Neodymium iron boron magnets (NdFeB) play a critical role in various technological applications due to their outstanding magnetic properties, such as high maximum energy product, high remanence and high coercivity. Production of NdFeB is expected to rise significantly in the coming years, for this reason, demand for the rare earth elements (REE) will not only remain high but it also will increase even more. The recovery of rare earth elements has become essential to satisfy this demand in recent years. In the present study rare earth elements recovery from NdFeB magnets as new promising process flowsheet is proposed as follows; (1) acid baking process is performed to decompose the NdFeB magnet to increase in the extraction efficiency for Nd, Pr, and Dy. (2) Iron was removed from the leach liquor during hydrolysis. (3) The production of REE-oxide from leach liquor using ultrasonic spray pyrolysis method. Recovery of mixed REE-oxide from NdFeB magnets via ultrasonic spray pyrolysis method between 700 °C and 1000 °C is a new innovative step in comparison to traditional combination of precipitation with sodium carbonate and thermal decomposition of rare earth carbonate at 850 °C. The synthesized mixed REE- oxide powders were characterized by X-ray diffraction analysis (XRD). Morphological properties and phase content of mixed REE- oxide were revealed by scanning electron microscopy (SEM) and Energy-dispersive X-ray (EDX) analysis. To obtain the size and particle size distribution of REE-oxide, a search algorithm based on an image-processing technique was executed in MATLAB. The obtained particles are spherical with sizes between 362 and 540 nm. The experimental values of the particle sizes of REE- oxide were compared with theoretically predicted ones.

Nanostructured zinc oxide (ZnO) particles were synthesized by the one step Ultrasonic Spray Pyrolysis (USP) process from nitrate salt solution (Zn(NO₃)₂·6H₂O). Various influential parameters, from Zn(NO₃)₂·6H₂O concentrations (0.01875–0.0375 M) in the initial solution, carrier gas (N₂) flow rates (0.5–0.75 L/min) to reaction temperature (400–800 °C), were tested to investigate their role on the final ZnO particles’ morphology. For this purpose, Scanning Electron Microscopy (SEM), High Resolution Transmission Electron Microscopy (HRTEM) and (Selected Area Electron Diffraction) SAED techniques were used to gain insight into how the ZnO morphology is dependent on the USP process. It was revealed that, by certain parameter selection, different ZnO morphology could be achieved, from spherical to sphere-like structures assembled by interwoven nanoplate and nanoplate ZnO particles. Further, a more detailed crystallographic investigation was performed by XRD and Williamson-Hall (W-H) analysis on the ZnO with unique and non-typical planar morphology that was not reported before by USP synthesis. Moreover, for the first time, a flexible USP formation model was proposed, ending up in various ZnO morphologies rather than only ideal spheres, which is highly promising to target a wide application area.

Yttrium oxide (Y₂O₃) particles were synthesised from a yttrium nitrate solution via ultrasonic spray pyrolysis (USP) method. The effects of temperature and precursor concentration on morphology and microstructural parameters were investigated. Y₂O₃ particles were characterised by scanning-electron-microscope energy-dispersive spectroscopy, Raman spectroscopy and X-ray diffraction analysis. Based on X-ray peak broadening, the crystallite size was calculated using the modified Debye–Scherrer (MDS) method. Furthermore, the crystallite size, crystal strain and the energy density of the crystal were evaluated using the Williamson–Hall (W–H) analysis integrated with the uniform deformation model, the uniform stress deformation model and the uniform deformation energy density model. A comparative evaluation of Y₂O₃ crystallite size using the MDS and W–H methods was carried out. This is part of a thematic issue on Nanoscale Materials Characterisation and Modeling by Advances Microscopy Methods - EUROMAT.

Due to their remarkable magnetic properties, such as a high maximum energy product, high remanence, and high coercivity, NdFeB magnets are used in a variety of technological applications. Because of their very limited recycling, high numbers of spent NdFeB magnets are widely available in the market. In addition to China’s monopoly on the supply of most rare earth elements, there is a need for the recovery of these critical metals, as their high import price poses an economic and environmental challenge for manufacturers. This paper proposes a pyrometallurgical recycling method for end-of-life NdFeB magnets by oxidizing them in air as first required step. The main goal of this method is to oxidize rare earth elements from NdFeB magnets in order to prepare them for the carbothermic reduction. The experimental conditions, such as the oxidation temperature and time, were studied in order to establish the phase transformation during oxidation using the Factsage Database and experimental conditions. Our thermogravimetric analysis TGA analysis revealed an increased sample mass by 35% between room temperature and 1100 °C, which is very close to the total calculated theoretical value of oxygen (36.8% for all elements, and only 3.6% for rare earth elements REE), confirming the complete oxidation of the material. The obtained quantitative analysis of the oxidation product, in (%), demonstrated values of 53.41 Fe₂O₃, 10.37 Fe₃O₄; 16.45 NdFeO₃; 0.45 Nd₂O₃, 1.28 Dy₂O₃, 1.07 Pr₂O₃, and 5.22 α-Fe.

Nanoparticle properties are correlated to their size, size distribution, and shape; it is essential to accurately measure these features in the field of nanoscience. In this study, silver nanoparticles (AgNPs) were synthesized with the ultrasonic-spray-pyrolysis (USP) method from a water solution of silver nitrate. The synthesized AgNPs were characterized by Dynamic Light Scattering (DLS) analysis and Scanning Electron Microscopy (SEM) to reveal their size and size distribution. A search algorithm based on an image-processing technique to obtain particle size and particle-size distribution from SEM micrographs is proposed. In order to obtain more quantitative information and data with respect to the morphology of particles synthesized under different process parameters, SEM micrographs with a nonhomogeneous background contrast were examined via image-processing techniques in MATLAB. Due to the inhomogeneous contrast of SEM micrographs, defining an overall threshold value was insufficient in the detection of whole nanoparticles. Thus, subimages were directly created according to the maximum and minimum particle size specified by the user to determine local threshold values. The obtained results were automatically combined to represent both particle dimension and location in the SEM micrographs. We confirmed that the results of our DLS analysis, theoretical calculation, and image-processing technique were correlated with our expected results.