The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering.En este trabajo se han estudiado los cambios microestructurales que se producen durante el tratamiento térmico de las ferritas de cobre-níquel-cinc y se ha analizado el proceso de precipitación de los dos tipos de cristales que aparecen durante el proceso de sinterización. Se ha encontrado que este proceso depende de la densidad relativa en seco de las muestras compactadas y de las siguientes variables de la etapa de sinterización: temperatura y tiempo de sinterización y velocidad de enfriamiento. La caracterización de los cristales precipitados se ha realizado por microscopía electrónica de barrido (MEB), microanálisis por dispersión de energía de rayos X (EDX), difracción de rayos X (DRX), y espectroscopía de fotoelectrones de rayos X (XPS). Estas técnicas han permitido determinar la naturaleza de estos cristales, que en este caso corresponden a los óxidos de cinc y de cobre. Se han propuesto dos reacciones químicas que permiten explicar el proceso de precipitación y la posterior re-disolución de estos cristales precipitados durante la sinterización de las muestras

Thermal cycle for obtaining a Ni-Zn ferrite: (II) Influence of the cooling stage

Las piezas cerámicas obtenidas a partir de polvos de ferritas de composición (Cu0.12Ni0.23Zn0.65)Fe2O4 destacan como absorbentes de radiación electromagnética entre las ferritas de Ni-Zn dopadas con Cu, impidiendo interferencias entre dispositivos electrónicos. En un trabajo previo se estableció la metodología para diseñar la etapa de sinterización de un ciclo térmico que permite obtener las piezas cerámicas mencionadas con una microestructura adecuada (elevada densidad relativa y escaso crecimiento de grano) para que presenten unas buenas propiedades electromagnéticas. En este trabajo se ha estudiado la etapa de enfriamiento del mismo ciclo térmico (etapa siguiente a la de sinterización), determinando la influencia que ejerce la velocidad de enfriamiento sobre la densidad relativa en cocido, el tamaño medio de grano y la distribución de tamaños de grano, variando el tiempo de sinterización del ciclo térmico empleadoCeramic bodies formed from (Cu0.12Ni0.23Zn0.65)Fe2O4 ferrite powders stand out as electromagnetic radiation absorbers among Cu-doped Ni-Zn ferrites, preventing interference between electronic devices. In a preliminary study, a methodology was established for designing the sintering stage of a thermal cycle, which allows the foregoing ceramic bodies to be obtained with the appropriate microstructure (high relative density and little grain growth) to provide them with good electromagnetic properties. The present study examines the cooling stage (i.e. the stage following the sintering stage) of that thermal cycle and the influence of the cooling rate on fired relative density, average grain size, and grain size distribution, varying the sintering time of the thermal cycle use

El proceso de secado por atomización: formación de gránulos y cinética de secado de gotas

Spray drying is a unit operation very common in many industrial processes. For each particular application, the resulting granulated material must possess determined properties that depend on the conditions in which the spray drying processing has been carried out, and whose dependence must be known in order to optimize the quality of the material obtained. The large number of variables that influence on the processes of matter and energy transfer and on the formation of granular material has required a detailed analysis of the drying process. Over the years there have been many studies on the spray drying processing of all kind of materials and the influence of process variables on the drying kinetics of the granulated material properties obtained. This article lists the most important works published for both the spray drying processing and the drying of individual droplets, as well as studies aimed at modeling the drying kinetics of drops.El proceso de secado por atomización es una operación unitaria que interviene en numerosas aplicaciones industriales. Para cada aplicación en concreto, el material granulado resultante debe poseer unas propiedades determinadas que dependen de las condiciones en las que se lleve a cabo el secado por atomización, y cuya dependencia debe conocerse para así optimizar la calidad del material obtenido. El gran número de variables que influyen en los procesos de transferencia de materia y energía que tienen lugar, y en la formación del material granulado, han hecho necesario el análisis en detalle del proceso de secado. A lo largo de los años han sido muchos los estudios realizados sobre el secado por atomización y la influencia de las variables del proceso en la cinética de secado y las propiedades del material granulado obtenido, para todo tipo de materiales. En este artículo se recogen los trabajos más importantes publicados correspondientes tanto al secado por atomización como al secado de gotas individuales, así como los estudios cuyo objetivo es el modelado de la cinética de secado de gotas

Characterization of silica–water nanofluids dispersed with an ultrasound probe: A study of their physical properties and stability

The stability and agglomeration state of nanofluids are key parameters for their use in different applications. Silica nanofluids were prepared by dispersing the nanoparticles in distilled water using an ultrasonic probe, which has proved to be the most effective system and gives the best results when compared with previous works. Results were obtained concerning the influence of the solid content, pH and salt concentration on the zeta potential, electrical double layer, viscosity, elastic and viscous moduli, particle size and light backscattering. Measurement of all these properties provides information about the colloidal state of nanofluids. The most important variable is the solid content. Despite the agglomeration due to high concentration, nanofluids with low viscosity and behaving like liquid were prepared at 20% of mass load thanks to the good dispersion achieved with the ultrasonic treatment. The pH of the medium can be used to control the stability, since the nanofluids are more stable under basic conditions far from the isoelectric point (IEP) and settle at pH = 2. Therefore, stable nanofluids for at least 48 h, with high solid content, can be prepared at high pH value (pH > 7) due to the electrostatic repulsion between particles

