Sonochemical synthesis of graphitic carbon nitrides‐wrapped bimetal oxide nanoparticles hybrid materials and their electrocatalytic activity for xanthine electro-oxidation

A novel network-like magnetic nanoparticle was fabricated on a graphitic carbon nitride through a facile sonochemical route at frequency 20 kHz and power 70 W. To enhance the electrocatalytic activity of the modified materials, the graphitic carbon nitrides (g-C₃N₄) was prepared from melamine. Monitoring of xanthine concentration level in biological fluids is more important for clinical diagnosis and medical applications. As modified CuFe₂O₄/g-C₃N₄ nanocomposite exhibits better electrochemical activity towards the oxidation of xanthine with higher anodic current compared to other modified and unmodified electrode for the detection of xanthine with larger linear range (0.03–695 µM) and lower limit of detection (13.2 nM). To compare with these methods, the electrochemical techniques may be an alternative high sensitive method due to their simplicity and rapid detection time. In addition, the practical feasibility of the sensor was inspected with biological samples, reveals the acceptable recovery of the sensor in real samples.     

Ultrasonic irradiation preparation of graphitic-C3N4/polyaniline nanocomposites as counter electrodes for dye-sensitized solar cells

In this research, polyaniline/graphitic carbon nitride (PANI/g-C₃N₄) nanocomposites were synthesized via in-situ electrochemical polymerization of aniline monomer whit different number of cyclic voltammetry scans (10, 20 and 30 cycles) after electrode surface pre-preparation using a potential shock under ultrasonic irradiation. PANI/g-C₃N₄ nanocomposites with two values of g-C₃N₄ (0.010 wt% and 0.015 wt%) were deposited on the surface of the transparent conducting film (FTO glass) by immersing FTO into the aniline solution and g-C₃N₄ during the electro-polymerization. The resulting PANI/g-C₃N₄ films were characterized by Fourier transformed infra-red (FTIR), power X-ray diffraction (PXRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) techniques. The prepared electrodes were applied as counter electrode in dye-sensitized solar cells. Among them, the prepared electrode with 10 cycles and 0.01 wt% g-C₃N₄ showed the best efficiency. These hybrids show good catalytic activity in elevating tri-iodide reduction and due to the synergistic effect of PANI and g-C₃N₄, PANI/g-C₃N₄ nanocomposite electrode shows power conversion efficiency about 1.8%.     

Facile synthesis of copper ferrite nanoparticles with chitosan composite for high-performance electrochemical sensor

Herein, the synthesis of copper ferrite nanoparticles (CuFe₂O₄ NPs)/chitosan have been prepared by sonochemical route under ultrasonic irradiation bath at 40 kHz and 50 W. A high sensitive and stable modified electrochemical sensor was developed using a composition of copper ferrite nanoparticles coordinated with biopolymer through a facile ultrasound approach. Besides, power and frequency parameters are highly important for sonochemical synthesis and specifically structure, and size of the nanomaterials development during the ultrasonic irradiation time. In this work, ultrasonic bath was used to synthesis of CuFe₂O₄ nanomaterial at 40 kHz with 1 h. CuFe₂O₄/chitosan was characterized by FESEM, EDX, XRD and electrochemical methods. Furthermore, 8-hydroxyguanine is one of biomarker by oxidative stress. The concentrations of 8-hydroxyguanine within a cell are a measurement of oxidative stress in human body. Consequently, the measurement of 8-hydroxyguanine in blood serum samples with high specificity is of greatest importance. The CuFe₂O₄/chitosan modified electrode is displayed a low detection limit of 8.6 nM and long linear range (0.025–697.175 µM).     

g-C3N4 modified Bi2O3 composites with enhanced visible-light photocatalytic activity

