Structural, Electromagnetic and Microwave Properties of Magnetite Extracted from Mill Scale Waste via Conventional Ball Milling and Mechanical Alloying Techniques.

This study presents the utilization of mill scale waste, which has attracted much attention due to its high content of magnetite (Fe3O4). This work focuses on the extraction of Fe3O4 from mill scale waste via magnetic separation, and ball milling was used to fabricate a microwave absorber. The extracted magnetic powder was ground-milled using two different techniques: (i) a conventional milling technique (CM) and (ii) mechanical alloying (MM) process. The Fe3O4/CM samples were prepared by a conventional milling process using steel pot ball milling, while the Fe3O4/MM samples were prepared using a high-energy ball milling (HEBM) method. The effect of milling time on the structural, phase composition, and electromagnetic properties were examined using X-ray diffraction (XRD) and a vector network analyzer (VNA). XRD confirmed the formation of magnetite after both the magnetic separation and milling processes. The results revealed that Fe3O4 exhibited excellent microwave absorption properties because of the synergistic characteristics of its dielectric and magnetic loss. The results showed that the Fe3O4/CM particle powder had a greater absorption power (reflection loss: <-10 dB) with 99.9% absorption, a minimum reflection loss of -30.83 dB, and an effective bandwidth of 2.30 GHz for 2 mm thick samples. The results revealed the Fe3O4/MM powders had higher absorption properties, including a higher RL of -20.59 dB and a broader bandwidth of 2.43 GHz at a matching thickness of only 1 mm. The higher microwave absorption performance was attributed to the better impedance matching property caused by the porous microstructure. Furthermore, the magnetite, Fe3O4 showed superior microwave absorption characteristics because of the lower value of permittivity, which resulted in better impedance matching. This study presents a low-cost approach method by reutilizing mill scale waste to fabricate a high purity crystalline Fe3O4 with the best potential for designing magnetic nano-sized based microwave absorbers.

Adsorptive Removal of Copper (II) Ions from Aqueous Solution Using a Magnetite Nano-Adsorbent from Mill Scale Waste: Synthesis, Characterization, Adsorption and Kinetic Modelling Studies.

In this study, magnetite nano-adsorbent (MNA) was extracted from mill scale waste products, synthesized and applied to eliminate Cu2+ from an aqueous solution. Mill scale waste product was ground using conventional milling and impacted using high-energy ball milling (HEBM) for varying 3, 5, and 7 milling hours. In this regard, the prepared MNA was investigated using X-ray diffraction (XRD), high-resolution transmission electron microscope (HRTEM), field emission scanning electron microscopy-energy-dispersive X-ray spectroscopy (FESEM-EDS), UV-Vis spectroscopy, Fourier-transform infrared (FTIR), Brunauer-Emmett-Teller (BET) and zeta potential. The resultant MNA-7 h milling time displayed a crystalline structure with irregular shapes of 11.23 nm, specific surface area of 5.98 m2g-1, saturation magnetization, Ms of 8.35 emug-1, and isoelectric point charge at pH 5.4. The optimum adsorption capacity, qe of 4.42 mg.g-1 for the removal of Cu2+ ions was attained at 120 min of contact time. The experimental data were best fitted to the Temkin isotherm model. A comparison between experimental kinetic studies and the theoretical aspects showed that the pseudo-second-order matched the experimental trends with a correlation coefficient of (R2 > 0.99). Besides, regeneration efficiency of 70.87% was achieved after three cycles of reusability studies. The MNA offers a practical, efficient, low-cost approach to reutilize mill scale waste products and provide ultra-fast separation to remove Cu2+ from water.

Structural, microstructural, magnetic and electromagnetic absorption properties of spiraled multiwalled carbon nanotubes/barium hexaferrite (MWCNTs/BaFe12O19) hybrid.

