Thermogravimetric Differential Thermal Analysis Research Articles

Synthesis and characterization of multi-responsive iron oxide nanoparticles: Evaluation of antibacterial properties and photocatalytic activity

Cape gooseberry (CG) plant leaf extract-mediated iron oxide nanoparticles (CG-IO NPs) were fabricated for antibacterial research. The ideal concentration of the precursor salt, pH (11) of the reaction mixture, reducing agent to precursor salt ratio, and the production time of iron oxide nanoparticles were 5 mM, 9.0, 3:7, and 25 min, respectively. The iron oxide nanoparticles were tested using ultraviolet–visible absorption spectroscopy, photoluminescence (PL) spectroscopy, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric/differential thermal analysis (TG/DTA), and Fourier transform infrared (FTIR) spectroscopy. FTIR spectroscopy was used to identify functional groups of the compounds, including the carbonyl, CH, and OH bands that reduced and produced nanoparticles. The size and shape of the synthesized CG-IO NPs were determined by TEM and dynamic light scattering, with the median and mean size of 13.9 nm and 15.8 nm, respectively. The thermal stability of the synthesized CG-IO NPs was assessed using TG/DTA in a nitrogen atmosphere. The elements and oxidation states of the CG-IO NP components were examined by XPS. The luminosity of the CG-IO NP was examined using PL spectroscopy. The synthetic CG-IO NPs exhibited strong antibacterial effects against dangerous bacteria, such as Salmonella enterica (S. entirica), Escherichia coli (E. coli), Streptococcus agalactiae, and Staphylococcus aureus. CG-IO NPs assisted in water reclamation by decomposing Malachite Green dye under solar light irradiation.

Date palm (Phoenix dactylifera L.) pollen-based microgel and its promising medical and environmental applications

Pollen, a natural bi-layered porous microcapsule, plays a crucial role in plant reproduction by protecting the plant's genetic material. Due to its unique properties, it has garnered attention for medical and environmental applications. Recent studies have focused on transforming the pollen's rigid structure to soft, gel-like matter, enabling the creation of pollen-based products such as paper and sponge. The main factor in the gelation process involves pectin-to-pectate conversion within the pollen's inner layer. Previously, claimed that this transformation is restricted to eudicot plants, and some others, such as monocot plant pollens do not exhibit this gelation phenomenon. In this study, we successfully produced microgel from date palm (Phoenix dactylifera L.) pollen (DPP), challenging this assertion. A significant portion of these monocot plant pollens exceeds the requirement of date production, presenting an opportunity for large-scale production without environmental concerns. Here, we have prepared pollen-based microgel, paper, and sponge and conducted a comprehensive analysis using various techniques such as optical and fluorescence microscopy, scanning electron microscopy (SEM), Brunauer-Emmett-Teller (BET), elemental CHN analysis, Fourier-transform infrared spectroscopy (FTIR), thermogravimetric differential thermal analysis (TGA/DTA), rheological measurements, mechanical analysis, pH-sensitivity tests, swelling analysis, and oil absorption capacity. By discerning the specific physicochemical properties of these materials, we propose potential medical and environmental applications for further investigation.

Green Synthesis of Al-ZnO Nanoparticles Using Cucumis maderaspatanus Plant Extracts: Analysis of Structural, Antioxidant, and Antibacterial Activities.

