Visible Spectrophotometry Research Articles

Harnessing Walnut-Based Zinc Oxide Nanoparticles: A Sustainable Approach to Combat the Disease Complex of Meloidogyne arenaria and Macrophomina phaseolina in Cowpea

Zinc oxide nanoparticles (ZnO NPs) exhibit diverse applications, including antimicrobial, UV-blocking, and catalytic properties, due to their unique structure and properties. This study focused on the characterization of zinc oxide nanoparticles (ZnO NPs) synthesized from Juglans regia leaves and their application in mitigating the impact of simultaneous infection by Meloidogyne arenaria (root-knot nematode) and Macrophomina phaseolina (root-rot fungus) in cowpea plants. The characterization of ZnO NPs was carried out through various analytical techniques, including UV–visible spectrophotometry, Powder-XRD analysis, FT-IR spectroscopy, and SEM-EDX analysis. The study confirmed the successful synthesis of ZnO NPs with a hexagonal wurtzite structure and exceptional purity. Under in vitro conditions, ZnO NPs exhibited significant nematicidal and antifungal activities. The mortality of M. arenaria juveniles increased with rising ZnO NP concentrations, and a similar trend was observed in the inhibition of M. phaseolina mycelial growth. SEM studies revealed physical damage to nematodes and structural distortions in fungal hyphae due to ZnO NP treatment. In infected cowpea plants, ZnO NPs significantly improved plant growth parameters, including plant length, fresh mass, and dry mass, especially at higher concentrations. Leghemoglobin content and the number of root nodules also increased after ZnO NP treatment. Additionally, ZnO NPs reduced gall formation and egg mass production by M. arenaria nematodes and effectively inhibited the growth of M. phaseolina in the roots. Furthermore, histochemical analyses demonstrated a reduction in oxidative stress, as indicated by decreased levels of reactive oxygen species (ROS) and lipid peroxidation in ZnO NP-treated plants. These findings highlight the potential of green-synthesized ZnO NPs as an eco-friendly and effective solution to manage disease complex in cowpea caused by simultaneous nematode and fungal infections.

Alterations in pH of Coffee Bean Extract and Properties of Chlorogenic Acid Based on the Roasting Degree.

Factors influencing the sour taste of coffee and the properties of chlorogenic acid are not yet fully understood. This study aimed to evaluate the impact of roasting degree on pH-associated changes in coffee bean extract and the thermal stability of chlorogenic acid. Coffee bean extract pH decreased up to a chromaticity value of 75 but increased with higher chromaticity values. Ultraviolet-visible spectrophotometry and structural analysis attributed this effect to chlorogenic and caffeic acids. Moreover, liquid chromatography-mass spectrometry analysis identified four chlorogenic acid types in green coffee bean extract. Chlorogenic acid isomers were eluted broadly on HPLC, and a chlorogenic acid fraction graph with two peaks, fractions 5 and 9, was obtained. Among the various fractions, the isomer in fraction 5 had significantly lower thermal stability, indicating that thermal stability differs between chlorogenic acid isomers.

Nanoflower-like cerium-doped ZnO photocatalyst deposited by spray pyrolysis for the degradation of methylene blue dye

In this study, the photodegradation of methylene blue (MB) dye and photocatalytic activities of pure ZnO and ZnO:Ce (2%, 4%, 6%, %8) films deposited with USP, an economical technique, were examined. The effect of Ce-doping on the optical, structural, surface and photocatalytic properties of the films was investigated using XRD, UV–Visible spectrophotometry, spectroscopic ellipsometry (SE), photoluminescence spectrometry, X-Ray Photoelectron Spectroscopy (XPS), field emission scanning microscope (FESEM) and atomic force microscope (AFM). In the morphology analyzes of the films, a chrysanthemum-like nanoflower structure was observed as a result of Ce-doping. Photoluminescence spectra were taken in order to determine the trap levels formed in the structure of ZnO:Ce films to be used in photocatalytic applications. Consequently, the photocatalytic properties of ZnO:Ce films were found to vary significantly depending on the surface morphology of the photocatalyst and surface defects (zinc interstitial, oxygen vacancies).