Microwave absorption properties were systematically studied for synthesised barium hexaferrite (BaFe12O19) nanoparticles and spiraled multiwalled carbon nanotubes (MWCNTs) hybrid. BaFe12O19 nanoparticles were synthesised by a high energy ball milling (HEBM) followed by sintering at 1400 °C and structural, electromagnetic and microwave characteristics have been scrutinized thoroughly. The sintered powders were then used as a catalyst to synthesise spiraled MWCNTs/BaFe12O19 hybrid via the chemical vapour deposition (CVD) process. The materials were then incorporated into epoxy resin to fabricate single-layer composite structures with a thickness of 2 mm. The composite of BaFe12O19 nanoparticles showed a minimum reflection loss is - 3.58 dB and no has an absorption bandwidth while the spiraled MWCNTs/BaFe12O19 hybrid showed the highest microwave absorption of more than 99.9%, with a minimum reflection loss of - 43.99 dB and an absorption bandwidth of 2.56 GHz. This indicates that spiraled MWCNTs/BaFe12O19 hybrid is a potential microwave absorber for microwave applications in X and Ku bands.

Effects of Recycled Fe2O3 Nanofiller on the Structural, Thermal, Mechanical, Dielectric, and Magnetic Properties of PTFE Matrix.

The purpose of this study was to improve the dielectric, magnetic, and thermal properties of polytetrafluoroethylene (PTFE) composites using recycled Fe2O3 (rFe2O3) nanofiller. Hematite (Fe2O3) was recycled from mill scale waste and the particle size was reduced to 11.3 nm after 6 h of high-energy ball milling. Different compositions (5-25 wt %) of rFe2O3 nanoparticles were incorporated as a filler in the PTFE matrix through a hydraulic pressing and sintering method in order to fabricate rFe2O3-PTFE nanocomposites. The microstructure properties of rFe2O3 nanoparticles and the nanocomposites were characterized through X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). The thermal expansion coefficients (CTEs) of the PTFE matrix and nanocomposites were determined using a dilatometer apparatus. The complex permittivity and permeability were measured using rectangular waveguide connected to vector network analyzer (VNA) in the frequency range 8.2-12.4 GHz. The CTE of PTFE matrix decreased from 65.28×10-6/°C to 39.84×10-6/°C when the filler loading increased to 25 wt %. The real (ε') and imaginary (ε″) parts of permittivity increased with the rFe2O3 loading and reached maximum values of 3.1 and 0.23 at 8 GHz when the filler loading was increased from 5 to 25 wt %. A maximum complex permeability of 1.1-j0.07 was also achieved by 25 wt % nanocomposite at 10 GHz.

Novel PVDF-PVP Hollow Fiber Membrane Augmented with TiO2 Nanoparticles: Preparation, Characterization and Application for Copper Removal from Leachate.

High proportion of copper has become a global challenge owing to its negative impact on the environment and public health complications. The present study focuses on the fabrication of a polyvinylidene fluoride (PVDF)-polyvinyl pyrrolidone (PVP) fiber membrane incorporated with varying loading (0, 0.5, 1.0, 1.5, and 2.0 wt%) of titanium dioxide (TiO2) nanoparticles via phase inversion technique to achieve hydrophilicity along with high selectivity for copper removal. The developed fibers were characterized based on scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), permeability, porosity, zeta potential, and contact angle. The improved membrane (with 1.0 wt% TiO2) concentration recorded the maximum flux (223 L/m2·h) and copper rejection (98.18%). Similarly, 1.0 wt% concentration of TiO2 nanoparticles made the membrane matrix more hydrophilic with the least contact angle of 50.01°. The maximum copper adsorption capacity of 69.68 mg/g was attained at 1.0 wt% TiO2 concentration. The experimental data of adsorption capacity were best fitted to the Freundlich isotherm model with R2 value of 0.99573. The hybrid membrane developed in this study has considerably eliminated copper from leachate and the concentration of copper in the permeate was substantially reduced to 0.044 mg/L, which is below standard discharge threshold.

Complex permittivity and power loss characteristics of α-Fe2O3/polycaprolactone (PCL) nanocomposites: effect of recycled α-Fe2O3 nanofiller.

