Navegação por autor "TURRILLAS, X."

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  • IPEN-DOC 27404

    MARANHAO, W.C.A. ; ICHIKAWA, R.U. ; TURRILLAS, X.; YOSHITO, W.K. ; SAEKI, M.J.; ORLANDO, M.T.D.; MARTINEZ, L.G. . Characterization of nanostructured Mn-Zn ferrites synthesized by coprecipitation method using CTAB. Materials Science Forum, v. 1012, p. 207-211, 2020. DOI: 10.4028/www.scientific.net/MSF.1012.207

    Abstract: In this work it was investigated the influence of CTAB surfactant concentration on the synthesis of the compound Mn0.75Zn0.25Fe2O4 by the coprecipitation method. It was also compared the influence of hydrothermal treatment on the synthesized materials. The magnetic properties were characterized by AC susceptometry for the determination of the magnetic susceptibility and magnetic density energy. The phases, crystal structure and morphology of the nanoferrites were determined by Rietveld analysis of X-ray diffraction data. It was found the presence of two phases: Franklinite and Akaganeite and it was shown that the samples synthesized only by coprecipitation presented the tendency to increasing the crystallite sizes of the akaganeite phase and decreasing of crystallite sizes of the Franklinite phase as a function of CTAB concentration. The samples submitted to subsequent hydrothermal treatment presented a tendency to decreasing the crystallite sizes of both phases and increasing in Franklinite phase fraction, compared to the samples synthesized only by coprecipitation, suggesting that the hydrothermal treatment was effective in obtaining nanostructured materials of smaller particles.

    Palavras-Chave: ferrites; manganese; zinc; nanostructures; manganese carbides; zinc oxides; coprecipitation; hydrothermal synthesis; x-ray diffraction; calculation methods

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  • IPEN-DOC 20628

    ICHIKAWA, R.U. ; MARTINEZ, L.G. ; IMAKUMA, K. ; TURRILLAS, X.. Development of a methodology for the application of the Warren-Averbach method. In: WORKSHOP OF APPLIED CRYSTALLOGRAPHY TO MATERIALS SCIENCE AND ENGINEERING, 4th, May 23-25, 2014, Vitoria, ES. Proceedings... 2014.

    Palavras-Chave: polycrystals; size; strains; algorithms; programming; fourier analysis; x-ray diffraction

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  • IPEN-DOC 17974

    MARTINEZ, L.G. ; GALVAO, A.S.A.; ROSSI, J.L. ; ORLANDO, M.T.D.; TURRILLAS, X.; CORREA, H.P.S.. Development of standard reference materials for powder diffraction. In: INTERNATIONAL LATIN-AMERICAN CONFERENCE ON POWDER TECHNOLOGY, 8th, November 6-9, 2011, Florianopolis, SC. Abstract... 2011. p. 2286.

    Palavras-Chave: powders; diffraction; calibration standards; synchrotron radiation; wavelengths; sample preparation

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  • IPEN-DOC 25103

    ICHIKAWA, R.U. ; LINHARES, H.S.M.D.; PERAL, I.; BALDOCHI, S.L. ; RANIERI, I.M. ; TURRILLAS, X.; MARTINEZ, L.G. . Evidence for a core–shell configuration in Tb-doped KY3F10 nanoparticles using synchrotron x-ray line profile and pair distribution function analyses. Materials Research Express, v. 5, n. 1, 2018. DOI: 10.1088/2053-1591/aaa0bc

    Abstract: The microstructure of Tb-doped KY3F10 nanoparticles synthesized by coprecipitation was analysed using x-ray synchrotron diffraction data. Size-strain analysis was performed by means of x-ray line profile (XLPA) methods such as Warren–Averbach and whole powder pattern modelling. Additionally, the structural coherence of the sample was accessed using pair distribution function analysis, supporting the XLPA results. The combination of all methods revealed that the nanoparticles exhibit a more ordered core and a less ordered surface comprising a core–shell configuration.

    Palavras-Chave: nanoparticles; terbium; doped materials; x-ray diffraction; pair production; pairing interactions; distribution functions; yttrium fluorides; configuration; shell models

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  • IPEN-DOC 23620

    ROSSETTO, C.M.; ICHIKAWA, R.U. ; MARTINEZ, L.G. ; CAREZZATO, G.L. ; CARVALHO, A.M.; TURRILLAS, X. . In situ hydration of sulphoaluminate cement mixtures monitored by synchrotron X-ray diffraction. In: CONGRESSO BRASILEIRO DE ENGENHARIA E CIENCIA DOS MATERIAIS, 22., 06-10 de novembro, 2016, Natal, RN. Abstract... 2016. p. 1801.