The complexation color development—visible spectrophotometry method for rapid determination of Ca2+ concentration in mine wastewater and its mechanism

Ca2+ is an important cation in coagulants used in the treatment of mine wastewater such as coal slime water, and its concentration directly affects the settling and flotation of coal slime water. The rapid determination of Ca2+ concentration is of great significance to guiding industrial production. Herein, the complexation color development—visible spectrophotometry (CCDVS) method was proposed to obtain the concentration information of Ca2+, wherein 1-(1-Hydroxy-4-methyl-2-phenylazo)-2-naphthol-4-sulfonic acid (Calmagite) was used as an indicator and the mechanism of complexation between the indicator and Ca2+ was explored. The strong correlation between spectral data and Ca2+ concentration (R2 = 0.997) indicated that this method could be used for Ca2+ detection, thereby a quantitative model was proposed to predict Ca2+ concentration by using the complexation color development—visible light absorption data. The chemical element and bonding analysis confirmed that Ca2+ was complexed with the sulfonic acid group on the indicator skeleton in the form of Ca(OH)+ intermediate in an alkaline environment. The generated complexation product (-S-O-Ca(OH)+) could stably absorb 620 nm light energy, and its absorption performance remained 99.8% after standing for 60 min. The relative standard deviation of the detection results of Ca2+ in different calcium source solutions was as low as 1.24%, which confirmed the strong calcium source compatibility of the proposed method. More importantly, the successful application of this method in the determination of Ca2+ concentration at different points in industrial coal slime water system proved its advantages of high accuracy (relative error is as low as 5.01%), low cost and simple operation. The LOD of this method is 0.038 mg/L. Therefore, the complexation color development—visible spectrophotometry method can maximize the potential for cost reduction and efficiency improvement in mine wastewater treatment.

Fagonia arabica extract-stabilized gold nanoparticles as a highly selective colorimetric nanoprobe for Cd2+ detection and as a potential photocatalytic and antibacterial agent

In the current study, polar leaves extract of the plant Fagonia arabica (FALE) from the Zygophyllaceae family was used to synthesize sunlight-assisted gold nanoparticles (FALE@AuNPs) with defined size and shape and of excellent colloidal stability. The effect of different physiochemical parameters (FALE dosage, Au3+ ions concentration, sunlight exposure time) on the formation of AuNPs was also studied. The synthesized FALE@AuNPs were characterized using UV–visible spectrophotometry, scanning electron microscopy-energy dispersive X-rays (SEM-EDX), Fourier-transform infrared spectroscopy (FTIR), powder XRD, zeta potential (ZP) and dynamic light scattering (DLS). The successful synthesis of FALE@AuNPs in solution was confirmed by the appearance of a localized surface plasmon resonance (LSPR) characteristic peak at 535 nm in UV–Vis spectra. The size estimated by UV–Vis (∼59 nm) was found in good agreement with that determined by SEM (∼60 nm) and DLS (∼61 nm). A zeta potential value of -28±1.5 mV confirms the colloidal stability of FALE@AuNPs. The FALE@AuNPs were utilized as a colorimetric nano-sensor for Cd2+ ion 15 nM limit of detection (LOD) and linear range detection of 0–600 nM. When utilized to identify Cd2+ ion in actual water samples, the nano-probe demonstrated high recovery rates of over 98 % and a low relative standard deviation (RSD) of about 4 %, demonstrating its dependability and efficiency in doing so. FALE@AuNPs were found to be antibacterial against gram-positive as well as gram-negative bacteria. An exceptionally high photocatalytic activity was shown by FALE@AuNPs with 80 % efficiency of degradation examined against methylene blue and methyl orange dye.

Hibiscus sabdariffa assisted green fabrication of reduced graphene oxide and its application for methyl orange removal: Optimization employing response surface methodology

Eco-friendly fabrication of reduced graphene oxide (rGO) is of paramount importance among various carbon nanostructures. In the current research, sustainable preparation of rGO via aqueous extract of Hibiscus sabdariffa L. calyces as the green reducer of graphene oxide (GO) without utilizing hazardous chemical agents was described. The structural characteristics of the GO and rGO were studied utilizing Fourier transform infrared (FT-IR) spectroscopy, UV–Visible spectrophotometry, X-ray diffraction (XRD), and scanning electron microscopy (SEM). The prepared nanostructure was applied as the potential adsorbent for effective methyl orange (MO) decolorization and degradation in aqueous solution. The effect of numerous independent parameters on the decolorization process involving rGO dosage, H2O2 volume, process time, and temperature were assessed and optimized via Box-Behnken design/response surface methodology BBD/RSM). A second-order model was proved to express the decolorization efficiency (D %) responses with high values of R2 and adjusted R2. Under optimal condition, the decolorization rate of MO using rGO was higher than 99 % in contact time of 31 min. The reusability of rGO for the MO removal manifested good efficiency in up to five cycles of recyclability. The findings of this research illustrate the feasibility of Hs based rGO as a suitable adsorbent for effective decolorization of MO dye from aqueous medium.

