SILAS CARDOSO DOS SANTOS
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Artigo IPEN-doc 30764 Correlation between zeta potential and electron paramagnetic resonance of thulium, europium co-doped yttria based suspensions2024 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.The formation of advanced ceramic components with homogeneous microstructure and functional characteristics demands a suitable control of particle dispersion. Thus, the characterization of particle stability as immersed in a liquid medium is important. The present paper reports an approach to evaluate the stability of europium, thulium co-doped yttria (YET) nanoparticles by a correlation between zeta potential and Electron Paramagnetic Resonance (EPR) techniques. Based on results, YET suspensions exhibited high stability apart from pH 10, while their isoelectric point presented a slight variation from pHIEP 8.5 to 9.2 according to thulium content 0 and 2 at.%, respectively. The peak-to-peak amplitude of EPR spectra of the YET suspensions increased as pH shifted toward alkaline condition, following zeta potential curves features. The present achievements are very useful parameters to form stable suspensions based on rare-earth oxides and to advance toward new materials for radiation dosimetry.Artigo IPEN-doc 29900 Building up europium thulium co-doped yttria nanoparticles with electron paramagnetic resonance response by colloidal synthesis2023 - SANTOS, SILAS C. dos; RODRIGUES JR., ORLANDO; CAMPOS, LETICIA L.In the radiation dosimetry field the research for new materials is a continuos demand with the aim to provide highly improvement procedures where ionizing radiation is used. Considering this challenge, the present work reports the colloidal synthesis of europium-thulium-co-doped yttria powders (YET) and evaluates the dopants effect on the promotion of EPR response of yttria. The powdered compositions prepared with up to 2at.%Tm and 2at.%Eu (at.%, atomic percentage) were evaluate by XRD, PCS, SEM, and EPR. Based on the results, the proposed synthesis method provided ceramic powders with cubic C-type form and mean particle size (d50) less than 160nm. The most significant EPR dose-response was noticed for the powdered composition prepared with 0.5at. %Tm (YET0.5) as irradiated with 5kGy (60Co). These findings are key parameters to advance toward the formation of new materials for radiation dosimetry.Artigo IPEN-doc 28522 Microstructure evolution of yttria compacts by powder technology2021 - SANTOS, SILAS C.; RODRIGUES JUNIOR, ORLANDO; CAMPOS, LETICIABackground: Innovation in ceramic materials relies on the processing of powders. Yttria, also known as yttrium oxide, belongs to the rare-earth group (RE2O3 - RE from La to Lu, including Sc and Y). Due to the great properties and end-use of RE-based materials since agriculture until astronomy, studies on processing, sintering and microstructural evolution of RE-based materials are essential to provide new materials with improved characteristics. The aim of this paper is to obtain dense compacts of yttria by powder technology, in which the effect of sintering temperature on sample's microstructure is evaluated. Methods: Yttria powders (Y2O3) were characterized by Photon Correlation Spectroscopy (PCS), X-ray Diffraction (XRD), and Scanning Electron Microscopy (SEM). Cylindrical powder compacts were produced by uniaxial compaction, followed by hydrostatic compaction. Sintered samples obtained under sintering temperatures from 1350 to 1550ºC were evaluated by SEM, XRD, apparent density, and true density. Results: Cubic C-type yttria powders exhibited a mean particle size (d50) of 1.6μm, and morphology like acicular. Powder compacts (diameter x height) of 9.57mm ± 0.01 x 1.53mm ± 0.01 presented mean apparent density of 53.69% (based on free powder density). Sintered samples at 1550ºC exhibited the most densification, 65.0% related to the green density and 91.0% related to theoretical density, respectively. Conclusion: Yttria cylindrical compacts with dense microstructure, and symmetric dimensions were formed by powder technology from powders with a mean particle size of 6.51μm, by compaction methods (uniaxial and hydrostatic), followed by sintering. The most densification of samples was achieved by the sintering condition of 1550ºC for 2h, providing samples with a theoretical density of 91%. These results provide useful subsidies to advance toward full densification of yttria-based materials.Artigo IPEN-doc 25214 Synthesis, processing, and electron paramagnetic resonance response of