The presence of metal with microwave irradiation has always invited controversial arguments as the metal will catch on fire easily. But interestingly, researchers found that arc discharge phenomena provide a promising way for molecule cracking to synthesize nanomaterials. This study developed a single-step yet affordable synthesis approach that combines microwave heating and arcing in transforming crude palm oil into magnetic nanocarbon (MNC), which can be considered a new alternative for the palm oil sectors. It involves synthesizing the medium at a partial inert condition with constant coiled stainless steel metal wire (dielectric media) and ferrocene (catalyst). This approach successfully demonstrates heating at a temperature ranging from 190.9 to 472.0 °C with different synthesis times (10-20 min). The produced MNC shows formations of spheres with average sizes of 20.38-31.04 nm, mesoporous structure (SBET: 14.83-151.95 m2/g), and high content of fixed carbon (52.79-71.24wt%), and the ratio of the D and G bands (ID/IG) is 0.98-0.99. The formation of new peaks in the FTIR spectra (522.29-588.48 cm-1) supports the appearance of the FeO compounds from the ferrocene. The magnetometer shows high magnetization saturation (22.32-26.84 emu/g) in ferromagnetic materials. The application of the MNC in wastewater treatment has been demonstrated by evaluating their adsorbent capability with Methylene Blue (MB) adsorption test at a different concentrations varying between 5 and 20 ppm. The MNC produced at synthesis time (20 min) shows the highest adsorption efficiency (10.36 mg/g) compared to others, with 87.79% removal of MB dye. As a result, the value for Langmuir is not promising compared to Freundlich, with R2 being around 0.80, 0.98, and 0.99 for MNC synthesized at 10 min (MNC10), 15 min (MNC15), and 20 min (MNC20), respectively. Hence, the adsorption system is in a heterogeneous condition. The microwave-assisted arcing thereby presents a promising approach to transforming CPO into MNC that could remove the hazardous dye.
The increasing demand for high-performance lithium-ion batteries (LIBs) has emphasized the need for affordable and sustainable materials, prompting the exploration of waste upcycling to address global sustainability challenges. In this study, we efficiently converted polypropylene (PP) plastic waste from used centrifuge tubes into activated polypropylene carbon (APC) using microwave-assisted pyrolysis. The synthesis of APC was optimized using response surface methodology/central composite design (RSM/CCD). Based on the RSM results, the optimal conditions for PP plastic conversion into carbon were determined as follows: HNO3 concentration of 3.5 M, microwave temperature of 230 °C, and holding time of 25 min. Under these conditions, the obtained intensity ratio of Id/Ig in PP carbon was 0.681 ± 0.013, with an error of 6.81 ± 0.013 % between predicted and actual values. The physicochemical studies, including FESEM-EDX, XRD, and Raman spectroscopy, confirmed the successful synthesis of APC samples. The APC 800 material exhibited a well-organized three-dimensional structure characterized by large pores and mesopores, enabling fast ion transport in the electrode. As a result, the APC 800 electrode demonstrated an initial discharge capacity of 381.0 mAh/g, an improved initial coulombic efficiency of 85.1%, and excellent cycling stability after 100 cycles. Notably, the APC 800 electrode displayed remarkable rate performance, showing a reversible capacity of 355.1 mAh/g when the current density was reset to 0.2 A/g, highlighting its high electrochemical reversibility. The outstanding characteristics of APC 800 as an anode electrode material for high-performance lithium-ion batteries suggest a promising future for its application in the field.
This paper provides a comprehensive analysis of the dielectric and physicochemical properties of the porous hydroxyapatite/cornstarch (HAp/Cs) composites in a new perspective. The porous composites have been characterized via SEM, FTIR, XRD and dielectric spectroscopy. The dielectric permittivity spectra were obtained in Ku-band (12.4-18.0 GHz) and it was correlated with the physicochemical properties of the porous HAp/Cs. Porous HAp/Cs composites exhibits low ε' and negative ε″, which influenced by the microstructural morphology, interaction between Hap and Cs, as well as crystalline features due to the various proportion of the HAp/Cs. The physicochemical effect of the composites results in the dielectric polarization and energy loss. This phenomenon indicates the presence of the three obvious relaxation responses in the ε' spectrum (13.2-14.0, 15.2-16.0, and 16.6-17.4 GHz) and the negative behaviours in the ε″ spectrum. The relationships between physicochemical and dielectric properties of the porous composite facilitate the development of the non-destructive microwave evaluation test for the porous composite.
