Synthesis of transition metal oxides by microwave irradiation is a faster and energy-saving method compared to conventional heating in an electrical furnace because microwave energy is directly converted into heat within precursors. However, not much is known about how the physical properties are modified by the power of microwaves. We synthesized LaMnO3+d by irradiating oxide precursors with microwaves and studied the impact of microwave power (P = 1000 W, 1200 W, 1400 W and 1600 W) on magnetism, resistivity, magnetoresistance, thermopower, magnetic entropy change, magnetostriction, and electron spin resonance. It is found that paramagnetic to ferromagnetic transition becomes sharper, saturation magnetization increases, and electrical resistivity at low temperatures dramatically decreases as P increases. While the resistivity of samples irradiated with MW power of P less than or equal to 1400 W show insulating-like behavior down to 50 K, an insulator-metal transition occurs in the sample exposed to P = 1600 W and this sample also shows a maximum magnetoresistance (= -55%), magneto-thermopower (=-87%), magnetostriction (-180 x10-6) for H = 50 kOe and magnetic entropy change of 4.78 J/kg. K for H = 30 kOe around the Curie temperature. The intensity of electron spin resonance spectra at 300 K increases with P. We postulate that the much enhanced physical properties observed for the P = 1600 W sample arise from the creation of higher hole density, chemical homogeneity, and increased grain size. Our study shows that microwave power can be used as a knob to tune magnetism and other physical properties to our advantage.
The use of microwave irradiation is a promising alternative heat source for the synthesis of inorganic materials such as perovskite oxides. The method offers massive energy and time savings as compared to the traditional ceramic method. In this work we review the basic principles of the microwave heating mechanism based on interactions between dipoles in the material and the electromagnetic microwave. Furthermore, we comment on and classify all different sub-types of microwave synthesis such as solid-state microwave and microwave assisted hydrothermal synthesis. In the experimental part of thi…
Microwave assisted magnetization reversal has been investigated in a bilayer system of Pt/ferromagnet by detecting a change in the polarity of the spin pumping signal. The reversal process is studied in two material systems, Pt/CoFeB and Pt/NiFe, for different aspect ratios. The onset of the switching behavior is indicated by a sharp transition in the spin pumping voltage. At a threshold value of the external field, the switching process changes from partial to full reversal with increasing microwave power. The proposed method provides a simple way to detect microwave assisted magnetization re…
The microwave assisted magnetisation reversal is modelled in a permalloy micron-sized magnetic ellipsoid. Our simulations confirm that this process requires less field than magnetisation reversal under a static field. This is due to a different reversal mode which in case of the microwave-assisted process is always a ripple structure. During the magnetisation reversal two stages: nucleation and relaxation are distinguished. The nucleation process is governed by spinwave instabilities. The relaxation process is related to the domain expansion through domain wall propagation determined by the pr…
Few layer graphene (FLG) was synthesized by $μ$-wave assisted exfoliation of expanded graphite in toluene with an overall yield from c.a. 7% to 20%. A significant difference in the absorption of $μ$-waves by the expanded graphite and toluene allowed a rapid heating of the medium. The number of FLG sheets varies from 3 to 12, while the lateral size of the sheets exceeds few $μ$ms. The obtained FLG exhibits very low resistance with average value of 1.6 k$Ω$ (500 $Ω$ minimum) which is comparable to that of high quality graphenes synthesized by CVD methods, and lower than numbers of exfoliated gra…
Water-free NH4V3O8 microcrystals have been successfully synthesized by a microwave-assisted hydrothermal method. The products were characterized by means of X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, thermal gravimetric analysis, cyclic voltammetry, and galvanostatic cycling. The results show phase-pure products whose particle size and morphology can be tailored by varying the reaction conditions, i.e., reaction temperature, synthesis duration, and initial pH value. For instance, at low pH (2.5 to 3), flower-like agglomerates with primary particle…
We have developed a simple, surfactant assisted synthesis route for the preparation, in gram quantities, of Co and Li doped ZnO nanocrystalline samples showing robust room temperature ferromagnetism. Our studies show that RTF is intrinsic to Zn0.85Co0.05Li0.10O and not due to any segregated secondary phases. In addition, it has been shown that the defects play an important role in activating RTF in these oxide systems. This also provide an explanation for the widely varying results observed in the literature. The method can also be extended for the synthesis of other transition metal doped ZnO…
We have designed a system to study microwave assisted domain wall nucleation in permalloy nanowires. We find a substantial decrease in the nucleation field when microwave fields are applied, in comparison to pulse fields. A clear resonance peak is observed in the frequency dependence of the nucleation field, which coincides with the uniform mode ferromagnetic resonance frequency. Owing to the well-defined nucleation process, the switching field distribution is small in contrast to previous reports. Our results show that localized microwave field provides an efficient tool for injecting domain …