Hydrophobic deep eutectic solvent-based vortex-assisted dispersive liquid–liquid microextraction with UV–visible spectrophotometry for copper determination in waste printed circuit boards

ABSTRACT Nearly all electronic devices utilise Printed Circuit Boards (PCBs), which contribute significantly to the generation of electronic waste (e-waste). They are rich in metal content, with copper being present in higher percentages. In this work, a simple, efficient and environment-friendly pre-concentration technique was developed, using hydrophobic deep eutectic solvent as an extractant in vortex-assisted dispersive liquid–liquid microextraction. This pre-concentration technique is coupled with spectrophotometry for the determination of copper in PCBs. The complexing agent, sodium diethyl di-thiocarbamate (DDTC), and copper formed a complex in the 2–3 pH range. The Cu-DDTC complex was vortexed for 1 min at 2800 rpm to extract in hydrophobic DES. The sediment was analysed using a UV–Visible spectrophotometer at λ max 435 nm. The optimisation parameters, including pH, extraction solvent selection and its volume, concentration and volume of chelating agent, interference of forein ios, etc., have been assessed. Analytical figures of merit such as limit of detection (1.98 μg/L), limit of quantification (5.9 μg/L), relative standard deviation (3.4%) and enrichment factor (10) have been obtained under optimal experimental conditions. The method was validated by a certified copper solution and applied successfully to determine copper in waste PCBs of personal computers.

Phytomediated zinc oxide and sulfur nanoparticles for management of soft-rot causing pathogenic fungi in ginger

Diseases management has been the greatest challenge to agriculture leading to huge crop failure, represented in low-profit production. Phytopathogenic fungi are among pathogens causing a variety of agricultural diseases. Various nanoparticles (NPs) have previously been employed to combat phytopathogenic fungi. Post-harvest deterioration due to fungal invasion is the most imperative cause of loss of ginger (Zingiber officinale) production. In the present study, four fungal pathogens isolated from soft-rot infected ginger were identified as Pythium spp. (isolate I and II), one Fusarium sp. (isolate III) and one Aspergillus sp. (isolate IV). Moringa oleifera mediated zinc oxide (ZnONPs) and sulfur nanoparticles (SNPs) were characterized by UV–Visible spectrophotometry and showed absorption maxima at 356 nm and 295 nm. Average size of NPs under Nanoparticle Tracking Analyzer was 78 nm and 26 nm respectively, confirmed by FESEM. Stable NPs with zeta potential of −14.1 mV (Standard deviation = 4.51 mV) and −21.1 mV (Standard deviation = 9.56 mV) were synthesized. FTIR detected the presence of various functional groups in NPs. In vitro antifungal activity was assessed by Kirby-Bauer disc diffusion assay and MIC values compared to antibiotic ketoconazole and fungicide mancozeb. Time kill assay represented the minimum time required by selected NPs to inhibit the growth of test pathogenic fungi. ZnONPs and SNPs can be used for further antifungal studies in the field as novel nanofungicides. Extrapolated and uncontrolled use can lead to the inhibition of germination, reduction in photosynthesis rate, and disruption of the plant roots. Thorough small-scale experimentation is necessary before commercialization.

Laser flash technique as an efficacious assessment approach for thermal conductivity of tungsten disulphide nanofluids

Two-dimensional tungsten disulphide (WS2) dispersed oil-based nanofluids are prepared by a two-step process and their stability and thermal properties are assessed. UV–visible spectrophotometry reveals marginal loss in relative absorbance over 15 days ensuring dispersion stability of the nano-additives. Thermal diffusivity of nanofluids is measured using the laser flash analyzer while specific heat capacity is studied by differential scanning calorimetry. The thermal diffusivity coupled with the specific heat capacity of the nanofluids provides an estimate of the thermal conductivity of the prepared nanofluids. Specific heat of the nanofluids is observed to increase with temperature and reduce with an increase in the concentration of the nano-additives. A statistical model is developed to predict the influence of density and temperature on the specific heat of the nanofluids. Higher thermal conductivity in comparison to the base fluid is observed which further enhances with an increment in concentration of the nano-additive. The parameters such as concentration of dispersoid and temperature reveal the effect on the thermal conductivity at elevated temperatures. Enhancement in thermal conductivity is observed between 3–12 % which is validated with an analytical model for thermal conductivity of composite nanofluids.

