperature Proton Exchange Membrane Fuel Cells (PEMFCs). In this study a Polybenzimidazole (PBI)/Ceria carbonate CHC (Ceria based heterostructure composite) membrane was prepared by drop casting method and tested as an electrolyte for a high temperature H2/Air PEMFC application in anhydrous condition. Inorganic composite of ceria and alkali metal carbonates (Li2CO3, Na2CO3) was prepared by solid state route to obtain Ceria carbonate CHC. X-Ray diffraction (XRD) study confirmed the formation of the heterostructure and their successful incorporation into the PBI membranes. Homogeneity of fillers inside the membrane was further verified by Energy Dispersive X-Ray Analysis (EDAX) and Scanning Electron Microscopy (SEM). 5wt% of inorganic powder induced inside the PBI fillers reduced the phosphoric acid uptake of composite membrane (∼17% less) compared to pristine PBI membrane, which ultimately resulted into a lower swelling and dimensional change of the composite membrane. Thermal robustness of the phosphoric acid doped composite and pristine PBI membranes was investigated by thermogravimetric analysis (TGA) which showed that the prepared membranes were gone under a less than 10% reduction in weight up till 200ºC, ensuring their validity of application in high temp PEM fuel cells. The added inorganic functionalities resulted in a slight increase in the proton conductivity of PA doped composite PBI membranes i.e., 42.3 mS cm-1 at 180 ºC while for pristine PBI membrane it is 36 mS cm-1 at same temperature. A single cell with composite PBI membranes outperformed a pristine PBI membrane resulted into a ∼120% higher peak power density i.e., 320.88 mW cm-2. The composite membrane also displayed the excellent durability and showed a less than 10-4 mV/h degradation in cell potential till 180 ºC.

Phosphate's second life: Upcycling phosphogypsum and clay by-product through acid geopolymer technology

The present study explores the repurposing of large amounts of phosphoric acid by-products, specifically phosphogypsum (PG), by evaluating its effectiveness as a precursor in acid-activated geopolymer technology. Geopolymers were elaborated using PG and calcined clays, activated with phosphoric acid. The research focused on evaluating the mechanical properties and microstructure of these geopolymers after a 28-day curing period. X-ray diffraction (XRD) analysis revealed the formation of new crystalline phases, including brushite, newberite, and berlinite. Fourier-transform infrared (FTIR) spectroscopy confirmed the presence of P-O and Si-O-Al bonds, indicative of successful geopolymerization. Scanning electron microscopy (SEM) imaging demonstrated a dense, cohesive microstructure in optimized samples. Based on the response surface methodology, the study identified optimal conditions for maximum compressive strength: 28.83% PG content, 14.39mol/L phosphoric acid concentration, and a curing temperature of 72.45°C. This optimized formulation produced a dense, cohesive microstructure with a notable compressive strength of 21.46MPa. The leaching test confirmed that no harmful substances were released from the geopolymer samples. These results suggest that PG can be effectively recycled through geopolymer technology for use in the construction industry.

Effect of H2O2/ascorbic acid degradation and gradient ethanol precipitation on the physicochemical properties and biological activities of pectin polysaccharides from Satsuma Mandarin

In this work, three degraded polysaccharides (DMPP-40, DMPP-60, DMPP-80) were successfully obtained by H2O2/ascorbic acid degradation and gradient ethanol precipitation from Satsuma mandarin peel pectin (MPP), and their physicochemical properties, antioxidant and prebiotic activities were investigated. The molecular weight of MPP, DMPP-40, DMPP-60, DMPP-80 were determined to be 336.83 ± 10.57, 18.93 ± 0.54, 26.07 ± 0.83 and 8.71 ± 0.27 kDa, respectively. The ethanol concentration significantly affected the physicochemical properties of DMPPs. DMPP-60 showed the highest yield (69.07 %) and uronic acid content (64.85 %), DMPP-80 showed the lowest molecular weight (8.71 kDa), and the composition and proportion of monosaccharides of DMPPs were significantly different. Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy (1H NMR) confirmed that DMPPs exhibited similar functional groups, while X-ray diffraction (XRD) indicated that DMPP-40 possessed some crystallographic sequences. Scanning electron microscopy (SEM) images directly verified the fragmented structure and reduced surface area of DMPPs. Besides, the H2O2/ascorbic acid treatment could obviously reduce the apparent viscosity and thermal stability of MPP. Meanwhile, the results of bioactivity assay showed that DMPPs possessed better antioxidant activity and probiotics pro-proliferative effects compared with MPP. DMPP-80 could significantly inhibit lipopolysaccharides (LPS)-stimulated production of inflammatory factors (including nitric oxide (NO), interleukin (IL)-6, tumor necrosis factor (TNF)-α and interleukin (IL)-1β) in RAW264.7 cells. Results suggest that the H2O2/ascorbic acid combined with gradient ethanol precipitation has potential applications in degradation and separation of MPP to improve its biological activities.