We develop an efficient and general method for optimizing the microwave field that achieves magnetization switching with a smaller static field. This method is based on optimal control and renders an exact solution for the 3D microwave field that triggers the switching of a nanomagnet with a given anisotropy and in an oblique static field. Applying this technique to the particular case of uniaxial anisotropy, we show that the optimal microwave field, that achieves switching with minimal absorbed energy, is modulated both in frequency and in magnitude. Its role is to drive the magnetization fro…
We studied the microwave assisted magnetic reversal of 65 nm by 71 nm elliptical Ni80Fe20 nanomagnets. Hysteresis curves were measured by magneto-optical Kerr effect for a range of microwave frequencies and amplitudes. The coercive field Hc was reduced by 26% for an rf field of 0.08Hc when the microwave frequency coincided with the minimum of the experimentally determined ferromagnetic resonance frequency with varying dc field. The experimental results for the fractional reduction in Hc with rf field amplitude are in good agreement with numerical simulations for an array of interacting macrosp…
Polymer assisted spherical FeNi nanoparticles were prepared via wet chemical method using hydrazine as a reducing agent and polymers (PVP and PEG) as reducing and stabilizing agent. Structural studies performed using XRD and TEM shows uniform dispersion of fine FeNi nanocrystallites in nanocomposite particles. The size and thermal stability of FeNi nanoparticles prepared under same reaction condition was found to be dependent on the type and the molecular weight of the polymer used. However, the magnetic properties of nanocomposite particles were not influenced by the polymers. The study highl…
Flower-like nanostructures formed by ZnO nanorods were synthesized and deposited on seeded silicon and glass substrates by a hexamethylenetetramine (HMTA) - assisted hydrothermal method at low temperature (90 oC) with methenamine ((CH3)6N4), as surfactant and catalyst. The substrates were seeded with ZnO nanoparticles. The structure and morphology of the nanostructures were studied by means of x-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), and scanning electron microscopy (SEM) techniques. Influence of the seed nanoparticle on the formation of the flower-lik…
Monochalcogenides of germanium (or tin) are considered as stable isoelectronic and isostructural analogue of black phosphorous. Their two-dimensional (2D) forms have been just predicted to shown strong thickness-dependent physical properties, and even indirect to direct band gap crossover at the monolayer limit. Here, we demonstrate the synthesis of atomically thin GeSe by direct sonication-assisted exfoliation of bulk microcrystalline powders in solvents. The exfoliated few-layer GeSe sheets characterize high crystallinity with lateral sizes over 100 nm and, importantly, strong resistance aga…
Air-Water Interface-Assisted Synthesis and Charge Transport Characterization of Quasi-2D Polyacetylene Films with Enhanced Electron Mobility via Ring-Opening Polymerization of Pyrrole
Visible-light photocatalyst titanium dioxide (TiO2) was successfully prepared via a novel and facile single-mode microwave assisted synthesis process. In this one-step synthesis, Ti as target material selectively oxides in magnetic field throughout rapid heating, whose process requires less energy consumption and short time. In obtained TiO2, self-doping of Ti3+ was confirmed, which makes TiO2 performed sufficient light absorption in visible region with wavelength above 400 nm. Such Ti3+ self-doped TiO2 exhibits much narrower optical bandgap (2.14 eV) to compare with stoichiometric TiO2 (3.0-3…
Currently, magnetic iron oxide nanoparticles are the only nano-sized magnetic resonance imaging (MRI) contrast agents approved for clinical use, yet commercial manufacturing of these agents has been limited or discontinued. Though there is still widespread demand for these particles both for clinical use and research, they are difficult to obtain commercially, and complicated syntheses make in-house preparation infeasible for most biological research labs or clinics. To make commercial production viable and increase accessibility of these products, it is crucial to develop simple, rapid, and r…
We report here an original single-step process for synthesis and self-organization of gold colloids by simply incorporating gold salts into a solution prepared with Polystyrene (PS) - Polymethylmethacrylate (PMMA) copolymer, thiolated PS and Propylene Glycol Methyl Ether Acetate (PGMEA) as solvent. The spin-coating and annealing of this solution allows then the formation of PS domains. Depending on the polymer concentration of the as-prepared solution, there can be either one or several gold nanoparticles (NPs) per PS domains. For high concentration of gold nanoparticles in PS domains, the cou…
The vapor phase synthesis of two-dimensional transition-metal dichalcogenides (MX2) and their heterostructures is often poorly reproducible and sensitive to uncontrolled environmental humidity. It was recently realized that water vapor can play important roles in the growth of MX2 by reacting with MX2 at high temperature to form volatile metal oxyhydroxide (MOx(OH)y) and hydrogen chalcogenides (H2X) that dramatically change the growth processes. Here we report the controllable synthesis of WS2, MoS2, and their heterostructures using water-assisted chemical vapor transport (CVT). The water vapo…
Submicron core/shell Ti/TiOx photocatalyst is successfully synthesized via single-mode magnetic microwave (SMMW) assisted direct oxidation of planetary ball-milled TiH2. The thickness of TiOx shell including highly concentrated defects such as Ti3+ and/or oxygen vacancies is controllable in the range from 6 to over 18 nm by varying the treatment time in the SMMW assisted reaction. In addition to its quite narrow optical bandgap (1.34-2.69 eV) and efficient visible-light absorption capacity, the submicron Ti/TiOx particle exhibits superior photocatalytic performance towards H2 production from w…