The purpose of this study was to synthesize high-quality recycled α-Fe2O3 to improve its complex permittivity properties by reducing the particles to nanosize through high energy ball milling. Complex permittivity and permeability characterizations of the particles were performed using open-ended coaxial and rectangular waveguide techniques and a vector network analyzer. The attenuation characteristics of the particles were analyzed with finite element method (FEM) simulations of the transmission coefficients and electric field distributions using microstrip model geometry. All measurements and simulations were conducted in the 8-12 GHz range. The average nanoparticle sizes obtained after 8, 10 and 12 h of milling were 21.5, 18, and 16.2 nm, respectively, from an initial particle size of 1.73 µm. The real and imaginary parts of permittivity increased with reduced particle size and reached maximum values of 12.111 and 0.467 at 8 GHz, from initial values of 7.617 and 0.175, respectively, when the particle sizes were reduced from 1.73 µm to 16.2 nm. Complex permeability increased with reduced particle size while the enhanced absorption properties exhibited by the nanoparticles in the simulations confirmed their ability to attenuate microwaves in the X-band frequency range.
Recycled hematite (α-Fe2O3) nanoparticles with enhanced complex permittivity properties have been incorporated as a filler in a polycaprolactone (PCL) matrix reinforced with oil palm empty fruit bunch (OPEFB) fiber for microwave absorption applications. The complex permittivity values were improved by reducing the particle sizes to the nano scale via high-energy ball milling for 12 h. A total of 5-20 wt.% recycled α-Fe2O3/OPEFB/PCL nanocomposites were examined for their complex permittivity and microwave absorption properties via the open ended coaxial (OEC) technique and the transmission/reflection line measurement using a microstrip connected to a two-port vector network analyzer. The microstructural analysis of the samples included X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR). At 1 GHz, the real (ε') and imaginary (ε″) parts of complex permittivity of recycled α-Fe2O3 particles, respectively, increased from 7.88 to 12.75 and 0.14 to 0.40 when the particle size was reduced from 1.73 μm to 16.2 nm. A minimum reflection loss of -24.2 dB was achieved by the 20 wt.% nanocomposite at 2.4 GHz. Recycled α-Fe2O3 nanoparticles are effective fillers for microwave absorbing polymer-based composites in 1-4 GHz range applications.
Microwave and conventional techniques were employed to synthesize a novel array of compounds 7a-g with 1,2,4-triazole and piperidine rings having great biological importance. The microwave assisted method has a better operational scope with respect to time and yield comparative to the conventional method. 1H-NMR, 13C-NMR and IR techniques were employed to justify the structure of synthesized compounds. The antioxidant, butyrylcholinesterase inhibition and urease inhibition potential of every synthesized compound was evaluated. Every member of the synthesized series was found potent against mentioned activities. Compound 7g was the most active anti-urease agent having IC50 (μM) value 16.5±0.09 even better than the thiourea with an IC50(μM) value of 24.3±0.24. The better urease inhibition potential of 7g was also elaborated and explained by docking and bovine serum albumin (BSA) binding studies.
Developing multifaceted, biocompatible, artificial implants for tissue engineering is a growing field of research. In recent times, several works have been reported about the utilization of biomolecules in combination with synthetic materials to achieve this process. Accordingly, in this study, the ability of an extract obtained from Aloe vera, a commonly used medicinal plant in influencing the biocompatibility of artificial material, is scrutinized using metallocene polyethylene (mPE). The process of coating dense fibrous Aloe vera extract on the surface of mPE was carried out using microwaves. Then, several physicochemical and blood compatibility characterization experiments were performed to disclose the effects of corresponding surface modification. The Fourier transform infrared spectrum showed characteristic vibrations of several active constituents available in Aloe vera and exhibited peak shifts at far infrared regions due to aloe-based mineral deposition. Meanwhile, the contact angle analysis demonstrated a drastic increase in wettability of coated samples, which confirmed the presence of active components on glazed mPE surface. Moreover, the bio-mimic structure of Aloe vera fibers and the influence of microwaves in enhancing the coating characteristics were also meticulously displayed through scanning electron microscopy micrographs and Hirox 3D images. The existence of nanoscale roughness was interpreted through high-resolution profiles obtained from atomic force microscopy. And the extent of variations in irregularities was delineated by measuring average roughness. Aloe vera-induced enrichment in the hemocompatible properties of mPE was established by carrying out in vitro tests such as activated partial thromboplastin time, prothrombin time, platelet adhesion, and hemolysis assay. In conclusion, the Aloe vera-glazed mPE substrate was inferred to attain desirable properties required for multifaceted biomedical implants.