    Abstract: The hydration of calcium sulphoaluminate cement mixtures was studied in situ by synchrotron X-ray diffraction at the XRD1 beamline of the Laboratório Nacional de Luz Síncrotron (LNLS – Campinas). The specimens were analyzed in borosilicate glass capillary tubes of 0.7 mm and imbued with deionized water. As the hydration reaction is very fast, the data collection was started after two minutes of mixing with water. The X-ray wavelength chosen to get an adequate flux for these short time acquisitions was 1.033258 Å, determined with a corundum standard. Diffraction patterns were collected every 35 seconds at temperatures ranging from 40°C to 55°C with accuracy better than 0.1°C attained with a hot air blower. The diffracted signal was collected with an array of 24 Mythen detectors. The diffraction patterns accumulated had appropriate statistics to determine the kinetics of the reaction either by quantitative Rietveld analysis or by fitting isolated diffraction peaks to Gaussian curves as a function of time. The most important phases involved in the hydration are Klein´s salt, also known as Ye’elimite, Ca4(AlO2)6SO4, and gypsum, CaSO4.2H2O to yield Ettringite, Ca6Al2(SO4)3(OH)12·26H2O, phase responsible for the mechanical properties. These studies show the potential of XRD1 beamline to investigate at controlled temperatures in situ fast reactions involving crystalline phases with time resolutions inferior to one minute, which is ideal for the hydration of cementitious mixtures.

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  • IPEN-DOC 23619

    TURRILLAS, X.; MARTINEZ, L.G. ; ROSSETTO, C.M.; ICHIKAWA, R.U. ; CARVALHO, A.M.; CAREZZATO, G.L. . In situ hydration of sulphoaluminate cement mixtures monitored by synchrotron X-ray diffraction. In: CONGRESSO BRASILEIRO DE ENGENHARIA E CIENCIA DOS MATERIAIS, 22., 06-10 de novembro, 2016, Natal, RN. Abstract... 2016. p. 1800.

    Abstract: The hydration of calcium sulpho-aluminate cement mixtures was studied in situ by synchrotron X-ray diffraction at the XRD1 beamline of the Laboratório Nacional de Luz Síncrotron (LNLS) in Campinas, SP. The powder specimens were introduced in borosilicate glass capillary tubes of 0.7 mm of internal diameter and imbued with deionized water. As the hydration reaction is very fast the capillaries were placed on the goniometer and the data collection was started after two minutes of mixing with water. The X-ray energy chosen to get an adequate flux for these short time acquisitions was 12 keV or more precisely 1.033258 Å, determined with polycrystalline corundum standard. Diffraction patterns were collected sequentially every 35 seconds for several hours at temperatures ranging from 40 degC to 55 degC with an accuracy better than 0.1 degC attained with the help of a hot air blower. The diffracted signal was collected with an array of twenty-four Mythen detectors at 760 mm from the capillary tube. The diffraction patterns had appropriate statistics to determine the kinetics of the reaction either by quantitative Rietveld analysis or by fitting isolated diffraction peaks to Gaussian curves as a function of time. The most important phases involved in the hydration are Klein´s salt, also known as Ye’elimite, Ca4(AlO2)6SO4, and gypsum, CaSO4.2H2O to yield Ettringite, Ca6Al2(SO4)3(OH)12·26H2O, phase responsible for the mechanical properties.

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  • IPEN-DOC 24500

    ICHIKAWA, R.U. ; PARRA, J.P.R.L.L.; VALLCORBA, O.; PERAL, I.; YOSHITO, W.K. ; SAEKI, M.J.; TURRILLAS, X.; MARTINEZ, L.G. . Mn-Zn ferrite nanoparticles probed by synchrotron pair distribution function analysis and anomalous X-ray scattering. In: RAU ANNUAL USERS MEETING LNLS/CNPEM, 27th, November 22-24, 2017, Campinas, SP. Abstract... 2017. p. 99-99.