Undoped and Mn-doped ZnS nanocrystals were produced by the microwave-assisted solvothermal method and characterized by X-ray diffraction, photoluminescence spectroscopy and scanning electron microscopy with energy-dispersive X-ray spectroscopy. All samples have the cubic zinc blende structure with the lattice parameter in the range of $a$ = 5.406-5.411 Å, and the average size of crystallites is in the range of 6-9 nm. These nanoparticles agglomerate and form large grains with an average size of up to 180 nm. The photoluminescence of the undoped ZnS sample shows a broad emission band located at…
The scalable synthesis of two-dimensional (2D) hexagonal boron nitride (h-BN) is of great interest for its numerous applications in novel electronic devices. Highly-crystalline h-BN films, with single-crystal sizes up to hundreds of microns, are demonstrated via a novel Ni foam assisted technique reported here for the first time. The nucleation density of h-BN domains can be significantly reduced due to the high boron solubility, as well as the large specific surface area of the Ni foam. The crystalline structure of the h-BN domains is found to be well aligned with, and therefore strongly depe…
In this work we studied the synthesis of BSCCO-2212 superconducting phase associating a quite similar method developed by Pechini (PM) with the microwave-assisted hydrothermal method, MAH. To study the influence of MAH on the properties of BSCCO system, we synthesized two samples by such method. For one sample we used carbonates (CMAH) and for the other one we used nitrates (NMAH) as chemical reagents. We also produced a reference sample (REF) just using carbonates by PM to compare their morphological and superconducting properties. The structural properties of the samples were analyzed by sca…
The general topic of energy is regarded to be one of the most important areas for any research and development activities at the start of the twentyfirst century. Therefore, large research efforts are already based on or will be targeted on the development of clean fuels to replace fossil fuels, the improvement of the existing resources and the discovery of new sustainable energy resources, the establishment of new efficient ways to store sustainable energy, and the replacement of the existing high energy consuming technologies with the more energy efficient ones. The latter concept has result…
The synthesis of Si3N4 nanowires from the reaction of silicon nanoparticles with N2 in the 1200-1440 C temperature range is reported. The nitridation conditions are such that the reaction with nitrogen is favoured by the presence of silicon oxide in the particles and by the active oxidation of silicon without a catalyst. It is shown that the Si to Si3N4 conversion rate depends on the amount of silicon particles used in the experiments and that, in general, the reaction slows down for greater amounts. This trend is explained by particle stacking, which restricts the exchange of gases between th…
The present work deals with the synthesis of crystalline carbon nitride thin films by microwave plasma assisted chemical vapour deposition in N$_2$/CH$_4$ gas mixture. The discharge analysis by optical emission spectroscopy shows that the increase in the N$_2$/CH$_4$ ratio involves an important production of the CN and C$_2$ radicals. In the films X-ray energy dispersion spectroscopy shows that the N/C ratio decreases when the CH$_4$ percentage in N$_2$ increases. Xray diffraction and electron diffraction are used to study the carbon nitride films nature. Scanning electron microscopy shows tha…
The present paper describes in situ preparation of Ni° nanoparticles immobilized on acid activated montmorillonite K10 (Ni°-Mont) by impregnation of Ni(OAc)2 into nanopores of acid activated montmorillonite K10 followed by polyol reduction. Ni° NPs was highly dispersed into the initiated mesopores on the surface or inside swelled-interlayers of the examined clay with average size of 10-20 nm. Acid treatment of montmorillonite was carried out with HCl (4 M) under controlled conditions for generation of the desired pore sizes as a host of Ni° NPs. The prepared Ni°-Mont was used as a highly effic…
Research into developing dual modality probes enabled for magnetic resonance imaging (MRI) and positron emission tomography (PET) has been on the rise recently due to the potential to combine the high resolution of MRI and the high sensitivity of PET. Current synthesis techniques for developing multimodal probes is largely hindered in part by prolonged reaction times during radioisotope incorporation - leading to a weakening of the radioactivity. Along with a time-efficient synthesis, the resulting products must fit within a critical size range (between 20-100nm) to increase blood retention ti…
Simple, yet versatile, methods to functionalize graphene flakes with metal (oxide) nanoparticles are in demand, particularly for the development of advanced catalysts. Herein, based on light-induced electrochemistry, a laser-assisted, continuous, solution route for the simultaneous reduction and modification of graphene oxide with catalytic nanoparticles is reported. Electrochemical graphene oxide (EGO) is used as starting material and electron-hole pair source due to its low degree of oxidation, which imparts structural integrity and an ability to withstand photodegradation. Simply illuminati…
We report a surfactant assisted synthesis of Mn doped ZnO polycrystalline samples showing robust room temperature ferromagnetism as characterized by X-ray diffraction analysis, Transmission Electron Microscopy, Electron Paramagnetic Resonance and DC magnetization mearurements. This surfactant assisted synthesis method, developed by us, is found to be highly reproducible. Further, it can also be extended to the synthesis of other transition metal doped ZnO.
