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    Coercivity and exchange bias in ti-doped maghemite nanoparticles
    (MDPI, 2022) Narayanaswamy, Venkatesha; Al-Omari, Imaddin A.; Kamzin, Aleksandr S.; Khurshid, Hafsa; Khaleel, Abbas; Issa, Bashar; Obaidat, Ihab M.
    Ti-doped maghemite nanoparticles of average crystallite size 12.9 nm were synthesized using the sol-gel method. The XRD profile mainly showed the presence of maghemite phase with very small phases of TiO2 (rutile and anatase). Magnetization hysteresis loops of the nanoparticles were obtained between -4 T to +4 T at temperatures of 2, 10, 30, 50, 70, 100, 150, 200, and 300 K under field cooling (FC) of 1, 2, 3, and 4 T and zero-field cooling conditions (ZFC). The coercivity displayed nonmonotonic field dependence while it decreased sharply with temperature and vanished at 150 K at all fields. Horizontal hysteresis loop shifts were observed in the 2-150 K temperature range in both the ZFC and FC conditions. The exchange bias effect became negligible in both ZFC and FC states above 50 K. Magnetization vs. applied field measurements were conducted in both ZFC and FC cooled conditions at several temperatures in the range of 2-400 K, with spin freezing being observed below 50 K. The exchange bias effect obtained below 50 K is suggested to be attributed to the competing roles of the long-range dipolar and short-range exchange coupled interactions.
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    Engineering of nickel, cobalt oxides and nickel/cobalt binary oxides by electrodeposition and application as binder free electrodes in supercapacitors
    (Nature Portfolio, 2023) Abbas, Qaisar; Khurshid, Hafsa; Yoosuf, Rahana; Lawrence, Jonathan; Issa, Bashar A.; Abdelkareem, Mohammad Ali; Olabi, Abdul Ghani
    Cobalt oxide, nickel oxide and cobalt/nickel binary oxides were synthesised by electrodeposition. To fine tune composition of CoNi alloys, growth parameters including voltage, electrolyte pH/concentration and deposition time were varied. These produced nanomaterials were used as binder free electrodes in supercapacitor cells and tested using three electrode setup in 2 MKOH aqueous electrolyte. Cyclic voltammetry and galvanostatic charge/discharge were used at different scan rates (5-100 mV/s) and current densities (1-10 A/g) respectively to investigate the capacitive behaviour and measure the capacitance of active material. Electrochemical impedance spectroscopy was used to analyse the resistive/conductive behaviours of these electrodes in frequency range of 100 kHz to 0.01 Hz at applied voltage of 10 mV. Binary oxide electrode displayed superior electrochemical performance with the specific capacitance of 176 F/g at current density of 1 A/g. This hybrid electrode also displayed capacitance retention of over 83% after 5000 charge/discharge cycles. Cell displayed low solution resistance of 0.35 Omega along with good conductivity. The proposed facile approach to synthesise binder free blended metal electrodes can result in enhanced redox activity of pseudocapacitive materials. Consequently, fine tuning of these materials by controlling the cobalt and nickel contents can assist in broadening their applications in electrochemical energy storage in general and in supercapacitors in particular.
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    Evaluation of Antiproliferative Properties of CoMnZn-Fe2O4 Ferrite Nanoparticles in Colorectal Cancer Cells
    (Mdpi, 2024) Narayanaswamy, Venkatesha; Rah, Bilal; Al-Omari, Imaddin A.; Kamzin, Alexander S.; Khurshid, Hafsa; Muhammad, Jibran Sualeh; Obaidat, Ihab M.