Nanoparticles derived from biological sources are currently garnering significant interest due to their diverse range of potential applications. The purpose of the study was to synthesize Al-doped nanoparticles of zinc oxide (ZnO) from leaf extracts of Cucumis maderaspatanus and assess their antioxidant and antimicrobial activity using some bacterial and fungal strains. These nanoparticles were analyzed using X-ray diffraction (XRD), ultraviolet-visible (UV-vis) spectroscopy, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM), and thermogravimetric analysis/differential thermal analysis (TG-DTA). The average crystalline size was determined to be 25 nm, as evidenced by the XRD analysis. In the UV-vis spectrum, the absorption band was observed around 351 nm. It was discovered that the Al-ZnO nanoparticles had a bandgap of 3.25 eV using the Tauc relation. Furthermore, by FTIR measurement, the presence of the OH group, C=C bending of the alkene group, and C=O stretching was confirmed. The SEM analysis revealed that the nanoparticles were distributed uniformly throughout the sample. The EDAX spectrum clearly confirmed the presence of Zn, Al, and O elements in the Al-ZnO nanoparticles. The TEM results also indicated that the green synthesized Al-ZnO nanoparticles displayed hexagonal shapes with an average size of 25 nm. The doping of aluminum may enhance the thermal stability of the ZnO by altering the crystal structure or phase composition. The observed changes in TG, DTA, and DTG curves reflect the impact of aluminum doping on the structural and thermal properties of ZnO nanoparticles. The antibacterial activity of the Al-ZnO nanoparticles using the agar diffusion method showed that the maximum zone of inhibition has been noticed against organisms of Gram-positive S. aureus compared with Gram-negative E. coli. Moreover, antifungal activity using the agar cup method showed that the maximum zone of inhibition was observed on Aspergilus flavus, followed by Candida albicans. Al-doping nanoparticles increases the number of charge carriers, which can enhance the generation of reactive oxygen species (ROS) under UV light exposure. These ROS are known to possess strong antimicrobial properties. Al-doping can improve the crystallinity of ZnO, resulting in a larger surface area that facilitates more interaction with microbial cells. The structural and biological characteristics of Al-ZnO nanoparticles might be responsible for the enhanced antibacterial activity exhibited in the antibacterial studies. Al-ZnO nanoparticles with Cucumis maderaspatanus leaf extract produced via the green synthesis methods have remarkable antioxidant activity by scavenging free radicals against DPPH radicals, according to these results.

Efficient Catalytic Reduction of Organic Pollutants Using Nanostructured CuO/TiO2 Catalysts: Synthesis, Characterization, and Reusability

The catalytic reduction of organic pollutants in water is a critical environmental challenge due to the persistent and hazardous nature of compounds like azo dyes and nitrophenols. In this study, we synthesized nanostructured CuO/TiO2 catalysts via a combustion technique, followed by calcination at 700 °C to achieve a rutile-phase TiO2 structure with varying copper loadings (5–40 wt.%). The catalysts were characterized using X-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR–FTIR) spectroscopy, thermogravimetric analysis-differential thermal analysis (TGA–DTA), UV-visible diffuse reflectance spectroscopy (DRS), and scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM–EDS). The XRD results confirmed the presence of the crystalline rutile phase in the CuO/TiO2 catalysts, with additional peaks indicating successful copper oxide loading onto TiO2. The FTIR spectra confirmed the presence of all the functional groups in the prepared samples. SEM images revealed irregularly shaped copper oxide and agglomerated TiO2 particles. The DRS results revealed improved optical properties and a decreased bandgap with increased Cu content, and 4-Nitrophenol (4-NP) and methyl orange (MO), which were chosen for their carcinogenic, mutagenic, and nonbiodegradable properties, were used as model organic pollutants. Catalytic activities were tested by reducing 4-NP and MO with sodium borohydride (NaBH4) in the presence of a CuO/TiO2 catalyst. Following the in situ reduction of CuO/TiO2, Cu (NPs)/TiO2 was formed, achieving 98% reduction of 4-NP in 480 s and 98% reduction of MO in 420 s. The effects of the NaBH4 concentration and catalyst mass were investigated. The catalysts exhibited high stability over 10 reuse cycles, maintaining over 96% efficiency for MO and 94% efficiency for 4-NP. These findings demonstrate the potential of nanostructured CuO/TiO2 catalysts for environmental remediation through efficient catalytic reduction of organic pollutants.