Y1.98Eu0.02O3 micro rods2018 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.Innovating dosimetric materials, which includes design and development of new dosimetric materials based on rare earth oxides, is challenging. Yttrium oxide (Y2O3) is one of the most important sesquioxides and presents crystal characteristics that enable doping with rare earth ions, making it a promising material for radiation dosimetry. This paper reports on the development and measurement of Electron Paramagnetic Resonance (EPR) signal response for Y1.98Eu0.02O3 micro rods that have undergone facile low-pressure hydrothermal synthesis and bio-prototyping. Assynthesized powders with narrow sub-micrometer particle size distribution with d50 of 584 nm exhibited a reactive surface, which led to the formation of stable aqueous suspensions by controlling the surface charge density of particles through alkaline pH adjustment. Ceramic samples with dense microstructure were formed by sintering at 1600 ºC for 4h at ambient atmosphere. Y1.98Eu0.02O3 micro rods were irradiated using a 60Co source with doses from 1 to 100 kGy, and EPR spectra were measured at room temperature in X-band microwave frequencies. Sintered samples exhibited linearity of the main EPR signal response from 10 Gy to 10 kGy. Supralinearity was observed for higher doses, which is possibly ascribed to formation of more defects. Using europium as a dopant enhanced the EPR signal of yttrium rods remarkably, due to 4f–4f transitions of the Eu3+ ion. These innovative findings make europium-doped yttrium oxide a promising material for radiation dosimetry.Artigo IPEN-doc 25136 EPR response of yttria micro rods activated by europium2018 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.Rare earth (RE) materials present excellent properties, which importance is recognized worldwide. Innovation approaches in energy, medicine, communication, transportation, militarism, and radiation dosimetry consist in RE based materials. As yttrium oxide (Y2O3) exhibits intrinsic lattice characteristics that enable doping with others RE elements (Y2O3:RE), new materials with promising characteristics can be developed. This work aims to evaluate EPR response of europium-yttria (Y2O3:Eu) rods obtained by bio-prototyping. Ceramic rods containing up to 10 at.%Eu were irradiated with gamma doses from 0.001 to 150 kGy and evaluated by Electron Paramagnetic Resonance (EPR) at room temperature with X-band EPR. Based on results, Y2O3:Eu rods with 2 at.%Eu exhibited the most significant response, in which linear behavior arose from 0.001 up to 50 kGy. Fading and thermal annealing evaluations revealed that 2 at%.Eu improved dosimetric characteristics of yttria remarkably. These innovative findings afford that Y2O3:Eu is a promising material for radiation dosimetry.Artigo IPEN-doc 24787 EPR dosimetry of yttria micro rods2018 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.The use of rare earths (RE) as dopant of materials has led the development of advanced materials for many applications such as optical tracers, special alloys, semiconductors, as well as radiation dosimeters. The development of new dosimetric materials based on REs is a great challenge in innovation of materials. Yttria (Y2O3) presents luminescent proprieties and is a promising material for radiation dosimetry. The present paper aims to evaluate paramagnetic defects of Y2O3 rods obtained via bio-prototyping by using Electron Paramagnetic Resonance (EPR) technique at room temperature. Ceramic rods were irradiated with gamma doses from 0.001 to 150 kGy and evaluated by EPR at room temperature with X-band EPR. According to EPR results, as sintered samples exhibited an EPR signal with principal g tensor of 2.020 and maximum line width around 2.3 mT, which is ascribed to interstitial oxygen ion. Dose response behaviour exhibited two distinct dose ranges, one is from 1 to 100Gy and the second is from 0.1 to 70 kGy. Thermal annealing approaches reveal that defect centres of yttria decay significantly at high temperature. These innovative results make Y2O3 a promising material for radiation dosimetry.Artigo IPEN-doc 24415 Advances in colloidal processing of rare earth particles2018 - SANTOS, SILAS C.; RODRIGUES, ORLANDO; CAMPOS, LETICIA L.Abstract: Background: New insights into materials science provide development of smart nano/micro structured materials for advanced applications. Rare earth includes a set of chemical elements (from La to Lu, including Sc and Y) with unique properties, the use of which is evidenced by luminescence