Novel g-C₃N₄ modified Bi₂O₃ (g-C₃N₄/Bi₂O₃) composites were synthesized by a mixing-calcination method. The samples were characterized by thermogravimetry (TG), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), UV–vis diffuse reflection spectroscopy (DRS), photoluminescence (PL) and photocurrent-time measurement (PT). The photocatalytic activity of the composites was evaluated by degradation of Rhodamine B (RHB) and 4-chlorophenol (4-CP) under visible light irradiation (>400 nm). The results indicated that the g-C₃N₄/Bi₂O₃ composites showed higher photocatalytic activity than that of Bi₂O₃ and g-C₃N₄. The enhanced photocatalytic activity of the g-C₃N₄/Bi₂O₃ composites could be attributed to the suitable band positions between g-C₃N₄ and Bi₂O₃. This leads to a low recombination between the photogenerated electron–hole pairs. The proposed mechanism for the enhanced visible-light photocatalytic activity of g-C₃N₄/Bi₂O₃ composites was proven by PL and PT analysis.     

Sonochemical synthesis and fabrication of neodymium sesquioxide entrapped with graphene oxide based hierarchical nanocomposite for highly sensitive electrochemical sensor of anti-cancer (raloxifene) drug

The ultrasound-assisted synthesis of a novel neodymium sesquioxide nanoparticles (Nd₂O₅ NPs) decorated graphene oxide (GO) nanocomposite under ultrasonic probe (Ultrasonic processor model-PR 1000; frequency-30 kHz; power of 100 W/cm²) has been reported. After then, SEM, TEM, XRD, EDX and electrochemical impedance spectroscopy characterized was analyzed using Nd₂O₅ NPs@GO nanomaterial. Furthermore, the nanomaterial modified GCE (glassy carbon electrode) shows excellent electrochemical sensing performance towards anti-cancer drug. Raloxifene is one of the important anti-cancer drug. Moreover, the fabricated electrochemical sensor has showed a wide linear range for raloxifene between 0.03 and 472.5 µM and nanomolar detection limit (18.43 nM). In addition, the Nd₂O₅ NPs@GO modified sensor has been applied to the determination of raloxifene in human blood and urine samples.     

Sonochemical synthesis and fabrication of perovskite type calcium titanate interfacial nanostructure supported on graphene oxide sheets as a highly efficient electrocatalyst for electrochemical detection of chemotherapeutic drug

In green approaches for electrocatalyst synthesis, sonochemical methods play a powerful role in delivering the abundant surface areas and nano-crystalline properties that are advantageous to electrocatalytic detection. In this article, we proposed the sphere-like and perovskite type of bimetal oxides which are synthesized through an uncomplicated sonochemical procedure. As a yield, the novel calcium titanate (orthorhombic nature) nanoparticles (CaTiO₃ NPs) decorated graphene oxide sheets (GOS) were obtained through simple ultrasonic irradiation by a high-intensity ultrasonic probe (Titanium horn; 50 kHz and 60 W). The GOS/CaTiO₃ NC were characterized morphologically and chemically through the analytical methods (SEM, XRD, and EDS). Besides, as-prepared nanocomposites were modified on a GCE (glassy carbon electrode) and applied towards electrocatalytic and electrochemical sensing of chemotherapeutic drug flutamide (FD). Notably, FD is a crucial anticancer drug and also a non-steroidal anti-androgen chemical. Mainly, the designed and modified sensor has shown a wide linear range (0.015–1184 µM). A limit of detection was calculated as nanomolar level (5.7 nM) and sensitivity of the electrode is 1.073 μA μM⁻¹ cm⁻². The GOS/CaTiO₃ modified electrodes have been tested in human blood and urine samples towards anticancer drug detection.     

Sonocatalytic degradation of tetracycline hydrochloride with CoFe2O4/g-C3N4 composite