Thermal cycle for obtaining a Ni-Zn ferrite: (I) Design of the sintering stage

Las piezas cerámicas obtenidas a partir de polvos de ferritas de composición (Cu0.12Ni0.23Zn0.65)Fe2O4 destacan como absorbentes de radiación electromagnética entre las ferritas de Ni-Zn dopadas con Cu, impidiendo interferencias entre dispositivos electrónicos. En este trabajo se ha establecido una metodología para diseñar la etapa de sinterización de un ciclo térmico, que permite obtener las piezas cerámicas mencionadas con una microestructura adecuada (elevada densidad relativa y escaso crecimiento de grano) para que presenten unas buenas propiedades electromagnéticas. La metodología establecida consiste, en primer lugar, en determinar las ecuaciones diferenciales que relacionan las velocidades de densificación y de crecimiento de grano con el tamaño medio de grano, la densidad relativa y la temperatura de sinterización, proponiendo en cada caso el mecanismo de difusión controlante de cada una de dichas velocidades. En segundo lugar, la integración simultánea de las dos ecuaciones de velocidad permite obtener la evolución de la densidad relativa y del tamaño medio de grano con el tiempo de sinterización a una temperatura previamente fijada. En tercer lugar, se ha determinado cómo dicha temperatura debe ir disminuyendo con el tiempo de sinterización para que, en cada instante, se mantenga una velocidad de densificación relativamente alta evitando al mismo tiempo que la velocidad de crecimiento de grano provoque un crecimiento irregular y exagerado de los mismosCeramic bodies formed from (Cu0.12Ni0.23Zn0.65)Fe2O4 ferrite powders stand out as electromagnetic radiation absorbers among Cu-doped Ni-Zn ferrites, preventing interference between electronic devices. This study establishes a methodology for designing the sintering stage of a thermal cycle, which allows the foregoing ceramic bodies to be obtained with the appropriate microstructure (high relative density and little grain growth) to provide them with good electromagnetic properties. The methodology consists, first, of determining the differential equations that relate the densification and grain-growth rates to average grain size, relative density, and sintering temperature, proposing the corresponding rate-controlling mass-transfer mechanism in each case. Secondly, the simultaneous integration of the two rate equations allows the evolution of relative density and average grain size with sintering time at a prefixed sintering temperature to be obtained. Thirdly, it is determined how this temperature needs to decrease with sintering time in order constantly to maintain a relatively high densification rate, while concurrently keeping the grain-growth rate from causing irregular and/or exaggerated grain growt

Microstructure and mechanical properties of grains of silica nanofluids dried in an acoustic levitator

The microstructure and mechanical properties of spray-dried grains are key factors in many applications. In this work single droplets of silica nanofluids were dried in an acoustic levitator under different experimental conditions of solid mass fraction, pH value, salt concentration, drying temperature and initial droplet volume. ANOVA method was used to determine their influence on the final grain diameter, the shell thickness and the mechanical strength. The solid content and the droplet volume are the variables that exert an influence on these three properties. In addition, the mechanical strength is influenced by the pH value. The maximum packing fraction of the particles inside the shell was obtained by modeling the viscosity data with the Quemada equation. The packing fraction was then used to calculate the shell thickness. The internal microstructure of the grains was observed by SEM and the shell thickness was measured. Experimental and calculated results show good agreemen

Frequency dispersion model of the complex permeability of soft ferrites in the microwave frequency range

The complex permeability of Cu-doped nickel-zinc polycrystalline ferrites is strongly dependent on microstructure, particularly, on relative density (urn:x-wiley:00027820:media:jace18267:jace18267-math-0001) and average grain size (urn:x-wiley:00027820:media:jace18267:jace18267-math-0002). In this study, a mathematical model, able to fit the measured magnetic permeability spectra from 106 to 109 Hz, is proposed and validated for a width range of average grain sizes (3.40–23.15 μm) and relative densities (0.83–0.96). To the authors’ knowledge, domain-wall motion and spin rotation contributions to magnetic permeability have been integrated jointly with the microstructure for the first time in the proposed model, highlighting the relative influence of each magnetizing mechanism and microstructure on the magnetic permeability at different angular frequencies.Funding for open access charge: CRUE-Universitat Jaume

Modeling of Drying Curves of Silica Nanofluid Droplets Dried in an Acoustic Levitator Using the Reaction Engineering Approach (REA) Model

The use of nanoparticles has become of great interest in different industrial applications. The spray drying of nanofluids forms nanostructured grains, preserving the nanoparticle properties. In this work, individual droplets of silica nanofluids were dried in an acoustic levitator. Tests were carried out under different experimental conditions to study the influence of the variables on the drying process. The drying curves were experimentally obtained and an REA model was used to obtain the theoretical curves and the correlations for the activation energy. The critical moisture content theoretically obtained was used to predict the grain diameter

Influence of Particle Size on the Drying Kinetics of Single Droplets Containing Mixtures of Nanoparticles and Microparticles: Modeling and Pilot-Scale Validation

The particle size of the primary particles is an important parameter influencing the drying behavior of droplets. In this work, the influence of particle size on the drying kinetics and grain properties was analyzed for droplets containing silica nanoparticles, microparticles, and mixtures of the two. The presence of microparticles was found to increase the drying rate and shrinkage of the droplet. The drying curves were modeled using a reaction engineering approach (REA) model. Finally, different suspensions were dried in a pilot-scale spray dryer in order to prove the influence of the particle size obtained in the levitator tests

Microwave-assisted digestion of ceramic frits for boron and lithium determination by inductively coupled plasma spectrometry (ICP-OES)

Boron and lithium are two elements commonly found in the chemical composition of ceramic frits. They are usually determined by volumetric titration and atomic absorption spectrometry, respectively, after melting the ceramic frit by high-temperature alkaline fusion and dissolving the melt in acid medium. This dissolution procedure is long and tedious, and does not enable determining both elements simultaneously. An alternative ceramic frit dissolution procedure based on microwave-assisted digestion in acid medium has been proposed, which allows jointly determining boron and lithium by inductively coupled plasma-optical emission spectrometry. This procedure is rapid and reproducible, and the results are independent of frit chemical composition