An experimental system for early screening of a breast tumor is presented in this article. The proposed microwave imaging (MI) system consists of a moveable array of nine improved negative-index metamaterial (MTM)-loaded ultrawideband (UWB) antenna sensor with incorporation of a corresponding SRR (split-ring resonator) and CLS (capacitively loaded strip) structure, in a circular array, the stepper motor-based array-mounting stand, the adjustable phantom hanging platform, an RF switching system to control the receivers, and a personal computer-based signal processing and image reconstruction unit using MATLAB. The improved antenna comprises of four-unit cells along one axis, where an individual unit cell integrates a balancing SRR and CLS pair, which makes the antenna radiation omnidirectional over the operating frequencies. The electrical dimensions of this proposed antenna are 0.28λ × 0.20λ × 0.016λ, measured at the lowest operating frequency of 2.97 GHz as the operating bandwidth of this is in between 2.97⁻15 GHz (134.82% bandwidth), with stable directional radiation pattern. SP8T 8 port switch is used to enable the eight receiver antennas to sequentially send a 3⁻8.0 GHz microwave signal to capture the backscattered signal by MATLAB software. A low-cost realistic homogeneous breast phantom with tumor material is developed and measured to test the capability of the imaging system to detect the breast tumors. A post-processing delay-multiply-and-sum (DMAS) algorithm is used to process the recorded backscatter signal to get an image of the breast phantom, and to accurately identify the existence and located area of multiple breast tumor tissues.
This study aimed at analyzing the concentrations of 23 minor and trace elements in aromatic spices by inductively coupled plasma-mass spectrometry (ICP-MS), after wet digestion by microwave system. The analytical method was validated by linearity, detection limits, precision, accuracy and recovery experiments, obtaining satisfactory values in all cases. Results indicated the presence of variable amounts of both minor and trace elements in the selected aromatic spices. Manganese was high in cinnamon (879.8 μg/g) followed by cardamom (758.1 μg/g) and clove (649.9 μg/g), strontium and zinc were high in ajwain (489.9 μg/g and 84.95 μg/g, respectively), while copper was high in mango powder (77.68 μg/g). On the whole some of the minor and essential trace elements were found to have good nutritional contribution in accordance to RDA. The levels of toxic trace elements, including As, Cd, and Pb were very low and did not found to pose any threat to consumers.
This work demonstrated the optimization and scale up of microwave-assisted extraction (MAE) and ultrasonic-assisted extraction (UAE) of bioactive compounds from Orthosiphon stamineus using energy-based parameters such as absorbed power density and absorbed energy density (APD-AED) and response surface methodology (RSM). The intensive optimum conditions of MAE obtained at 80% EtOH, 50mL/g, APD of 0.35W/mL, AED of 250J/mL can be used to determine the optimum conditions of the scale-dependent parameters i.e. microwave power and treatment time at various extraction scales (100-300mL solvent loading). The yields of the up scaled conditions were consistent with less than 8% discrepancy and they were about 91-98% of the Soxhlet extraction yield. By adapting APD-AED method in the case of UAE, the intensive optimum conditions of the extraction, i.e. 70% EtOH, 30mL/g, APD of 0.22W/mL, AED of 450J/mL are able to achieve similar scale up results.
Recent progress with tailored growth and post-process sorting enables carbon nanotube (CNT) assemblies with predominantly metallic or semi-conducting concentrations. Cryogenic and microwave measurements performed here show transport dimensionality and overall order increasing with increasing metallic concentration, even in atmospheric doping conditions. By 120 GHz, the conductivity of predominantly semi-conducting assemblies grew to 400% its DC value at an increasing growth rate, while other concentrations a growth rate that tapered off. A generalized Drude model fits to the different frequency dependent behaviors and yields useful quality control parameters such as plasma frequency, mean free path, and degree of localization. As one of the first demonstrations of waveguides fabricated from this material, sorted CNTs from both as-made and post-process sources were inserted into sections of practical micro-strip. With both sources, sorted CNT micro-strip increasingly outperformed the unsorted with increasing frequency-- illustrating that sorted CNT assemblies will be important for high frequency applications.