In this work, different mass percent ratios of CoFe₂O₄ coupled g-C₃N₄ (w%-CoFe₂O₄/g-C₃N₄, CFO/CN) nanocomposites were integrated through a hydrothermal process for the sonocatalytic eradication of tetracycline hydrochloride (TCH) from aqueous media. The prepared sonocatalysts were subjected to various techniques to investigate their morphology, crystallinity, ultrasound wave capturing activity and charge conductivity. From the investigated activity of the composite materials, it has been registered that the best sonocatalytic degradation efficiency of 26.71 % in 10 min was delivered when the amount of CoFe₂O₄ was 25% in the nanocomposite. The delivered efficiency was higher than that of bare CoFe₂O₄ and g-C₃N₄. This enriched sonocatalytic efficiency was credited to the accelerated charge transfer and separation of e⁻-h⁺ pair through the S-scheme heterojunctional interface. The trapping experiments confirmed that all the three species i.e. ^•OH, h⁺ and ^•O₂⁻ were involved in the eradication of antibiotics. A strong interaction was shown up between CoFe₂O₄ and g-C₃N₄ in the FTIR study to support charge transfer as confirmed from the photoluminescence and photocurrent analysis of the samples. This work will provide an easy approach for fabricating highly efficient low-cost magnetic sonocatalysts for the eradication of hazardous materials present in our environment.     

A feasible sonochemical approach to synthesize CuO@CeO2 nanomaterial and their enhanced non-enzymatic sensor performance towards neurotransmitter

A nanostructured and high conductive cupric oxide (CuO NPs) with hierarchical CeO₂ sheets-like structure was synthesized by a facile sonochemical approach. Furthermore, CuO/CeO₂ nanostructure is synthesized by high-intensity ultrasonic probe (Ti-horn, 50 kHz and 100 W) at ambient air. Moreover, the synthesized CuO/CeO₂ material was characterized by various analytical techniques including FESEM, EDX, XRD and electrochemical methods. Then, the synthesized CuO/CeO₂ composite was applied for the electrocatalytic detection of dopamine using CV and DPV techniques. In addition, the CuO/CeO₂ modified electrode has good electrocatalytic performance with high linear range from 0.025 to 98.5 µM towards the determination of dopamine drug and high sensitivity of the CuO/CeO₂ modified drug sensor was calculated as 16.34 nM and 4.823 μA·µM⁻¹·cm⁻², respectively. Moreover, a repeatability, reproducibility and stability of the CuO@CeO₂ mixture modified electrode were analyzed towards the determination of dopamine biomolecule. Interestingly, the real time application of CuO@CeO₂ modified electrode was established in different serum and drug samples.     

A sonochemical synthesis of SrTiO3 supported N-doped graphene oxide as a highly efficient electrocatalyst for electrochemical reduction of a chemotherapeutic drug

A sonochemical based green synthesis method playa powerful role in nanomaterials and composite development. In this work, we developed a perovskite type of strontium titanate via sonochemical process. SrTiO₃ particles were incorporated with nitrogen doped graphene oxide through simple ultrasonic irradiation method. The SrTiO₃/NGO was characterized by various analytical methods. The nanocomposite of SrTiO₃/NGO was modified with laser-induced graphene electrode (LIGE). The SrTiO₃/NGO/LIGE was applied for electrochemical sensor towards chemotherapeutic drug detection (nilutamide). Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques have been used to examine the electrochemical performance of nilutamide (anti-cancer drug). DPV was found to be more sensitive and found to exhibit a sensitivity 8.627 µA µM⁻¹ cm⁻² for SrTiO₃/NGO/LIGE with a wide linear range (0.02–892 µM) and low Limit of detection (LOD: 1.16 µM). SrTiO₃/NGO/LIGE has been examined for the detection of nilutamide in blood serum and urine samples and obtained a good recovery in the range of 97.2–99.72 %. The enhanced stability and selectivity and practical application results indicates the suitability of SrTiO₃/NGO/LIGE towards the detection of nilutamide drug in pharmaceutical industries.     