The effects of filling method on silicone rubber composites filled with SiO2 and TiO2

Silica (SiO₂) serves as a reinforcing filler, while titanium dioxide (TiO₂) functions as a functional filler, imparting exceptional mechanical strength and UV resistance to silicone rubber. However, compatibility issues may arise when both fillers are incorporated into silicone rubber. This study explores potential solutions through processing methods, specifically by comparing the effects of graded filling and mixed filling on the properties of silicone rubber. Field emission scanning electron microscopy reveals that the mixed filling method promotes a more uniform dispersion of fillers, leading to enhanced performance. Curing tests indicate that the effect of the filling method on the curing processing performance of silicone rubber is negligible. Tensile test results reveal that, compared to the graded filling system, the mixed filling system improves the tensile strength and elongation at break of the silicone rubber composites by 13% and 13.4%, respectively, while simultaneously reducing the Mullins effect, thereby enhancing material stability. Thermogravimetric analysis (TGA) and differential thermal analysis (DTG) results indicate that the uniform dispersion achieved through mixed filling optimizes thermal transfer pathways, resulting in superior thermal stability compared to graded filling. Ultraviolet (UV) spectroscopy results demonstrate that composites containing added TiO₂ exhibit almost zero transmittance in the UV range of 200-400 nm, underscoring their excellent UV resistance; the mixed filling method provides superior UV protection compared to the graded fill method. In summary, for the dual-filler system of SiO₂ and TiO₂, the mixed filling approach enhances filler compatibility by improving dispersion, thereby elevating material performance and broadening potential applications.

Low-cost preparation and characterization of new CuO/ZnO and Cu3N/ZnO nanocomposites

CuO/ZnO and Cu3N/ZnO nanocomposites were prepared in a three-step synthesis consisting of the co-precipitation of Cu2+ and Zn2+ hydroxide carbonates (Cu/Zn-Carb) followed by their thermal treatment first in air and second in gaseous ammonia. The morphology and phase composition of the hydroxide carbonates were determined by the Cu:Zn molar ratio and the presence of polyvinylpyrrolidone (PVP) acting as a capping agent, respectively. The Cu/Zn-carbonates could be annealed in the air at 550 °C either as powders or as thin films. The latter were deposited on a silicon substrate using a choice of spin- or dip-coating techniques. The resulting CuO/ZnO samples were heated under gaseous ammonia at 300 °C in the final step of the process to form Cu3N/ZnO nanocomposites. The fabricated samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) with energy dispersive X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), thermogravimetric − differential thermal analysis (TG-DTA) and infrared spectroscopy (IR). SEM and XRD analysis indicates that the average diameter of spherical particles was about 130 nm (CuO/ZnO) and 100 nm (Cu3N/ZnO), composed of crystallites with 10–20 nm sizes. The thermal treatment under air and NH3 did not affect the morphology of the composites. The implication is, therefore, that the shape and size of CuO/ZnO oxide and Cu3N/ZnO nitride/oxide composite nanostructures are determined at the point of hydroxide carbonate coprecipitation and can be controlled during precursor synthesis. This has significant ramifications for the reproducible fabrication of nanocomposite films of precise stoichiometry and bespoke morphology.

Thermoanalytical and Kinetic Studies for the Thermal Stability of Emerging Pharmaceutical Pollutants Under Different Heating Rates.