Optimizing the content of Li2CO3, Na2SO4 and TEA in fly ash–cement system by response surface methodology

With an optimized dosage, hardening accelerators become a vital means of modifying fly ash-cement system (FAC). This study comprehensively investigated the mechanical properties of FAC modified by Li2CO3, Na2SO4, and triethanolamine (TEA) under different dosages, and optimized the dosage of accelerators through the response surface method (RSM). The synergistic effect of accelerators on the hydration of FAC was characterized by thermogravimetric differential scanning calorimetry (TG-DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The results demonstrated that the factors and response value followed a quadratic polynomial model. The regression coefficients R2 of the model were all greater than 0.9, indicating good agreement with the experimental data. The content of Li2CO3 and Na2SO4 had an extremely significant effect on the compressive strength of 1d and 3d, followed by TEA. The optimal mix ratio predicted by RSM was 0.12% Li2CO3, 0.47% Na2SO4, and 0.40% TEA. Early hydration stages revealed that the combined action of these accelerators increased the formation of CH, CaCO3, and amorphous C-(A)-S-H gel. Microscopically, the surface of fly ash exhibited alkali-induced corrosion, thereby enhancing its pozzolanic reactivity.

Preliminary investigation on spent garnet as a novel supplementary cementitious material

The escalating global demand for cement, a fundamental material in infrastructure development, has exacerbated environmental challenges, particularly through significant carbon dioxide (CO₂) emissions, which account for approximately 8.3 % of global anthropogenic CO₂ output. This research explores the potential of spent garnet powder, a byproduct of abrasive water jet machining, as a sustainable supplementary cementitious material (SCM) to mitigate these impacts. The spent garnet powder, characterized by a high concentration of silicon dioxide (SiO₂), aluminum oxide (Al₂O₃), and iron oxide (Fe₂O₃), was subjected to rigorous analysis. X-ray Fluorescence (XRF) confirmed its chemical suitability for pozzolanic applications, while laser particle size analysis revealed a finer granulometry relative to Ordinary Portland Cement (OPC), which is advantageous for enhancing pozzolanic reactivity. Scanning Electron Microscopy (SEM) demonstrated the angular and irregular morphology of the garnet particles, which is conducive to improved interfacial bonding within the cement matrix. X-ray Diffraction (XRD) identified active mineral phases that are critical for promoting pozzolanic reactions, and Thermogravimetric Analysis (TGA) demonstrated the material’s superior thermal stability, with minimal decomposition at elevated temperatures. Fourier Transform Infrared Spectroscopy (FTIR) identified strong silicon-oxygen (Si-O) and aluminum-oxygen (Al-O) bond structures, indicative of robust pozzolanic potential. The Strength Activity Index (SAI) and Frattini tests further substantiated the pozzolanic activity, revealing that a 10 % replacement of OPC with SGP not only enhances compressive strength but also meets the stringent requirements of ASTM C618. Additionally, the economic analysis underscores the cost-effectiveness of utilizing spent garnet powder, presenting a viable strategy for reducing both production costs and CO₂ emissions in the cement industry. This study conclusively positions spent garnet powder as a highly promising supplementary cementitious material, with significant implications for advancing sustainable construction practices and reducing the environmental footprint of cement production.