ZnFe2O4的固相法和水热法制备及其电化学性能研究

本文用固相反应法和水热法制备了ZnFe₂O₄材料,X射线衍射(X-ray diffraction, XRD)表明制备出来的ZnFe₂O₄为尖晶石结构,表面形貌测试 (scanning electron microscopy, SEM) 显示两种方法制备的材料的平均粒径分别为500 nm和200 nm.比表面积测试结果表明,两种方法制备的样品的比表面积分别为136.7 m² g^{-1关键词： 2O₄')" href="#">ZnFe₂O₄ 尖晶石结构 电化学性能 锂离子电池}     

Fabrication of g-C3N4/NiO heterostructured nanocomposite modified glassy carbon electrode for quercetin biosensor

Herein, we report a one-pot synthesis of structurally uniform and electrochemically active graphitic carbon nitride/nickel oxide (g-C₃N₄/NiO) nanocomposite and an investigation on the electrocatalytic oxidation of quercetin (QR). The synthesized g-C₃N₄/NiO nanocomposite has uniform surface distribution, which was characterized with scanning electron microscopy (SEM). Moreover, the composition of synthesized g-C₃N₄/NiO nanocomposite was characterized by UV–vis-spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR spectra), BET, SEM and HRTEM. The g-C₃N₄/NiO was electrochemically treated in 0.1 MPBS solution through cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The peak current response increases linearly with QR concentration from 0.010 μM to 250 µM with a fast response time of less than 2 s and a detection limit of 0.002 μM. To further evaluate the feasibility of using this sensor for real sample analysis, QR content in various real samples including green tea, green apple, honey suckle were determined and satisfactory results were achieved.     

Modified g-C3N4/TiO2 nanosheets/ZnO ternary facet coupled heterojunction for photocatalytic degradation of p-toluenesulfonic acid (p-TSA) under visible light

Novel ternary nanocomposites with facet coupled structure were synthesized by using modified g-C₃N₄, TiO₂ nanosheets and nano-ZnO. Nanosheet/nanosheet heterojunction structure was investigated by TEM, XPS and XRD. FT–IR and Nitrogen adsorption were illustrated for chemical/physical structure analyses. Solution of p-Toluenesulfonic acid (p-TSA) was chosen as target pollutant for visible light photodegradation and the excellent removal efficiency was achieved by this structurally modified g-C₃N₄/TiO₂/ZnO hybrid. The visible light absorption improvement and quantum efficiency enhancement, which were testified by UV–vis DRS, PL and p-TSA photodegradation measurements, due to the facet coupled structure and appropriate quantity of modified g-C₃N₄ in the nanocomposites.     

Mechanistic investigations on emission characteristics from g-C3N4, g-C3N4@Pt and g-C3N4@Ag nanostructures using X-ray absorption spectroscopy

An improved method for the preparation of g-C₃N₄ is described. Currently, heating (>400 C°) of urea is the common method used for preparing the g-C₃N₄. We have found that sonication of melamine in HNO₃ solution, followed by washing with anhydrous ethanol, not only reduce the crystallite size of g-C₃N₄ but also facilitate intriguing electronic structure and photoluminescence (PL) properties. Moreover, loading of metal (Pt and Ag) nanoparticles, by applying the borohydride reduction method, has resulted in multicolor-emission from g-C₃N₄. With the help of PL spectra and local electronic structure study, at C K-edge, N K-edge, Pt L-edge and Ag K-edge by X-ray absorption spectroscopy (XAS), a precise mechanism of tunable luminescence is established. The PL mechanism ascribes the amendments in the transitions, via defect and/or metal states assimilation, between the π* states of tris-triazine ring of g-C₃N₄ and lone pair states of nitride. It is evidenced that interaction between the C/N 2p and metal 4d/5d orbitals of Ag/Pt has manifested a net detraction in the δ*→LP transitions and enhancement in the π*→LP and π*→ π transitions, leading to broad PL spectra from g-C₃N₄ organic semiconductor compound.     