The development of microwave absorbing materials based on recycled hematite (α-Fe2O3) nanoparticles and polycaprolactone (PCL) was the main focus of this study. α-Fe2O3 was recycled from mill scale and reduced to nanoparticles through high energy ball milling in order to improve its complex permittivity properties. Different compositions (5% wt., 10% wt., 15% wt. and 20% wt.) of the recycled α-Fe2O3 nanoparticles were melt-blended with PCL using a twin screw extruder to fabricate recycled α-Fe2O3/PCL nanocomposites. The samples were characterized for their microstructural properties through X - ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). The complex permittivity and microwave absorption properties were respectively measured using the open ended coaxial (OEC) probe and a microstrip in connection with a vector network analyzer in the 1-4 GHz frequency range. An average α-Fe2O3 nanoparticle size of 16.2 nm was obtained with a maximum imaginary (ε") part of permittivity value of 0.54 at 4 GHz. The complex permittivity and power loss values of the nanocomposites increased with recycled α-Fe2O3 nanofiller content. At 2.4 GHz, the power loss (dB) values obtained for all the nanocomposites were between 13.3 dB and 14.4 dB and at 3.4 GHz, a maximum value of 16.37 dB was achieved for the 20 % wt. nanocomposite. The recycled α-Fe2O3/PCL nanocomposites have the potential for use in noise reduction applications in the 1-4 GHz range.

Utilization of Nano-TiO2 as an Influential Additive for Complementing Separation Performance of a Hybrid PVDF-PVP Hollow Fiber: Boron Removal from Leachate.

The continuous increase in anthropogenic activities resulting in an increase in boron concentration in the environment is becoming a serious threat to public health and the ecosystem. In this regard, a hybrid polyvinylidene fluoride (PVDF)-polyvinyl pyrrolidone (PVP) hollow fiber was synthesized with hydrophilic nano-titanium oxide (TiO2) at varied loadings of 0, 0.5, 1.0, 1.5, and 2.0 wt% using the phase inversion technique. The resultant membranes were characterized in terms of Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), contact angle, porosity, and zeta potential. The permeability flux was assessed using both pure water and leachate; also, rejection performance was evaluated based on boron removal from the leachate. The results revealed that the membrane with 1.0 wt% loading had the highest flux alongside an upturn in boron rejection percentage of 223 L/m2·h and 94.39%, respectively. In addition, the lowest contact angle of 50.01° was recorded with 1.0 wt% TiO2 loading, and this implies that it is the most hydrophilic. Throughout the experiment cycles, the fiber with 1.0 wt% TiO2 loading demonstrated a high flux recovery varying between 92.82% and 76.26% after 9 h filtration time. The physicochemical analysis of the permeate revealed that the boron concentration was significantly reduced to 0.43 mg/L, which is far lower than the discharge limit of 1.0 mg/L.

An investigation of microstructural, magnetic and microwave absorption properties of multi-walled carbon nanotubes/Ni0.5Zn0.5Fe2O4.

The enhancement of microwave absorbing properties in nickel zinc ferrite (Ni0.5Zn0.5Fe2O4) via multiwall carbon nanotubes (MWCNT) growth is studied in this research work. Ni0.5Zn0.5Fe2O4 was initially synthesized by mechanical alloying followed by sintering at 1200 °C and the microstructural, electromagnetic and microwave characteristics have been scrutinized thoroughly. The sintered powder was then used as a catalyst to grow MWCNT derived from chemical vapor deposition (CVD) method. The sample was mixed with epoxy resin and a hardener for preparation of composites. The composite of multi-walled carbon nanotubes/Ni0.5Zn0.5Fe2O4 shown a maximum reflection loss (RL) of -19.34 dB at the frequency and bandwidth of 8.46 GHz and 1.24 GHz for an absorber thickness of 3 mm for losses less than -10 dB. This acquired result indicates that multi-walled carbon nanotubes/Ni0.5Zn0.5Fe2O4 could be used as a microwave absorber application in X-band.

Complex Permittivity and Microwave Absorption Properties of OPEFB Fiber-Polycaprolactone Composites Filled with Recycled Hematite (α-Fe2O3) Nanoparticles.

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.

Enhancement of Complex Permittivity and Attenuation Properties of Recycled Hematite (α-Fe2O3) Using Nanoparticles Prepared via Ball Milling Technique.

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.

Photothermal Effect of Modulating Laser Irradiation on the Thermal Diffusivity of Al2O3 Nanofluids.