Emerging pharmaceutical pollutants like ciprofloxacin (CIP) and ibuprofen (IBU) are frequently detected in aquatic environments, posing risks to ecosystems and human health. Since pollutants rarely exist alone in the environment, understanding the thermal stability and degradation kinetics of these compounds, especially in mixtures, is crucial for developing effective removal strategies. This study therefore investigates the thermal stability and degradation kinetics of CIP and IBU, under different heating rates. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were employed to examine the thermal behavior of these compounds individually and in mixture (CIP + IBU) at heating rates of 10, 20, and 30 °C/min. The kinetics of thermal degradation were analyzed using both model-fitting (Coats-Redfern (CR)) and model-free (Kissinger-Akahira-Sunose (KAS), Flynn-Wall-Ozawa (FWO), and Friedman (FR)) methods. The results showed distinct degradation patterns, with CIP decomposing between 280 and 550 °C and IBU between 152 and 350 °C, while the mixture exhibited multistep decomposition in the 157-500 °C range. The CR model indicated first-order kinetics as a better fit for the degradation (except for IBU). Furthermore, CIP exhibits higher thermal stability and activation energy compared to IBU, with the KAS model yielding activation energies of 58.09 kJ/mol for CIP, 11.37 kJ/mol for IBU, and 41.09 kJ/mol for CIP + IBU mixture. The CIP + IBU mixture generally showed intermediate thermal properties, suggesting synergistic and antagonistic interactions between the compounds. Thermodynamic parameters (ΔH°, ΔG°, ΔS°) were calculated, revealing non-spontaneous, endothermic processes for all samples (except in the FWO method) with a decrease in molecular disorder and positive ΔG° values across all models and heating rates. The study found that higher heating rates led to less thermodynamically favorable conditions for degradation. These findings provide important information concerning the thermal behavior of these pharmaceutical pollutants, which can inform strategies for their removal from the environment and the development of more effective waste-treatment processes.

Evaluating the thermal stability of hazelnut oil in comparison with common edible oils in Turkey using ATR infrared spectroscopy

Hazelnut oil (HO), a high-quality nutrient rich in monounsaturated fatty acids and antioxidants, is not commonly used due to a lack of awareness of its nutritional benefits. The purpose of the current study is to evaluate the stability of HO during the heating process in comparison with Riviera olive, sunflower and corn oils, the most commonly used edible oils in Turkey, by using Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR). The oils were heated at 180 °C for 24h, divided into 8-h periods over the course of three days and the measurements were performed on oil samples taken every 2h. Thermogravimetric analysis-differential thermal analysis (TGA-DTA) and the measurement of the specific absorbance of conjugated dienes and trienes by using UV-visible spectroscopy were also performed to confirm the ATR-FTIR data. The spectroscopic results showed that the heating process led to an increase in the amount of primary and secondary oxidation products, a decrease in the amount of cis fatty acids and an increase in the amount of trans fatty acids in all oils. Based on the results of linear regression analysis, HO has the lowest slope value for all parameters, indicating that it is the most resistant to thermal oxidation. Principal Component Analysis (PCA), Hierarchical Cluster Analysis (HCA) and TGA-DTA results confirmed that HO has a higher thermal stability than the other oils. These findings revealed that HO has the highest thermal stability among the oils compared and can be utilized as a healthy alternative for cooking. This study also showed that ATR-FTIR spectroscopy holds significant promise in oil analysis, competing with routine quality control techniques.

Synthesis and characterization of thermal properties of poly(p-cumylphenyl methacrylate-co-methoxyethyl methacrylate) copolymers

The poly(p-cumylphenyl methacrylate-co-methoxyethyl methacrylate) copolymers has been fabricated in a simple way. The p-cumylphenyl methacrylate and methoxy methacrylate were polymerized by free radical mechanism using benzoyl peroxide as an initiator. The synthesized copolymers were confirmed by Fourier transform infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H NMR) and carbon nuclear magnetic resonance (13C NMR) spectral techniques. The heat durability of copolymers has been investigated by Thermogravimetric analysis (TGA), derivative thermogravimetry, and differential thermal analysis (DTA). The glass transition temperature (Tg) of copolymer was carried out using differential scanning calorimetry (DSC). The scanning electron microscopy (SEM) was utilized to observe the surface texture and morphology roughness of copolymers. The obtained copolymers have possess an excellent coating property, anti-corrosive property, and optical property. Hence, these can be utilize in different way like solar, sensors, polymer conductivity, battery electrolytes, nanotechnology, viscosity, and biomedical.