    Abstract: Among the numerous applications of Mn1-xZnxFe2O4 nanoparticles we can highlight biomedical applications as magnetic tracer in Alternate Current Biosusceptometry (ACB), Magnetic Resonance Imaging (MRI), for diagnosis of cancer and others diseases as diabetes and Parkinson, whose severity can be monitored by analyzing the disturbances of the gastrointestinal motility [1,2]. Specifically, the former (ACB) method is promising because of its low cost, it is non-invasive method and because it can be conducted without ionizing radiation. Major advances have been achieved by developing a bionanocomposite based on ferrites for the theranostics [3] as well, of breast cancer, by carrying drugs or hyperthermia. Recently, we reported that Mn0.75Zn0.25Fe2.8O4 nanoparticles with different surface charge can be produced precipitating them by NaOH with different concentrations [2]. This behavior is observed if an excess of Iron is introduced to the ferrite. Five samples precipitated with different NaOH concentrations were analyzed by X-ray synchrotron diffraction (XRD) which revealed a less crystalline phase contribution alongside the main peaks of the cubic spinel ferrite phase. Pair Distribution Function (PDF) analysis was used to probe the local structure and showed that Fe-Fe, Mn-Mn and Zn-Zn bond distances in the 3.0 up to 3.5 Å range are different from the ones usually reported in the literature. Lastly, for the sample with best magnetic behavior anomalous X-ray scattering (AXS) using three energies close to the absorption edges of Mn, Zn and Fe was applied to determine its cation distribution complementing the previous result from PDF analysis.

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  • IPEN-DOC 21597

    FERREIRA, E.G.A.; VICENTE, R. ; TURRILLAS, X.; VOKAICHIYA, F.; FRANCO, M. ; MARTINEZ, L.G. ; MARUMO, J.T. . Portland cement paste behaviour under gamma radiation field in geological repository. In: WASTE MANAGEMENT CONFERENCE, March 15-19, 2015, Phoenix, USA. Abstract... 2015.

    Palavras-Chave: portland cement; gamma radiation; sealed sources; waste management; x-ray diffraction; irradiation procedures; geologic deposits; radioisotopes

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  • IPEN-DOC 20764

    ICHIKAWA, R.U. ; MARTINEZ, L.G. ; IMAKUMA, K. ; LINHARES, H.M.S.M.D. ; RANIERI, I.M. ; TURRILLAS, X.. Size-strain analysis in RE-doped KY3F10 fluorides using X-ray line profile analysis. In: WORKSHOP OF APPLIED CRYSTALLOGRAPHY TO MATERIALS SCIENCE AND ENGINEERING, 4th, May 23-25, 2014, Vitoria, ES. Anais... 2014.

    Palavras-Chave: nanostructures; rare earths; doped materials; ytterbium fluorides; strains; x-ray diffraction

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  • IPEN-DOC 21606

    ICHIKAWA, R.U. ; PARRA, J.P.R.L.L.; MARTINS, M.L.; YOSHITO, W.K. ; SAEKI, M.J.; TURRILLAS, X.; MARTINEZ, L.G. . Size-strain analysis of nanostructured Mn-Zn ferrites using x-ray line profile methods. In: SIZE-STRAIN CONFERENCE DIFFRACTION ANALYSIS OF THE MICROSTRUCTURE OF MATERIALS, 7th, September 21-24, 2015, Oxford, UK. Abstract... 2015.

    Palavras-Chave: nanostructures; magnetic materials; ferrites; manganese; zinc; magnetic properties; nmr imaging; contrast media

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  • IPEN-DOC 22319

    ICHIKAWA, R.U. ; MARTINEZ, L.G. ; IMAKUMA, K. ; TURRILLAS, X.; GUSATTI, M.; RIELLA, H.G.. Size-strain x-ray line profile analysis and crystallite size distribution of nanostructured ZnO. In: TALLER DE LA ASSICIACION ARGENTINA DE CRISTALOGRAFIA, 2.; REUNION ANUAL DE LA ASSOCIACION ARGENTINA DE CRYSTALOGRAFIA, 9.; REUNION LATINOAMERICANA DE CRISTALOGRAFIA, 1., 28 de octubre - 1 novembre, 2013, Cordoba, Argentina. Proceedings... 2013.