applications. Colloidal processing offers great possibilities to obtain smart materials by controlling inter-particle forces, as well as their evolution during ceramic processing. The present article reports a review on colloidal processing with emphasis on rare earth powders. A general view about rare earths properties, including scientific investigations and applications are also presented. Methods: General view on rare earth sources, classification, properties, studies, and applications are reported. Besides, a review on colloidal processing covering particle characteristics, inter- particle forces, dispersion methods, rheology of suspensions, shaping process, drying-sintering stage, and microstructure formation is reported. Results: Yttria is the most used rare earth oxide in phosphors applications (70%). Synthesis routes imply on powder properties. Particle characteristics as size, shape, density, and surface area are important parameters for colloidal processing. The control of inter- particle forces by zeta potential evaluation and using dispersion methods provide conditions to prepare stable suspensions. Consolidation of colloidal particles into a desired shape depends on both viscosity and rheological behavior of suspensions. Drying-sintering conditions are effective on microstructure formation and component characteristics. Bio-prototyping is a low cost method, which provides components with complex shape and cellular architecture. Conclusion: Rare earths exhibit remarkable properties, being applied in diverse technological end-use. Colloidal processing provides opportunities to form smart materials since synthesis of colloids until development of complex ceramic components by shaping methods and thermal treatment. Even though colloidal processing is quite mature, investigations on rare earths involving inter- particle forces, shaping, drying-sintering stage, and microstructure formation are very scarce.Artigo IPEN-doc 23196 Bio-prototyping of europium-yttria based rods for radiation dosimetry2017 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.The application of solid state dosimeters in radiation protection has grown significantly as consequence of advances in the development of dosimetric materials using rare earths. The conception of new dosimetric materials concerns synthesis methods, which control the evolution of material structure, including further processing steps as, shaping, drying, and sintering. The present study reports a full bio-prototyping approach to produce europium doped yttria rods with potential application in radiation dosimetry. Ceramic particles synthesized by hydrothermal route were characterized by Photon Correlation Spectroscopy (PCS), X-ray diffraction (XRD), and Scanning Electron Microscopy (SEM). The effect of europium on promoting electronic defects in yttria host was evaluated by Electron Paramagnetic Resonance (EPR). Low pressure hydrothermal synthesis led to formation of rounded particles with mean diameter of 410 nm. Aqueous suspensions with 20 vol% of particles prepared at pH 10, and 0.2 wt% binder exhibited apparent viscosity of 213 mPa s, being suitable for bio-prototyping of rods. Sintering of shaped samples at 1600 degrees C for 4 h provided formation of dense ceramic rods. Europium-yttria rods containing 5 at.% Eu exhibited the most intense EPR response.Artigo IPEN-doc 22838 Processing, microstructure and thermoluminescence response of biomorphic yttrium oxide ceramics2016 - SANTOS, S.C.; YAMAGATA, C.; CAMPOS, L.L.; MELLO-CASTANHO, S.R.H.The present work reports a fast-direct bio-prototyping process using Luffa Cylindrica vegetable sponge to produce biomorphic yttrium oxide ceramics with reticulated-porous architecture and thermoluminescence response. Processing parameters as rheology of yttrium oxide suspensions, bio-template surface treatment and thermal decomposition of bio-template were investigated. Shear thinning suspensions of 30 vol% yttrium oxide with apparent viscosity of 243mPa.s provided a successful impregnation of samples, whereby bio-templates with smooth ceramic layer and hierarchical reticulated architecture were formed. By thermal treatment at 1600 degrees C for 2 h biomorphic yttrium oxide ceramics with porous microstructure and TL response at 150 degrees C and lambda=550 nm were produced. The proposed fast direct bio-prototyping process is suitable for the production of ceramic components with complex shape and demonstrates potential for general applicability to any bio-template. (C) 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.