Synthesis and Properties of a Red Na5Zn2Gd1−x(MoO4)6: xEu3+ Phosphor

Novel Eu3+-doped Na5Zn2Gd(MoO4)6 triple molybdate phosphors were fabricated by the sol-gel method. The structure, morphology, and luminescent properties have been characterized by X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), FTIR spectroscopy, and luminescence spectroscopy. The results indicated that the synthesized Na5Zn2Gd1−x(MoO4)6: xEu3+ phosphor consisted of a pure phase with monoclinic structure. Under excitation at 465 nm, the Na5Zn2Gd1−x(MoO4)6: xEu3+ phosphor exhibits an intensive red emission band around 610 nm corresponding to the transition of 5D0→7F2 which is much higher than that 5D0→7F1 at 594 nm, which was appropriate for a blue LED. According to the influence of the synthesis conditions, the phosphors showed the highest emission intensity when the doping concentration of Eu3+ was 25 mol.% and the molar ratio of citric acid to metal ions was 2:1. Na5Zn2Gd0.75(MoO4)6: 0.25 Eu3+ with the color coordinates (x = 0.658, y = 0.341) is a more stable red phosphor for blue-based white LEDs than the commercial Y2O2S: Eu3+ red phosphor (0.48, 0.50) due to its being closer to the NTSC standard values (0.670, 0.330).

Plant-mediated synthesis, characterization, and evaluation of a copper oxide/silicon dioxide nanocomposite by an antimicrobial study

Abstract This study presents an innovative, environmentally friendly method for biosynthesizing copper oxide–silica (Cu2O/SiO2) nanocomposites (CSNCs) utilizing an aqueous leaf extract of Callistemon viminalis (C. viminalis). The goal of this work is to fabricate CSNCs using a less hazardous and sustainable synthesis approach. Copper acetate and sodium metasilicate were used as precursors, whereas the C. viminalis green leaf extract was used as the reducing and stabilizing agent. Analysis of the plant extract using Fourier transform infrared spectroscopy indicated the presence of polyphenolic compounds, primarily phenolic acids, which functioned as both reducing and stabilizing agents in the synthesis of CSNCs. A combination of energy dispersive X-ray spectroscopy and scanning electron microscopy was used to study the formation of spherical copper–silica hybrid nanostructures. Powder X-ray diffraction analysis revealed the successful integration of silica with copper(i) oxide (Cu2O) through the presence of distinct Cu2O peaks and a broad amorphous SiO2 peak at 2θ = 22.77°. The thermal stability of the nanocomposites (NCs) was assessed using thermogravimetric analysis and differential thermal analysis under a nitrogen atmosphere. The biogenic NCs also successfully inhibited pathogenic strains of Staphylococcus aureus (S. aureus) and Candida albicans (C. albicans); however, S. aureus was found to be more susceptible to the biocidal activity of the NCs than P. aeruginosa. These findings suggest that this simple, cost-effective, and eco-friendly method for producing biologically active hybrid nanomaterials holds significant promise for future applications in both biological and materials sciences.

Quantitatively characterization of rare earth ore by terahertz time-domain spectroscopy

The Bayan Obo deposit is the world’s largest polymetallic associated minerals deposit of rare earths, iron and niobium, and the rarity of its physical properties restrict the knowledge and understanding of its laws. Taking the high-grade mixed rare earth concentrate of Bayan Obo as the research object, terahertz time-domain spectroscopy (THz-TDS) has been adopted for the systematic investigation of high-grade rare earth concentrate base on the traditional X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) and thermogravimetric-differential thermal analysis (TG-DTA). The absorption coefficient and refractive index of high-grade rare earth ores and their associated minerals of fluorite and dolomite, are all investigated by terahertz time-domain spectroscopy. The terahertz spectral response is affected by the type of mineral and its content. The acquired rare earth terahertz spectral data are processed by correlation analysis. Three machine learning algorithms, Partial Least Squares Regression (PLSR), Random forest (RF) and Multilayer Perceptron (MLP), are used to achieve quantitative detection of their concentrations and components with the coefficient of determination R2 of the absorption coefficient of the optical parameter reaching up to 0.975, 0.992 and 0.984, respectively. This work promotes the growing understanding of terahertz transmission spectroscopy of rare earth-bearing minerals, which can be used to help guide the search for minerals, and to detect, identify as well as quantify them in geology. Terahertz time-domain spectroscopy supplies a new method for study of rare earth resources, and the comprehensive development and utilization of resources in the Bayan Obo deposit.