PEG- and PVP-assisted wet-chemical synthesis of ZnS nanocrystals via hydrothermal and co-precipitation methods for route-dependent structural and bandgap tuning
Ghulam Ishaq Khan Institute of Engineering Sciences and Technology（古拉姆·伊沙克汗工程科学与技术学院）；University of Illinois Urbana-Champaign（伊利诺伊大学厄巴纳-香槟分校）
The lanthanide pyrochlore oxides Ln$_2$B$_2$O$_7$ are one of the most intensely studied classes of materials within condensed matter physics, firmly centered as one of the pillars of frustrated magnetism. The extensive chemical diversity of the pyrochlores, coupled with their innate geometric frustration, enables realization of a wide array of exotic and complex magnetic ground states. Thus, the discovery of new pyrochlore compositions has been a persistent theme that continues to drive the field in exciting directions. The recent focus on the mixed B-site pyrochlores offers a unique route tow…
We report on the deposition of gallium oxide using microwave irradiation technique on III nitride epi layers. We also report on the first demonstration of a gallium oxide device, a visible blind deep UV detector, with GaN based heterostructure as the substrate. The film deposited in the solution medium, at less than 200 C, using a metalorganic precursor, was nanocrystalline. XRD confirms that as deposited film when annealed at high temperature turns polycrystalline beta gallium oxide. SEM shows the as deposited film to be uniform, with a surface roughness of 4 to 5 nm, as revealed by AFM. Inte…
Synthesis of large-scale, uniform, easily transferable, and highly crystalline monolayer (1L) molybdenum disulfide (MoS2) on different substrates is a challenge and could decide its suitability for opto-electronic device applications. Herein, we report a facile NaCl-assisted Chemical Vapor Deposition (CVD) synthesis of high-quality MoS2 on amorphous, crystalline and layered substrates. Optical microscopy and Raman spectroscopy show that sapphire and SiO2/Si are suitable substrates for large 1L-MoS2 flakes growth, while mica is excellent for large-area continuous films. Comparatively lesser ful…
The current state-of-the-art thermoelectric materials are generally composed of expensive, scarce, and toxic elements. In this respect, copper-based sulfide compounds have emerged as viable alternatives. Herein, we report for the first time the successful synthesis of single-phase cubic isocubanite CuFe2S3 using mechanical-alloying combined with microwave-assisted synthesis. The isocubanite phase synthesized via this ultra-fast out-of-equilibrium process exhibits a maximum thermoelectric figure of merit, zTmax ~ 0.14 at 673 K. Besides the thermoelectric properties, insights about the structure…
We report on the systematic investigation of the optical properties of a selectively grown quantum dot gain material assisted by block-copolymer lithography for potential applications in active optical devices operating in the wavelength range around 1.55 um and above. We investigated a new type of diblock copolymer PS-b-PDMS (polystyrene-block-polydimethylsiloxane) for the fabrication of silicon oxycarbide hard mask for selective area epitaxy of InAs/InP quantum dots. An array of InAs/InP quantum dots was selectively grown via droplet epitaxy. Our detailed investigation of the quantum dot car…
Kernel Learning Assisted Synthesis Condition Exploration for Ternary Spinel
University of Toronto（多伦多大学）；Acceleration Consortium（加速联盟）；National Research Council Canada（加拿大国家研究委员会）；Clean Energy Innovation Research Center（清洁能源创新研究中心）
Macroscopic fibers of carbon nanotubes (CNT) have emerged as an ideal architecture to exploit the exceptional properties of CNT building blocks in applications ranging from energy storage to reinforcement in structural composites. Controlled synthesis and scalability are amongst the most pressing challenges to further materialize the potential of CNT fibers. This workshows that under floating catalyst chemical vapor conditions in the direct spinning method, used both in research and industry,the ceramic reactor tube plays an unsuspected active role in CNT growth, leading for example to doublin…
