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  • Artigo IPEN-doc 30764
    Correlation between zeta potential and electron paramagnetic resonance of thulium, europium co-doped yttria based suspensions
    2024 - 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 synthesis
    2023 - 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.
  • Resumo IPEN-doc 28642
    Synthesis of thulium-yttria nanoparticles with EPR response
    2021 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.
    Introduction: High dose dosimetry demands a continuous effort towards the development of new materials with the aim to guarantee assurance of activities in which ionizing radiation is used. The present work reports a hydrothermal synthesis based on a relative low temperature and pressure to form thulium-yttria nanoparticles with electron paramagnetic resonance response. Material and method: Thulium-yttria nanoparticles (Tm:Y2O3) prepared with 0.1at.%Tm (atomic percentage, at.%) were synthesized by an eco-friendly hydrothermal process as reported in previous study[1]. The nanoparticles were characterized by Photon Correlation Spectroscopy (PCS), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Electron Paramagnetic Resonance (EPR). Results: According to results, the hydrothermal method provided thulium-yttria nanoparticles with cubic C-type structure, mean particle size (d50) less than 90nm (Fig.1), and EPR response. The EPR spectra of powders exhibited two resonance peaks p1 and p2 recorded at 350 and 160mT, respectively (Fig.2). Conclusions: The enhancement of the EPR response of yttria by the use of thulium as a dopant provide meaningful parameters to advance in the formation of new rare earth based materials for radiation dosimetry.
  • Artigo IPEN-doc 28522
    Microstructure evolution of yttria compacts by powder technology
    2021 - SANTOS, SILAS C.; RODRIGUES JUNIOR, ORLANDO; CAMPOS, LETICIA
    Background: 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 28431
    Colloidal processing of thulium-yttria microceramics
    2022 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.
    The development of new dosimetric materials is essential for the safe and effective use of nuclear technology. In the present study, an eco-friendly bio-prototyping approach was developed for preparing thulium-yttria microceramics with potential applications in radiation dosimetry. Micro-powder compacts were obtained by casting colloidal thulium-yttria suspensions prepared with 20 vol% particles in thin-walled tube templates. Samples were sintered at 1600 °C for 2 h under the environmental pressure and atmosphere to obtain thulium-yttria microceramics with dimensions of 3.33 ± 0.01 mm × 2.27 ± 0.01 mm (height × diameter), as well as a cubic C-type structure, pycnometric density of 4.79 g cm−3 (95.61% theoretical density), and surface microstructure comprising hexagon-like grains bonded at the boundaries. The use of thulium as an activator of yttria greatly improved the electron paramagnetic resonance (EPR) response of the microceramics, where the main EPR peak (p1) was recorded at 351.24 mT and the g factor was 2.0046. The innovative findings obtained in this study may facilitate the production of new solid state dosimeters.
  • Artigo IPEN-doc 27832
    Dispersion of thulium-yttria nanoparticles to build up smart structures
    2021 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.
    The development of new materials for radiation dosimetry is a challenge to assure quality improvement practices related to radiation protection concept. On this context, colloidal stability provides conditions to build up smart structured materials from bottom-up perspective. The present work reports zeta potential characterization of thulium-yttria nanoparticles in aqueous medium. Thulium-yttria nanoparticles formed by a relative low temperature hydrotermal synthesis were characterized by XRD, PCS, and SEM. The stability of particles in aqueous medium was evaluated by electrophoretic mobility measurements, followed by zeta potential calculation. The results revealed that the isoelectric point of thulium-yttria suspensions shifted in accordance with thulium concentration from pH 8.5 (“pure” yttria) to pH 9.2 (2at.%Tm). Besides, most suspensions could be stabilized at pH 10.5, presenting zeta potential values around 30 mV. These results are substantial parameters to advance toward new materials for radiation dosimetry.
  • Artigo IPEN-doc 27736
    Towards a new promising dosimetric material from formation of thulium-yttria nanoparticles with EPR response
    2021 - SANTOS, S.C.; RODRIGUES JUNIOR, O.; CAMPOS, L.L.
    Advances toward new materials for dosimetry application is essential to enhance quality assurance and quality improvement practices based on radiation protection concept. Face to this challenge the present work reports an approach to produce thulium-yttria nanoparticles with electron paramagntic resonance response by an alternative hydrothermal synthesis based on a relative low temperature and pressure. Distinct compositions of thulium-yttria nanoparticles with up to 2 at.%Tm (at.%, atomic percentage) were prepared and characterized by XRD, SEM, PCS, and EPR. The proposed synthesis method followed by thermal treatment of the precursor powder at 1100 ◦C for 2 h provided thulium-yttria nanoparticles with rounded shape, cubic C-type structure, and mean particle size (d50) less than 160 nm. Among all compositions formed, thulium-yttria nanoparticles prepared with 0.1%Tm presented the most remarkable EPR response. The production of fine thulium-yttria nanoparticles with EPR response supply meaningful parameters to advance in the formation of new dosimetry materials based on rare earths.
  • Artigo IPEN-doc 26662
    Formation and EPR response of europium-yttria micro rods
    2019 - SANTOS, SILAS C. dos; RODRIGUES JUNIOR, ORLANDO; CAMPOS, LETICIA L.
    Designing new materials with suitable dose-response efficiency is a great challenge in radiation dosimetry search. Yttria (Y2O3) has excellent optical, mechanical, chemical, and thermal properties. Besides, yttria exhibits crystal characteristics that provide insertion of other rare earths, forming innovative materials. Nevertheless, there are quite few studies on formation, microstructural and EPR response evaluation of yttria. This work reports the formation and EPR characterization of europium-yttria micro rods for radiation dosimetry. Ceramic rods obtained by sintering at 1600ºC/4h in air were exposed to gamma radiation with doses from 1Gy to 150kGy. Particle, microstructural and dosimetry characterizations were performed by PCS, XRD, SEM, OM, and EPR techniques. As sintered europiumyttrium rods exhibited dense microstructure (90% theoretical density) and linear EPR dose response behavior up to 10kGy. These results show that europium-yttria is a promising material for radiation dosimetry.
  • Artigo IPEN-doc 25136
    EPR response of yttria micro rods activated by europium
    2018 - 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 23196
    Bio-prototyping of europium-yttria based rods for radiation dosimetry
    2017 - 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.