Removal of acetyl-rich impurities from chitosan using liquefied dimethyl ether

Chitosan, recognized for its excellent biodegradability, biocompatibility, and antibacterial properties, has several potential applications, particularly in the biomedical field. However, its widespread use is hindered by inherent limitations such as low mechanical strength and safety concerns arising from a low degree of deacetylation and the presence of impurities. This study aimed to introduce an innovative purification method for chitosan via liquefied dimethyl ether (DME) extraction. The proposed technique effectively addresses the challenges associated with chitosan by facilitating deacetylation and impurity removal. Liquefied DME is emerging as the extraction solvent of choice owing to its advantages, such as low boiling point, safety, and environmental sustainability. The degree of deacetylation of chitosan was extensively evaluated using thermogravimetric–differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, intrinsic viscosity measurements, solid-state nuclear magnetic resonance spectroscopy and X-ray photoelectron spectroscopy, and elemental analysis. The solubility of chitosan in liquefied DME was investigated using Hansen solubility parameters. This study contributes to the improvement of the safety profile of chitosan, thereby expanding its potential applications in various fields. The use of liquefied DME as an extraction solvent proved to be efficient in addressing the existing challenges and is consistent with the principles of safety and environmental sustainability.

An experimental insight into a promising novel organic nonlinear optical single crystal Guanidinium 2,4-dichlorobenzoate (G24DCB)

Guanidinium 2,4-dichlorobenzoate (G24DCB), a new chloro substituted benzoic acid based organic single crystal is synthesized, grown and added to the guanidinium family of single crystals. Such G24DCB crystal was obtained by a versatile slow evaporation solution growth technique. The analysis of single crystal X-ray diffraction examined the phase identification and determination of lattice parameters for the synthesized compound. The G24DCB crystal has monoclinic system and adopts space group P21/c. Powder X-ray diffraction explores the studied crystal's crystalline characteristics. The study of Fourier Transform-Infrared (FTIR) spectroscopy examined the necessary vibrational assignments for the formation of the structure of G24DCB. The UV–Visible-NIR analysis entails the determination of the cut-off wavelength of the G24DCB compound from its transmittance spectrum and the computation of other related optical parameter values. Photoluminescence analysis was employed to investigate the studied crystal's emission characteristics. The thermal stability of the G24DCB crystal was examined through thermogravimetric analysis and differential thermal analysis. The laser-induced damage threshold of the crystal was determined using a Nd:YAG laser. The various mechanical attributes exhibited by the synthesized compound were elucidated by microhardness studies and it corresponds to a soft material type. The various third order nonlinear optical characteristics were probed by Z scan study. The positive results of the aforementioned studies suggest the emerging significance possessed by the novel title crystal Guanidinium 2,4-dichlorobenzoate in nonlinear optical applications.