Microwave pyrolysis of oil palm fiber (OPF) with three types of Na-based catalysts was experimentally investigated to produce biochar. Sodium hydroxide (NaOH), sodium chloride (NaCl), and sodium carbonate (Na2CO3) with purity 99.9% were selected for this investigation. Microwave muffle reactor (Model: HAMiab-C1500) with a microwave power controller including a microwave generator was used to perform the microwave pyrolysis. OPF particles were used after removing foreign materials, impurities, and dust. Microwave power ranges from 400 to 900 W, temperature ranges from 450 to 700 °C, and N2 flow rates ranges from 200 to -1200 cm3/min were used along with all three Na-based catalysts for this investigation. Lower microwave power, temperature, and N2 flow rate have been found favorable for higher yield of biochar. NaOH is to be found as the more suitable catalyst than NaCl and Na2CO3 to produce biochar. A maximum biochar yield (51.42 wt%) has been found by using the catalysts NaOH at N2 flow rate of 200 cm3/min. One sample of the biochar (maximum yield without catalysts) was selected for further characterization via thermo gravimetric analysis (TGA), scanning electron microscopy (SEM), BET surface area, Fourier transform infrared spectroscopy (FTIR), and ultimate and proximate analysis. SEM and BET surface area analysis showed the presence of some pores in the biochar. High percentage of carbon (60.24 wt%) was also recorded in the sample biochar. The pores and high percentage of carbon of biochar have significant impact on soil fertilization by increasing the carbon sequestration in the soil. It assists to slow down the decomposition rate of nutrients from soil and therefore enhances the soil quality.
Microwave-assisted extraction (MAE) is widely employed in the analysis and the extraction of active compounds from plants. This review summarizes the research done during the last decade on the MAE of active ingredients from plants. Advances and modifications to improve the performance of MAE are presented and discussed in detail. Modified MAE such as vacuum microwave-assisted extraction (VMAE), nitrogen-protected microwave-assisted extraction (NPMAE), ultrasonic microwave-assisted extraction (UMAE), dynamic microwave-assisted extraction (DMAE) and other advancements in MAE are also detailed in this article. In addition, the microwave extraction procedures and the important parameters influencing its performance are also included, together with the advantages and the drawbacks of each MAE techniques.
Optimization process is an important aspect in the natural product extractions. Herein, an alternative approach is proposed for the optimization in extraction, namely, the Generalized Likelihood Uncertainty Estimation (GLUE). The approach combines the Latin hypercube sampling, the feasible range of independent variables, the Monte Carlo simulation, and the threshold criteria of response variables. The GLUE method is tested in three different techniques including the ultrasound, the microwave, and the supercritical CO2 assisted extractions utilizing the data from previously published reports. The study found that this method can: provide more information on the combined effects of the independent variables on the response variables in the dotty plots; deal with unlimited number of independent and response variables; consider combined multiple threshold criteria, which is subjective depending on the target of the investigation for response variables; and provide a range of values with their distribution for the optimization.
A rapid, sustainable, and ecologically sound approach is urgently needed for the production of semiconductor nanomaterials. CuSe nanoparticles (NPs) were synthesized via a microwave-assisted technique using CuCl2·2H2O and Na2SeO3 as the starting materials. The role of the irradiation time was considered as the primary concern to regulate the size and possibly the shape of the synthesized nanoparticles. A range of characterization techniques was used to elucidate the structural and optical properties of the fabricated nanoparticles, which included X-ray diffraction, energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy, field emission scanning electron microscopy, Raman spectroscopy (Raman), UV-Visible diffuse reflectance spectroscopy (DRS), and photoluminescence spectroscopy (PL). The mean crystallite size of the CuSe hexagonal (Klockmannite) crystal structure increased from 21.35 to 99.85 nm with the increase in irradiation time. At the same time, the microstrain and dislocation density decreased from 7.90 × 10-4 to 1.560 × 10-4 and 4.68 × 10-2 to 1.00 × 10-2 nm-2, respectively. Three Raman vibrational bands attributed to CuSe NPs have been identified in the Raman spectrum. Irradiation time was also seen to play a critical role in the NP optical band gap during the synthesis. The decrease in the optical band gap from 1.85 to 1.60 eV is attributed to the increase in the crystallite size when the irradiation time was increased. At 400 nm excitation wavelength, a strong orange emission centered at 610 nm was observed from the PL measurement. The PL intensity is found to increase with an increase in irradiation time, which is attributed to the improvement in crystallinity at higher irradiation time. Therefore, the results obtained in this study could be of great benefit in the field of photonics, solar cells, and optoelectronic applications.