Spectroscopic monitoring of polyurethane-based nanocomposite as a potential catalyst for the reduction of dyes

In this study, AgNPs-loaded polyurethane-sodium alginate (PU-S/Alg) composite polymers were prepared by precipitation polymerization and in-situ reduction method. Their catalytic potential was evaluated for the reduction of methyl orange (MO), brilliant blue (BB), Rhodamine B (RhB), 4-nitroaniline (4-NA), and 4-nitrophenol (4-NP). Successful preparation of samples was confirmed by UV–Visible spectrophotometry (UV–Visible), Fourier transform infrared (FTIR), and Scanning electron microscopy (SEM) analysis. During the catalytic study, the value of kapp for the reduction of MO in the presence of NaBH4 and catalyst was found 0.488 min−1 while, in the presence of NaBH4 and catalyst alone, were found as 0.9 × 10-4 and 0.8 × 10-5 min−1, respectively which indicates the role of catalyst in making the reaction speedy. The value of kapp for the reduction of BB, RhB, 4-NA, and 4-NP was found as 0.764, 0.475, 0.212 and 0.757 min−1, respectively. Simultaneous reduction of dyes induced a decreased reaction completion time under the same reaction conditions. A slight increase in the value of kapp for the catalytic reduction of MO was also observed when reactions were performed in the presence of ionic media of different salts such as NaCl, KCl, CaCl2, and MnCl2. The rate of reduction of MO was increased with the increase in ionic strength of the medium. However, the presence of SDS (surfactant) in the reaction mixture induced the decreased activity of the catalyst and increased reaction completion time. The same value of kapp for the reduction of MO was observed in the case of freshly prepared and several days old nanocomposite catalyst. These results illustrate the stability and maintained catalytic potential of metal NPs for a prolonged time. Our reported catalyst also showed good potential for the treatment of dyes-polluted textile industry wastewater.

Emission reduction effect of eco-friendly asphalt modified with isocyanate-nanoclay composites

The environmental and health issues associated with the generation of fumes during hot mix asphalt used in road construction necessitate the exploration of cleaner production methods. This study investigated the viability of utilizing isocyanate-nanoclay composites as modifiers for eco-friendly modified asphalt. The composite modified asphalt samples were prepared by adding isocyanate (isophorone diisocyanate, IPDI) and nanoclay (organic montmorillonite, OMMT or attapulgite, ATT) to the base asphalt at varying contents. A device for generating and collecting asphalt fumes was developed. The impact of modifier dosage on fume emission reduction was assessed quantitatively and qualitatively using ultraviolet–visible spectrophotometry and gas chromatography-mass spectrometry, yielding the optimal ratio of composite modifiers. The fume emission reduction mechanism of the modifiers was elucidated by analyzing changes in distribution, functional group composition and micromolecular spacing of asphalt using fluorescence microscopy, fourier-transform infrared reflection, and X-ray diffraction. Results revealed that the intercalation effect between nanoclay and asphalt, combined with chemical reactions between isocyanates and functional groups of nanoclay/asphalt components, effectively impeded the escape of fume molecules. Modified asphalt with 3% ATT+3% IPDI achieved an impressive fume emission reduction rate of 44.67% and enhanced basic performance of base asphalt. The findings contribute to the development of cleaner production methods for hot mix asphalt, thus paving the way for sustainable and safer construction practices in the future.

Hydrothermal synthesis of kesterite CZTSSe nanoparticles for highly efficient thin film

CZTSSe kesterite nanoparticles have been investigated for the efficient. The hydrothermal method has been used to prepare the material. The various characterization like X-ray diffraction (XRD), Raman scattering, Scanning Electron Microscopy (SEM) for (UV–Vis) ultraviolet–visible spectrophotometry and (EDS) energy-dispersive X-ray spectroscopy and of the prepared nano particles have been studied. Furthermore, numerical analysis of the synthesized material has also been investigated to optimize the performance for more characterization at the device level. For the optimization purpose, we have modelled a device structure of the hybrid buffer layer and optimized its physical parameters for the efficient. Theoretical efficiency is found to be 18.46 % for the prepared model. The results of this study show that Cu2ZnSn (S, Se)4 could be used as an absorbent layer for efficient solar cell.