Ultrasound wave assisted removal of Ceftriaxone sodium in aqueous media with novel nano composite g-C3N4/MWCNT/Bi2WO6 based on CCD-RSM model

The aim of this study was ultrasound assisted removal of Ceftriaxone sodium (CS) based on CCD model. Using sonochemical synthesized Bi₂WO₆ implanted on graphitic carbon nitride/Multiwall carbon nanotube (g-C₃N₄/MWCNT/Bi₂WO₆). For this purpose g-C₃N₄/MWCNT/Bi₂WO₆ was synthesized and characterized using diverse approaches including XRD, FE-SEM, XPS, EDS, HRTEM, FT-IR. Then, the contribution of conventional variables including pH, CS concentration, adsorbent dosage and ultrasound contact time were studied by central composite design (CCD) under response surface methodology (RSM). ANOVA was employed to the variable factors, and the most desirable operational conditions mass provided. Drug adsorption yield of 98.85% obtained under these defined conditions. Through conducting five experiments, the proper prediction of the optimum point were examined. The respective results showed that RSD% was lower than 5% while the t-test confirmed the high quality of fitting. Langmuir isotherm equation fits the experimental data best and the removal followed pseudo-second order kinetics. The estimation of the experimentally obtained maximum adsorption capacities was 19.57 mg.g⁻ of g-C₃N₄/MWCNT/Bi₂WO₆ for CS. Boundary layer diffusion explained the mechanism of removal via intraparticle diffusion.     

Preparation and characterisation of ZnFe2O4/ZnO polymer nanocomposite sensors for the detection of alcohol vapours

During the last 10 years, a large interest has developed in the preparation of nanocomposite structures by embedding inorganic nanoparticles into polymeric materials. These materials combine the properties of the inorganic fillers with the processability and flexibility of polymers. The versatility of polymer nanocomposite systems is of special interest to the gas sensor industry where arrays of polymer/carbon black composites have been used to identify gases and odours. These polymer gas sensors provide selectivity based on their chemical structures and operate at room temperature, which provide advantages over thick-film metal oxide gas sensors. ZnFe₂O₄ and ZnO have excellent stability, high sensitivity, low fabrication complexity and moderate operating temperatures, which are ideal properties for a gas sensing material. In this work, the development of a thick-film ZnFe₂O₄/ZnO sensor, which operates at room temperature and a drop-coated conducting polymer composite sensor containing 30 w/w% ZnFe₂O₄/ZnO nanoparticles is discussed. The sensors were tested in a fully automated test rig and showed promising results for the detection of alcohol vapours.     

Ultrasound-assisted synthesis of 3D flower-like zinc oxide decorated fMWCNTs for sensitive detection of toxic environmental pollutant 4-nitrophenol

Sonochemical synthesis of functionalized multi-walled carbon nanotubes (fMWCNTs) embellished 3D flower-like zinc oxide (ZnO) nanocomposite based novel electrochemical sensor for the detection of toxic environmental pollutant 4-nitrophenol (4-NP) is detailed in this paper. We have used laser-assisted synthesis technique in the development of 3D flower-like ZnO nanoparticles (NPs) and ultrasonication method was employed in preparation of ZnO NPs@fMWCNTs nanocomposite using a high-intensity ultrasonic bath DC200H with power of 200 W/cm² and 40 KHz frequency. The nanocomposite was meticulously fabricated on screen printed carbon electrode (SPCE) to carry out various electrochemical analysis. Different characterizations such as Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, UV visible spectroscopy (UV–Vis), X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM) of the materials used in this work were taken. Cyclic voltammetry (CV) and differential pulse voltammetry (DPV) techniques are used in electrochemical investigations. We have observed well-defined oxidation and reduction peak currents representing electrochemical mechanism of 4-NP at very low potentials for ZnO NPs@fMWCNTs/SPCE. Furthermore, we were able to achieve efficient electrochemical determination of 4-NP using the developed sensor with a high sensitivity of 11.44 μA μM⁻¹ cm⁻² and very low detection limit (LOD) of 0.013 μM in a broad linear range of 0.06–100 μM. All the significant features of a good sensor including anti-interference, good stability, excellent repeatability, and reproducibility were exhibited by the sensor. Moreover, we have tested practical feasibility of sensor by carrying out real sample analysis on different water samples.     