    Palavras-Chave: corrections; nanostructures; zinc oxides; x-ray diffraction; calibration standards; size; strains; distribution

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  • IPEN-DOC 21594

    ICHIKAWA, R.U. ; LINHARES, H.M.S.M.D. ; RANIERI, I.M. ; TURRILLAS, X.; MARTINEZ, L.G. . Structural and microstructural analysis of luminescent Tb:KY3F10 nanophosphor using X-ray synchrotron diffraction. In: PSI SUMMER SCHOOL ON CONDENSED MATTER RESEARCH, 14th, August 15-21, 2015, Zuoz, Switzerland. Abstract... 2015.

    Palavras-Chave: structural chemical analysis; microstructure; luminescence; x-ray diffraction; phosphors; nanomaterials; doped materials; potassium compounds; yttrium fluorides; terbium

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  • IPEN-DOC 21605

    MARTINEZ, L.G. ; ICHIKAWA, R.U. ; TURRILLAS, X.. Study of a highly crystalline Y2O3 sample by Rietveld and Pair Distribution Function Analysis. In: ANNUAL USERS MEETING, 25th, September 16-17, 2015, Campinas, SP. Abstract... 2015. p. 54.

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  • IPEN-DOC 24487

    ROSSETTO, C.M.; MARTINEZ, L.G. ; ICHIKAWA, R.U. ; CAREZZATO, G.L. ; CARVALHO, A.M.G.; TURRILLAS, X.. Study of hydration of sulphoaluminate cement by in situ synchrotron diffraction. In: RAU ANNUAL USERS MEETING LNLS/CNPEM, November 22-24, 2017, Campinas, SP. Abstract... 2017. p. 135-135.

    Abstract: The hydration of calcium sulphoaluminate cement mixtures was studied in situ by synchrotron X-ray diffraction at the XRD1 beamline at the Laboratório Nacional de Luz Síncrotron (LNLS – Campinas). The specimens were analyzed in borosilicate glass capillary tubes of 0.7 mm and imbued with deionized water. As the hydration reaction is very fast, the data collection was started after two minutes of mixing with water. The Xray wavelength chosen to get an adequate flux for these short time acquisitions was 1.033258 Å (12 keV), determined with a corundum standard. Diffraction patterns were collected every 35 seconds at temperatures ranging from 40 °C to 55 °C with accuracy better than 0.1 °C attained with a hot air blower. The diffracted signal was collected with an array of 24 Mythen detectors [1]. The diffraction patterns accumulated had appropriate statistics to determine the kinetics of the reaction either by quantitative Rietveld analysis or by fitting isolated diffraction peaks to Gaussian curves as a function of time. The most important phases involved in the hydration are Klein´s salt, also known as Ye’elimite, Ca4(AlO2)6SO4, and gypsum, CaSO4.2H2O to yield Ettringite, Ca6Al2(SO4)3(OH)12·26H2O, phase responsible for the mechanical properties. These studies show the potential of XRD1 beamline to investigate at controlled temperatures in situ fast reactions involving crystalline phases with time resolutions inferior to one minute, which is ideal for the hydration of cementitious mixtures. The series of diffraction patterns collected for one and half hour are shown in Figure 1(a) and (b). In Figure 1(c) the evolution of the relative proportions of crystalline phases can be seen. Non-crystalline phases such as CSH gel or Al(OH)3 (gibbsite) are not taken in consideration [2]. The figures clearly show that the ettringite formation happens in two stages, the second one starting after approximately forty minutes. It is also interesting to notice that this stages seem to coincide with the depletion of Ca2SiO4 (C2S) for the first stage and the depletion of Ca3SiO5 (C3S) for the second one.

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  • IPEN-DOC 27006

    GOULART, F. ; ICHIKAWA, R.U. ; TURRILLAS, X.; MARTINEZ, L.G. . Study on the microstructure of UNS S32304 duplex steel submitted to heat-treatments. In: ENCONTRO CIENTÍFICO DE FÍSICA APLICADA, 8., 4-7 de setembro, 2017, Vitória, ES. Anais... São Paulo, SP: Blucher Proceedings, 2017. p. 45-48. DOI: 10.5151/phypro-viii-efa-12

    Abstract: Duplex stainless steels are characterized by a good combination of mechanical properties and corrosion resistance. Due to the metastable equilibrium between the ferritic (α) and austenitic (γ) phases, significant changes in the microstructure of these steels may occur when subjected to temperatures higher than the ambient, degrading their properties. In this work, it was investigated the influence of heat treatments on the microstructure and mechanical properties of a duplex stainless steel UNS-S32304. The heat-treatments were performed at four temperatures (300°C, 600°C, 900°C and 1000°C) with two treatment times (1 h and 6 h) and two processes of cooling down (in air and water). The samples were studied by X-ray diffraction using Pawley method to determine the lattice parameters, mean crystallite sizes and microstrain for the two phases and compared to Vickers microhardness results.