Tunable annealing effect to enhance structural and magnetic properties of spinel cobalt magnesium ferrite nanoparticles

Cobalt magnesium ferrite nanoparticles, with the chemical formula Co0.5Mg0.5Fe2O4 (CMFO), were synthesized via co-precipitation and subjected to annealing at 200–800 °C with a step size of 200. Thermal analysis for the as-dried sample was investigated through thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The presence of a plateau region in the DTA curve above 366 °C, combined with the slight weight loss noted in the TGA curve, indicates that the ferrite sample, specifically CMFO, has successfully transitioned into its final phase. X-ray diffraction and Fourier transform infrared spectroscopy (FTIR) analysis unveiled the formation of spinel CMFO NPs belonging to the Fd-3m space group. The Williamson–Hall method showed particle size increasing from 8.20 to 52.15 nm and tensile microstrain decreasing from 6.90 to 1.84 × 10−3 with higher annealing temperatures, noted by the shift of the (311) plane. TEM images confirmed the formation of smaller nanoparticles with minimal agglomeration. Particles of nearly uniform size are achieved at the optimum annealing temperature of 600 °C, owing to its narrow distribution profile. The experimental magnetization data were analyzed using the Langevin function and the law of approach to saturation to determine the saturation magnetization, spanning from 15.46 to 43.90 emu/g. The magnetic characteristics of the annealed samples exhibited a rise in coercive force, reaching up to 349.74 Oe with the elevation of the annealing temperature. The range of attributes exhibited by CMFO makes it highly advantageous for various applications, including sensor technology, high-frequency devices, and energy storage devices.

A facile synthesis procedure for Engelhard titanosilicate (ETS-4) and its Cs+ and Sr2+ ion exchange properties

This manuscript reports an environmentally benign method for the synthesis of Engelhard titanosilicate (ETS-4) using titanium isopropoxide or anatase as titanium source and citric acid as complexing agent. Slow release of Ti from the hydroxide or oxide precursors through the citric acid complex plays crucial role in formation of titanosilicate. Characterizations of the prepared material were carried out by powder X-ray diffraction (XRD), Scanning Electron Microscope – Energy Dispersive X-ray spectroscopy (SEM-EDS), Thermogravimetric – Differential Thermal Analysis (TG-DTA) and ion exchange studies. Caesium and strontium exchange capacities of the synthesised ETS-4 were found to be 220 mg/g and 76.2 mg/g, respectively. The saturation exchange equilibrium was attained within 60 min.

Enhanced morphological and thermal properties of epoxy composites reinforced with Palm and Prosopis Juliflora fibers

Abstract This study investigates the fabrication and characterization of a hybrid epoxy matrix composite reinforced with Palm and Prosopis Juliflora fibers fabricated using the hand layup technique. Three composite samples were prepared with varying weight percentages of palm and Prosopis Juliflora fiber reinforcements: 5% (Sample A), 10% (Sample B), and 15% (Sample C). Sample B having 10 weight percentage each of Palm fiber and Prosopis Juliflora fiber and 80 weight percentage of Epoxy matrix, exhibited superior performance with a tensile strength of 45.5 MPa and a hardness of 86.5 Shore D. Thermal analysis revealed Sample B’s exceptional thermal stability, with distinct decomposition stages observed through Thermogravimetric Analysis (TGA) and Differential Thermal Analysis (DTA). Void content analysis indicated Sample C had the lowest void content at 4.5%. Energy Dispersive x-ray (EDX) Analysis confirmed homogeneous fiber distribution and strong fiber-matrix adhesion, supported by carbon and oxygen peaks. Fourier-transform infrared spectroscopy (FTIR) spectra showed interactions between functional groups, including alcohols, carboxylic acids, and carbonyl compounds. These findings underscore the composite’s potential for high strength, toughness, and thermal stability applications.