We developed an innovative single-step pyrolysis approach that combines microwave heating and activation by CO2 or steam to transform orange peel waste (OPW) into microwave activated biochar (MAB). This involves carbonization and activation simultaneously under an inert environment. Using CO2 demonstrates dual functions in this approach, acting as purging gas to provide an inert environment for pyrolysis while activating highly porous MAB. This approach demonstrates rapid heating rate (15-120 °C/min), higher temperature (> 800 °C) and shorter process time (15 min) compared to conventional method using furnace (> 1 h). The MAB shows higher mass yield (31-44 wt %), high content of fixed carbon (58.6-61.2 wt %), Brunauer Emmett Teller (BET) surface area (158.5-305.1 m2/g), low ratio of H/C (0.3) and O/C (0.2). Activation with CO2 produces more micropores than using steam that generates more mesopores. Steam-activated MAB records a higher adsorption efficiency (136 mg/g) compared to CO2 activation (91 mg/g), achieving 89-93 % removal of Congo Red dye. The microwave pyrolysis coupled with steam or CO2 activation thereby represents a promising approach to transform fruit-peel waste to microwave-activated biochar that remove hazardous dye.
A micro-mesoporous activated carbon (AC) was produced via an innovative approach combining microwave pyrolysis and chemical activation using NaOH/KOH mixture. The pyrolysis was examined over different chemical impregnation ratio, microwave power, microwave irradiation time and types of activating agents for the yield, chemical composition, and porous characteristic of the AC obtained. The AC was then tested for its feasibility as textile dye adsorbent. About 29 wt% yield of AC was obtained from the banana peel with low ash and moisture (<5 wt%), and showed a micro-mesoporous structure with high BET surface area (≤1038 m2/g) and pore volume (≤0.80 cm3/g), indicating that it can be utilized as adsorbent to remove dye. Up to 90% adsorption of malachite green dye was achieved by the AC. Our results indicate that the microwave-activation approach represents a promising attempt to produce good quality AC for dye adsorption.
Microwave-steam activation (MSA), an innovative pyrolysis approach combining the use of microwave heating and steam activation, was investigated for its potential production of high grade activated carbon (AC) from waste palm shell (WPS) for methylene blue removal. MSA was performed via pyrolytic carbonization of WPS to produce biochar as the first step followed by steam activation of the biochar using microwave heating to form AC. Optimum yield and adsorption efficiency of methylene blue were obtained using response surface methodology involving several key process parameters. The resulting AC was characterized for its porous characteristics, surface morphology, proximate analysis and elemental compositions. MSA provided a high activation temperature above 500 °C with short process time of 15 min and rapid heating rate (≤150 °C/min). The results from optimization showed that one gram of AC produced from steam activation under 10 min of microwave heating at 550 °C can remove up to 38.5 mg of methylene blue. The AC showed a high and uniform surface porosity consisting high fixed carbon (73 wt%), micropore and BET surface area of 763.1 and 570.8 m2/g respectively, hence suggesting the great potential of MSA as a promising approach to produce high grade adsorbent for dye removal.
Microwave vacuum pyrolysis of palm kernel shell was examined to produce engineered biochar for application as additive in agriculture application. The pyrolysis approach, performed at 750 W of microwave power, produced higher yield of porous biochar (28 wt%) with high surface area (270 cm2/g) compared to the yield obtained by conventional approach (<23 wt%). Addition of the porous biochar in mushroom substrate showed increased moisture content (99%) compared to the substrate without biochar (96%). The mushroom substrate added with biochar (150 g) was optimal in shortening formation, growth, and full colonization of the mycelium within one month. Using 2.5% of the biochar in mushroom substrate desirably maintained the optimum pH level (6.8-7) during the mycelium colonization period, leading to high mycelium growth (up to 91%) and mushroom yield (up to 280 g). The engineered biochar shows great potential as moisture retention and neutralizing agent in mushroom cultivation.