Modulated continuous wave (CW) lasers cause photothermal effect that leads to rapid optical absorption and generation of thermal waves around the irradiated nanostructures. In this work, we examined the effect of modulated CW laser irradiation on the particle fragmentation process to enhance the thermal diffusivity of nanofluids. A facile and cost-effective diode laser was applied to reduce the agglomerated size of Al2O3 nanoparticles in deionized water. The thermal wave generation, which was determined by the modulated frequency of the laser beam and the optical and thermal properties of the nanofluid, is also briefly discussed and summarized. The influence of laser irradiation time on nanoparticle sizes and their size distribution was determined by dynamic light scattering and transmission electron microscopy. The thermal diffusivity of the nanofluid was measured using the photopyroelectric method. The data obtained showed that the modulated laser irradiation caused the partial fragmentation of some agglomerated particles in the colloids, with an average diameter close to the original particle size, as indicated by a narrow distribution size. The reduction in the agglomerated size of the particles also resulted in an enhancement of the thermal diffusivity values, from 1.444 × 10-3 to 1.498 × 10-3 cm2/s in 0 to 30 min of irradiation time. This work brings new possibilities and insight into the fragmentation of agglomerated nanomaterials based on the photothermal study.

Effect of Ratio in Ammonium Nitrate on the Structural, Microstructural, Magnetic, and AC Conductivity Properties of BaFe12O19.

This paper investigates the effect of the ratio of ammonium nitrate (AN) on the structural, microstructural, magnetic, and alternating current (AC) conductivity properties of barium hexaferrite (BaFe12O19). The BaFe12O19 were prepared by using the salt melt method. The samples were synthesized using different powder-to-salt weight ratio variations (1:3, 1:4, 1:5, 1:6 and 1:7) of BaCO3 + Fe2O3 and ammonium nitrate salt. The NH4NO3 was melted on a hot plate at 170 °C. A mixture of BaCO3 and Fe2O3 were added into the NH4NO3 melt solution and stirred for several hours using a magnetic stirrer under a controlled temperature of 170 °C. The heating temperature was then increased up to 260 °C for 24 hr to produce an ash powder. The x-ray diffraction (XRD) results show the intense peak of BaFe12O19 for all the samples and the presence of a small amount of the impurity Fe2O3 in the samples, at a ratio of 1:5 and 1:6. From the Fourier transform infra-red (FTIR) spectra, the band appears at 542.71 cm - 1 and 432.48 cm - 1 , which corresponding to metal⁻oxygen bending and the vibration of the octahedral sites of BaFe12O19. The field emission scanning electron microscope (FESEM) images show that the grains of the samples appear to stick each other and agglomerate at different masses throughout the image with the grain size 5.26, 5.88, 6.14, 6.22, and 6.18 µm for the ratios 1:3, 1:4, 1:5, 1:6, and 1:7 respectively. From the vibrating sample magnetometer (VSM) analysis, the magnetic properties of the sample ratio at 1:3 show the highest value of coercivity Hc of 1317 Oe, a saturation magnetization Ms of 91 emu/g, and a remnant Mr of 44 emu/g, respectively. As the temperature rises, the AC conductivity is increases with an increase in frequency.

Influence of pH Adjustment Parameter for Sol-Gel Modification on Structural, Microstructure, and Magnetic Properties of Nanocrystalline Strontium Ferrite.

Synthesis of nanocrystalline strontium ferrite (SrFe12O19) via sol-gel is sensitive to its modification parameters. Therefore, in this study, an attempt of regulating the pH as a sol-gel modification parameter during preparation of SrFe12O19 nanoparticles sintered at a low sintering temperature of 900 °C has been presented. The relationship of varying pH (pH 0 to 8) on structural, microstructures, and magnetic behaviors of SrFe12O19 nanoparticles were characterized by X-ray diffraction (XRD), field emission scanning microscope (FESEM), and vibrating sample magnetometer (VSM). Varying the pH of precursor exhibited a strong effect on the sintered density, crystal structure and magnetic properties of the SrFe12O19 nanoparticles. As the pH is 0, the SrFe12O19 produced relatively largest density, saturation magnetization, Ms, and coercivity, Hc, at a low sintering temperature of 900 °C. The grain size of SrFe12O19 is obtained in the range of 73.6 to 133.3 nm. The porosity of the sample affected the density and the magnetic properties of the SrFe12O19 ferrite. It is suggested that the low-temperature sintered SrFe12O19 at pH 0 displayed Ms of 44.19 emu/g and Hc of 6403.6 Oe, possessing a significant potential for applying in low-temperature co-fired ceramic permanent magnet.