Phase evolution and heavy metal solidification of cement desulphurized electrolytic manganese residue composite cementitious system under steam curing conditions based on thermodynamic simulation

The mechanical properties and microstructure of desulphurized electrolytic manganese (D-EMR) cement mortar under steam curing at 80 °C for 7 h and 7 days and standard curing for 3 days and 28 days were studied. The hydration products, microstructure and pore distribution were studied by Quantitative X-ray diffraction analysis (QXRD), scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS), thermogravimetric-differential thermal analysis (TG-DTA) and backscattered electron (BSE). At the same time, the evolution of hydration products with age and the existence form of heavy metals under different curing conditions were simulated by GEMS thermodynamics. The results show that steam curing can promote the hydration reaction of cement and the secondary hydration of D-EMR. With the extension of steam curing time, the mechanical properties of the early stage are significantly improved. At a D-EMR content of 15 %, the compressive strength of D-EMR cement mortar after steam curing for 7 days is 1.15 times that of the control group under the same conditions, and the content of calcium hydroxide (CH) is 65.91 % of the control group. Steam curing can significantly improve the degree of C3S hydration of cement clinker and the secondary hydration of D-EMR, and increase the degree of polymerization of hydrated calcium silicate (C-S-H) gel. In addition, thermodynamic simulation showed that when the pH value was greater than 7.5, Mn2+ was mainly stable in the form of Mn(OH)2, MnOOH and Mn3O4, and there was no leaching risk. This will provide theoretical support for the use of D-EMR as a new type of supplementary cementitious material (SCM).

Enhancing mechanical properties of PVC composites through surface composite modified calcium sulfate whiskers

Abstract To enhance the high-value utilization of industrial wastewater, this study used ammonium sulfate wastewater discharged from a rare earth plant as a raw material for producing anhydrous calcium sulfate whiskers (CSWs) through a hydrothermal method. Subsequently, the whiskers underwent modification using a C18H36O2–titanate coupling agent. The modification mechanism of CSW was investigated by comparing the surface contact angle before and after modification, along with characterization and analysis involving X-ray diffraction, scanning electron microscopy, Fourier-transform infrared spectroscopy, thermogravimetric-differential thermal analysis, and X-ray photoelectron spectroscopy. Finally, composite-modified calcium sulfate whiskers (CMCSWs) were incorporated into polyvinyl chloride (PVC) composites, and their mechanical properties were evaluated. The results indicated that at a modifier dosage of 15%, a modification time of 25 min, a modification temperature of 80°C, a stirring speed of 400 rpm, a drying temperature of 100°C, and a C18H36O2-to-titanate coupling agent compound ratio of 1:2, the contact angle reached 124.45°, and a nanoscale hydrophobic layer with a thickness of 15.63 nm was formed on the surface. Regarding PVC reinforcement, the tensile strength and elongation at the break of PVC composite with 15 parts of CMCSW added increased by 73 and 262%, respectively, compared to the material without CSW. This CSW serves as an innovative reinforcing agent for PVC composites. The study developed modified CSW with high hydrophobicity, offering theoretical insights for effectively modifying fiber-type whiskers and their reinforcement in PVC applications.

Research on the mechanism of natural antibacterial properties of Calotropis gigantea fiber

This research explores the antibacterial mechanism of Calotropis gigantea (CG) fiber through systematic antimicrobial testing and microstructural characterizations on different types of dried CG fibers. Different temperatures and light exposure times were employed to prepare a series of fiber samples. Standard antimicrobial tests were conducted, revealing that both light exposure time and drying temperature significantly influenced the fiber's antibacterial properties against Escherichia coli. Prolonged light exposure time and drying temperatures notably suppressed the antibacterial efficacy. Chemical composition, surface morphology, and thermal stability were further investigated using various techniques, including laser microscopy, Raman, FTIR, and X-ray photoelectron spectroscopies, as well as thermogravimetric-differential thermal analysis. The results revealed a minor role of surface profile and lignin in the variation of antibacterial properties of CG fiber, which should mainly be associated with the alteration of flavonoids, despite the presence of distinct mass losses and decomposition temperature shifts after fiber drying. This study not only unveils and confirms the resource and mechanism of the antimicrobial activity of Calotropis gigantea fiber but also provides insights to guide future optimization of processes and control of microstructure. These findings hold promise for the development of Calotropis gigantea fiber applications in antibacterial products.