Physicochemical and biological characterization of propolis-loaded composite polyamide-6/soybean protein nanofibers for wound healing applications

Dressings are pivotal in aiding wound recovery, yet they are burdened by significant constraints. In addition to possessing antibacterial properties, the effectiveness of a wound dressing must be rigorously assessed for its potential utility across diverse medical applications. Propolis (Pro) is widely acknowledged for its antioxidant, antibacterial, and anti-inflammatory properties, positioning it as a promising candidate for wound healing and tissue engineering applications. This study presents a novel composite nanofiber (NF) material comprising polyamide-6 (PA6) and soybean protein as matrix components, incorporating Pro as a payload. We aimed to mimic the extracellular matrix, thus promotion the proliferation and adhesion of mouse embryonic fibroblast cells (NIH3T3) on the scaffold's surface. The morphology and composition of the NFs, examined through scanning electron microscopy (SEM) imaging and Fourier-transform infrared (FTIR) spectroscopy. The Pro-loaded fibers exhibited diameters ranging from 102 to 270 nm. Notably, the NFs demonstrated a dose-dependent increase in porosity, water vapor transmission rate, and fluid uptake capacity. However, the hydrophilic categorized nanofibers (NFs) did not exhibit a concentration-dependent effect on contact angle measurements. After a 15-day period, the Pro-loaded fibers experienced degradation within the range of 39–53 %. Using UV–visible spectrophotometry, the amount of pro released was measured. The rates of release were found to be 29.93 %, 41.02 %, and 60.06 % within 24 h for PA6/Soy/Pro5 %, PA6/Soy/Pro10 %, and PA6/Soy/Pro20 % NFs, respectively. Importantly, our study showcased the significant inhibitory effects of Pro-loaded fibers on the growth of E. coli and S. aureus, with inhibition increasing proportionally with higher Pro concentrations. This observation underscores the potential of Pro-based composite NFs as effective antimicrobial agents for wound dressings and tissue scaffolds. Furthermore, the biocompatibility of the fabricated nanofibrous mats was confirmed through the MTT test, affirming the non-toxic nature of all formulations. SEM imaging further demonstrated the optimal adhesion of cells on the NFs, confirming the findings of the MTT test and highlighting the suitability of Pro-loaded NFs for cell attachment and proliferation.

Exploration of the photothermal role of curcumin-loaded targeted carbon nanotubes as a potential therapy for melanoma cancer

In this research, the hydrophilic structure of multi-walled carbon nanotubes (MWCNTs) was modified by synthesizing polycitric acid (PCA) and attaching folic acid (FA) to create MWCNT–PCA–FA. This modified nanocomplex was utilized as a carrier for the lipophilic compound curcumin (Cur). Characterization techniques including TGA, TEM, and UV–visible spectrophotometry were used to analyze the nanocomplex. The mechanism of cancer cell death induced by MWCNT–PCA–FA was studied extensively using the MTT assay, colony formation analysis, cell cycle assessment via flow cytometry, and apoptosis studies. Furthermore, we assessed the antitumor efficacy of these targeted nanocomplexes following exposure to laser radiation. The results showed that the nanocomposites and free Cur had significant toxicity on melanoma cancer cells (B16F10 cells) while having minimal impact on normal cells (NHDF cells). This selectivity for cancerous cells demonstrates the potential of these compounds as therapeutic agents. Furthermore, MWCNT–PCA–FA/Cur showed superior cytotoxicity compared to free Cur alone. Colony formation studies confirmed these results. The researchers found that MWCNT–FA–PCA/Cur effectively induced programmed cell death. In photothermal analysis, MWCNT–PCA–FA/Cur combined with laser treatment achieved the highest mortality rate. These promising results suggest that this multifunctional therapeutic nanoplatform holds the potential for combination cancer therapies that utilize various established therapeutic methods.