Mechanisms of effective gold shell on Fe3O4 core nanoparticles formation using sonochemistry method

Sonochemical synthesis (sonochemistry) is one of the most effective techniques of breaking down large clusters of nanoparticles (NPs) into smaller clusters or even individual NPs, which ensures their dispersibility (stability) in a solution over a long duration. This paper demonstrates the potential of sonochemistry becoming a valuable tool for the deposition of gold (Au) shell on iron oxide nanoparticles (Fe₃O₄ NPs) by explaining the underlying complex processes that control the deposition mechanism. This review summarizes the principles of the sonochemistry method and highlights the resulting phenomenon of acoustic cavitation and its associated physical, chemical and thermal effects. The effect of sonochemistry on the deposition of Au NPs on the Fe₃O₄ surface of various sizes is presented and discussed. A Vibra-Cell ultrasonic solid horn with tip size, frequency, power output of ½ inch, 20 kHz and 750 W respectively was used in core@shell synthesis. The sonochemical process was shown to affect the surface and structure of Fe₃O₄ NPs via acoustic cavitation, which prevents the agglomeration of clusters in a solution, resulting in a more stable dispersion. Deciphering the mechanism that governs the formation of Au shell on Fe₃O₄ core NPs has emphasized the potential of sonication in enhancing the chemical activity in solutions.     

An optimal low-temperature tartrate precursor method for the synthesis of monophasic nanosized ZnFe2O4

In this study, the synthesis of monophasic nanocrystalline zinc ferrite (ZnFe₂O₄) was achieved by controlling the thermal decomposition conditions of a zinc–iron tartrate precursor method. Differential thermal analysis/thermogravimetry (DTA/TG), X-ray diffraction (XRD), Fe²⁺ content analysis, transmission electron microscopy (TEM), and Brunauer-Emmett-Teller (BET) techniques were used to investigate the effect of heat treatment conditions on the calcined powders. The thermal decomposition of the precursor led to an intermediate phase formation of ZnO, Fe₃O₄, and γ-Fe₂O₃. It was found that the Fe₃O₄ → γ-Fe₂O₃ oxidation reaction is the key step in producing monophasic nanosized ZnFe₂O₄. The monophasic nanoparticles of ZnFe₂O₄ can be obtained when the precursor is heat treated under a low temperature (300–400 °C) and long residence time (4 h) process that can prompt the Fe₃O₄ oxidation and prevent the formation of α-Fe₂O₃.     

Magnetic properties of ZnFe2O4 nanoparticles

Fine particles of ZnFe₂O₄ were synthesized by a wet chemical method in the (80 wt.% Fe₂O₃ + 20 wt.% ZnO) system. The morphological and structural properties of the mixed system were investigated by scanning electron microscopy, X-ray diffraction, inductively coupled plasma atomic emission, and X-ray photoelectron spectroscopy. The major phase was determined to be the ZnFe₂O₄ spinel with particle size of 11 nm. The magnetic properties of the material were investigated by ferromagnetic resonance (FMR) in the temperature range from liquid helium to room temperature. A very intense, asymmetric FMR signal from ZnFe₂O₄ nanoparticles was recorded, which has been analyzed in terms of two Callen-lineshape lines. Temperature dependence of the FMR parameters was obtained from fitting the experimental lines with two component lines. Analysis of the FMR spectra in terms of two separate components indicates the presence of strongly anisotropic magnetic interactions.     

Synthesis of ZnFe2O4 nanomagnets by Fe-ion implantation into ZnO and post-annealing

Fe ions of dose 8 × 10¹⁶ cm^-2 are implanted into a ZnO single crystal at 180 keV. Annealing at 1073 K leads to the formation of zinc ferrite (ZnFe₂O₄), which is verified by synchrotron radiation X-ray diffraction (SR-XRD) and X-ray photoelectron spectroscopy (XPS). The crystallographically oriented ZnFe₂O₄ is formed inside the ZnO with the orientation relationship of ZnFe₂O₄ (111)//ZnO (0001). Superconducting quantum interference device (SQUID) measurements show that the as-implanted and post-annealing samples are both ferromagnetic at 5 K. The synthesized ZnFe₂O₄ is superparamagnetic, with a blocking temperature (T_B = 25 K), indicated by zero field cooling and field cooling (ZFC/FC) measurements.