    The PEG-coated ferrite nanoparticles Co0.2Mn0.6Zn0.2Fe2O4 (X1), Co0.4Mn0.4Zn0.2Fe2O4 (X2), and Co0.6Mn0.2Zn0.2Fe2O4 (X3) were synthesized by the coprecipitation method. The nanoparticles were characterized by XRD, Raman, VSM, XPS, and TEM. The magnetic hyperthermia efficiency (MH) was determined for PEG-coated nanoparticles using an alternating magnetic field (AMF). X2 nanoparticles displayed the highest saturation magnetization and specific absorption rate (SAR) value of 245.2 W/g for 2 mg/mL in a water medium. Based on these properties, X2 nanoparticles were further evaluated for antiproliferative activity against HCT116 cells at an AMF of 495.25 kHz frequency and 350 G strength, using MTT, colony formation, wound healing assays, and flow cytometry analysis for determining the cell viability, clonogenic property, cell migration ability, and cell death of HCT116 cells upon AMF treatment in HCT116 cells, respectively. We observed a significant inhibition of cell viability (2% for untreated control vs. 50% for AMF), colony-forming ability (530 cells/colony for untreated control vs. 220 cells/colony for AMF), abrogation of cell migration (100% wound closure for untreated control vs. 5% wound closure for AMF), and induction of apoptosis-mediated cell death (7.5% for untreated control vs. 24.7% for AMF) of HCT116 cells with respect to untreated control cells after AMF treatment. Collectively, these results demonstrated that the PEG-coated (CoMnZn-Fe2O4) mixed ferrite nanoparticles upon treatment with AMF induced a significant antiproliferative effect on HCT116 cells compared with the untreated cells, indicating the promising antiproliferative potential of the Co0.4Mn0.4Zn0.2Fe2O4 nanoparticles for targeting colorectal cancer cells. Additionally, these results provide appealing evidence that ferrite-based nanoparticles using MH could act as potential anticancer agents and need further evaluation in preclinical models in future studies against colorectal and other cancers.
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    Hyperthermia of magnetically soft-soft core-shell ferrite nanoparticles
    (MDPI, 2022) Narayanaswamy, Venkatesha; Jagal, Jayalakshmi; Khurshid, Hafsa; Al-Omari, Imaddin A. A.; Haider, Mohamed; Kamzin, Alexander S. S.; Obaidat, Ihab M. M.; Issa, Bashar
    Magnetically soft-soft MnFe2O4-Fe3O4 core-shell nanoparticles were synthesized through a seed-mediated method using the organometallic decomposition of metal acetyl acetonates. Two sets of core-shell nanoparticles (S1 and S2) of similar core sizes of 5.0 nm and different shell thicknesses (4.1 nm for S1 and 5.7 nm for S2) were obtained by changing the number of nucleating sites. Magnetic measurements were conducted on the nanoparticles at low and room temperatures to study the shell thickness and temperature dependence of the magnetic properties. Interestingly, both core-shell nanoparticles showed similar saturation magnetization, revealing the ineffective role of the shell thickness. In addition, the coercivity in both samples displayed similar temperature dependencies and magnitudes. Signatures of spin glass (SG) like behavior were observed from the field-cooled temperature-dependent magnetization measurements. It was suggested to be due to interface spin freezing. We observed a slight and non-monotonic temperature-dependent exchange bias in both samples with slightly higher values for S2. The effective magnetic anisotropy constant was calculated to be slightly larger in S2 than that in S1. The magnetothermal efficiency of the chitosan-coated nanoparticles was determined by measuring the specific absorption rate (SAR) under an alternating magnetic field (AMF) at 200-350 G field strengths and frequencies (495.25-167.30 kHz). The S2 nanoparticles displayed larger SAR values than the S1 nanoparticles at all field parameters. A maximum SAR value of 356.5 W/g was obtained for S2 at 495.25 kHz and 350 G for the 1 mg/mL nanoparticle concentration of ferrogel. We attributed this behavior to the larger interface SG regions in S2, which mediated the interaction between the core and shell and thus provided indirect exchange coupling between the core and shell phases. The SAR values of the core-shell nanoparticles roughly agreed with the predictions of the linear response theory. The concentration of the nanoparticles was found to affect heat conversion to a great extent. The in vitro treatment of the MDA-MB-231 human breast cancer cell line and HT-29 human colorectal cancer cell was conducted at selected frequencies and field strengths to evaluate the efficiency of the nanoparticles in killing cancer cells. The cellular cytotoxicity was estimated using flow cytometry and an MTT assay at 0 and 24 h after treatment with the AMF. The cells subjected to a 45 min treatment of the AMF (384.50 kHz and 350 G) showed a remarkable decrease in cell viability. The enhanced SAR values of the core-shell nanoparticles compared to the seeds with the most enhancement in S2 is an indication of the potential for tailoring nanoparticle structures and hence their magnetic properties for effective heat generation.