Photocatalytic activity of rare earth elements (Gd and ce) co-doped ZnO nanostructured films

Organic dyes, which are one of the main sources of surface and groundwater pollution, cause health problems as well as environmental hazards. For this reason, ZnO, which stands out among the promising semiconductor photocatalysts in wastewater treatment due to its advantages, was preferred. In particular, Gd–Ce co-doped ZnO nanostructured films, which have been studied for the first time in the literature, were produced by ultrasonic spray pyrolysis (USP) technique and photocatalytic degradation of Methylene blue (MB) dye was carried out. Ultraviolet–Visible Spectrophotometry (UV–Vis) and Field Emission Scanning Electron Microscopy (FESEM) were used to obtain the transmittance and morphology of thin films. According to the FESEM analysis results, morphological changes in the type of nanostructure were observed after the doping. While the photocatalytic degradation percentage of the ZnO film with Gd doping was 65.84 %, when both Gd and Ce were doped, the degradation percentage increased significantly, reaching 91.58 %. Photocatalytic studies revealed that Gd–Ce co-doped ZnO films exhibited better photocatalytic efficiency compared to only Gd doped ZnO films. Therefore, when all the results are evaluated, it is concluded that ZnO:Gd:Ce photocatalysts may have a significant potential application in environmental remediation.

Physicochemical characterization of the fraction components of the theabrownin isolates from Pu'er tea

This study focuses on the isolation of theabrownins (TBs) from Pu'er tea. This isolation process involves low temperature water extraction, membrane separation, and multi-stage extraction with organic solvents. Subsequently, purification was performed using column chromatography with macroporous adsorbent resin D-101 and ethanol aqueous solution with a concentration of 0–64.81 g/100g. Five purified fractions were obtained, namely TBs-D1, TBs-D2, TBs-D3, TBs-D4, and TBs-D5, collectively referred to as TBs-D(1–5). These fractions were found to contain TBs and polysaccharides but lacked catechins, caffeine, theaflavin, and free protein. The average molecular weights of these fraction components exceeded 104 Da. These results indicated that TBs-D(1–5) were not free, but combined with tea polysaccharide conjugates (TPC), that is, TBs-TPC complexes. Furthermore, ultraviolet–visible spectrophotometry and Flourier transformation infrared spectroscopy confirmed the nature of TBs-D(1–5) as TBs-TPC complexes. Fluorescence spectra revealed that polysaccharides exert a quenching effect on the intrinsic fluorescence of TBs. Atomic force microscopy indicated that the sample forms a spherical cluster due to the aggregation of theabrownin molecules. Additionally, measurements of interfacial tension and water contact angle demonstrated that TBs-D(1–5) exhibit some amphiphilic properties. This research provides a theoretical foundation for the industrial production and utilization of TBs.

Dye-assisted analysis of fluoride in water using UV–visible spectrophotometry: a preliminary study

ABSTRACT Dye-assisted method for the analysis of fluoride content of water has been developed in this study using dyes obtained from some flowering plants. This was done to evaluate the potentials of locally accessible dyes in spectrophotometrically detecting F– levels in fluoride-containing water samples. Dye solutions obtained from scarlet jungle flame, Hibiscus flower, Peacock flower or Barbados pride, Royal poinciana, Pink bauhinia, Barbados lily, or Easter lily were adopted to monitor absorbance and corresponding concentrations of serially prepared F− concentrations in a range of 0.001–0.012 ppm. Dye from the Hibiscus flower gave an optimal performance with R2 = 0.9792. Using this dye, the F– content in water samples obtained from tap waters from Moremi Estate, Modomo, Asherifa, Postgraduate Hall of Obafemi Awolowo University, Ile-Ife, and a well water sample from Modomo gave 0.052, 0.053, 0.053, 0.058, and 0.061 ppm, respectively. A comparison of these values indicated that all the water samples monitored were safe for human consumption without experiencing health challenges as the maximum F– limit for potable water recommended by WHO was not exceeded. This study concluded that dye from Hibiscus flower could satisfactorily assist in monitoring F– content in water where ion-selective electrodes are not readily accessible.

Preparation and Performance Study of HTPB-g-(PNIPAM/PEG) Thermoresponsive Polymer Brush.

In recent years, a great deal of work has been devoted to the development of thermoresponsive polymers that can be made into new types of smart materials. In this paper, a branched polymer, HTPB-g-(PNIPAM/PEG), with polyolefin chain segments as the backbone and having polyethylene glycol (PEG) and poly(N-isopropylacrylamide) (PNIPAM) as side chains was synthesized by ATRP and click reactions using N3-HTPB-Br as the macroinitiator. This initiator was designed and synthesized using hydroxyl-terminated polybutadiene (HTPB) as the substrate. The temperature-responsive behavior of the branched polymer was investigated. The lower critical solution temperature (LCST) of the branched polymer was determined by ultraviolet and visible spectrophotometry (UV-vis) and was found to be 35.2 °C. The relationship between the diameter size of micelles and temperature was determined by dynamic light scattering (DLS). It was found that the diameter size changed at 36 °C, which was nearly consistent with the result obtained by UV-vis. The results of the study indicate that HTPB-g-(PNIPAM/PEG) is a temperature-responsive polymer. At room temperature, the polymer can self-assemble into composite micelles, with the main chain as the core and the branched chain as the shell. When the temperature was increased beyond LCST, the polyolefin main chain along with the PNIPAM branched chain assembled to form the nucleus, and the PEG branched chain constituted the shell.

Ultrasonic-Assisted Electrodeposition of Mn-Doped NiCo2O4 for Enhanced Photodegradation of Methyl Red, Hydrogen Production, and Supercapacitor Applications

This paper presents a novel ultrasonic-assisted electrodeposition process of Mn-doped NiCo2O4 onto a commercial nickel foam in a neutral electroplating bath (pH = 7.0) under an ultrasonic power of 1.2 V and 100 W. Different sample properties were studied based on their crystallinity through X-ray diffraction (XRD), morphology was studied through scanning electron microscopy (SEM), and photodegradation was studied through ultraviolet–visible (UV–Vis) spectrophotometry. Based on the XRD results, the dominant crystallite phase obtained was shown to be a pure single NiCo2O4 phase. The optical properties of the photocatalytic film showed a range of energy band gaps between 1.72 and 1.73 eV from the absorption spectrum. The surface hydroxyl groups on the catalytic surface of the Mn-doped NiCo2O4 thin films showed significant improvements in removing methyl red via photodegradation, achieving 88% degradation in 60 min, which was approximately 1.6 times higher than that of pure NiCo2O4 thin films. The maximum hydrogen rate of the composite films under 100 mW/cm2 illumination was 38 μmol/cm2 with a +3.5 V external potential. The electrochemical performance test also showed a high capacity retention rate (96% after 5000 charge–discharge cycles), high capacity (260 Fg−1), and low intrinsic resistance (0.8 Ω). This work concludes that the Mn-doped NiCo2O4 hybrid with oxygen-poor conditions (oxygen vacancies) is a promising composite electrode candidate for methyl red removal, hydrogen evolution, and high-performance hybrid supercapacitor applications.

Covalent vs. Non covalent chemical modification of multiwalled carbon nanotubes based-nanofluids: Stability and thermal conductivity steadiness over temperature

Thermal conductivity enhancement coupled to nanoparticle dispersion stability over time are the two main conflicting requirements to overcome to develop carbon nanomaterial-based nanofluids. Both covalent and non-covalent approaches, having their own advantages and disadvantages, are commonly used for carbon nanotube based nanofluids development. However, they are rarely compared regarding their impact on stability and thermal conductivity performances for the same kind of nanofluid. In this work, multiwalled carbon nanotubes have been chemically modified by both covalent and non-covalent functionalization. For the covalent functionalization, a simple oxidation method is applied. It consists of refluxing the powdered MWCNTs in H2SO4/HNO3 at 5 M concentration. For the non-covalent approach, both an anionic (sodium dodecyl sulfate) and a non-ionic (Pluronic P123, comprising poly(ethylene oxide) (PEO) and poly(propylene oxide) (PPO) in an alternating linear fashion, PEO-PPO-PEO) surfactants were employed at a concentration of 1 wt%. Nanofluids were prepared with multiwalled carbon nanotubes at a fixed concentration of 0.2 wt% for both chemical modification approaches. The oxidation reaction occurs without significant structure damaging as shown by transmission electron microscopy, Raman spectroscopy, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. UV–visible spectrophotometry analysis shows a remarkable stability with temperature in the 293.15–303.15 K range over one-week and for a longer period of 49 days for all the three types of nanofluids. Their thermal conductivity has been investigated in the same temperature range. For all the three nanofluid series prepared with a fixed concentration of carbon nanomaterials, a thermal conductivity enhancement compared to that of the base fluid has been observed. The thermal conductivity evolution with temperature is different for each type of nanofluid. The covalently oxidized multiwalled carbon nanotube based nanofluids showed the better thermal conductivity enhancement steadiness (around 7 %) with temperature. The discussion on the surfactant-based nanofluid behavior proposes the possible involved mechanisms as temperature increases for each surfactant.