    Palavras-Chave: microstructure; stainless steels; microhardness; vickers hardness

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  • IPEN-DOC 22321

    MARTINEZ, L.G. ; ICHIKAWA, R.U. ; IMAKUMA, K. ; ORLANDO, M.T.D.; TURRILLAS, X.. Synchrotron diffraction characterization of alternative powder diffraction standards. In: ENCONTRO CIENTÍFICO DE FÍSICA APLICADA, 5., 25-28 de maio, 2014, Domingos Martins, ES. Anais... 2014.

    Palavras-Chave: comparative evaluations; calibration standards; powders; diffraction; synchrotrons; x-ray diffraction; heat; oxides; silicon

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  • IPEN-DOC 23790

    COUTO, C.P.; COSTA, P.D.O.L.; MARTINEZ, L.G. ; TURRILLAS, X. ; ROSSI, J.L. . The use of X-ray diffraction for phase identification of press hardened steels. In: WORKSHOP OF APPLIED CRYSTALLOGRAPHY TO MATERIALS SCIENCE AND ENGINEERING, 6th, 13-15 de maio, 2015, Vitória, ES. Proceedings... São Paulo: Blucher Proceedings, 2015.

    Abstract: The numbers of hot stamped components have been steadily increasing in the automotive industry. Press hardened steels are generally used in hot stamping process since at the end of the process, the steel may achieve a tensile strength about 1500 MPa. The hot stamping process consists to heat the steel blank at total austenitization temperature and to transfer the blank into the press tooling for shaping and fast cooling to fully martensitic transformation. The transfer of the blank from the furnace to the press might promote at some extent, steel oxidation. The application of metallic coatings avoids this hindrance. The Al-Si has been the most applied coating on steel. In parallel, alternative coatings such as Zn-Ni have been developed. It is known that the heating causes chemical elements diffusion, which results in intermetallic formation between the elements presents in the coating and in the substrate. This study had the objective of characterizing hot stamped and coated 25MnB5 steel samples with Al-Si and Zn-Ni, with X rays diffraction (XRD) technique. Some literature suggested phases such as Zn-Fe, Zn-Ni-Fe or Al-Fe-Si were not seen on XRD results. Nonetheless, X-ray diffraction detected the presence of ZnO and α-Fe for Zn-Ni coated steel plate and Al5Fe2, AlFe3 and α-Fe for the Al-Si coated steel plate.

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  • IPEN-DOC 24432

    CAREZZATO, G.L. ; COUTO, C.P. ; ROSSI, J.L. ; MARTINEZ, L.G. ; TURRILLAS, X.. A versatile setup in reflection mode for in situ diffraction patterns acquisition from flat polycrystalline specimens bathed in a liquid medium. In: RAU ANNUAL USERS MEETING LNLS/CNPEM, November 22-24, 2017, Campinas, SP. Abstract... 2017. p. 50-50.

    Abstract: A cell to perform in situ diffraction measurements of specimens regularly immersed in a liquid medium has been developed. The assembly (see Fig. 1) has been adapted to work in beamline XRD2 in reflection mode. Basically consists of a polypropylene box with two windows made of poliimide to allow the passage of X-rays (incident and diffracted) at lower angles. The flat sample is placed in the middle of the box that is on top of the goniometer head. For safety reasons the central box is positioned over a tray to avoid spillage of liquid. On the bottom of the cell there is a connection to the pipe linked to the syringe. The syringe is driven by a beamline stepping motor. This way it is easy to synchronise the filling and evacuation of liquid from the cell with the actual data acquisition of diffraction patterns. The idea is to soak the flat specimen with the liquid and then remove it to acquire the diffraction data. This can be done in a sequential way for several hours to monitor the crystalline phases present on the surface (or rather a few microns deep) of the flat specimen. Various reactions can be investigated this way, provided that the sample is flat. Ceramics, metals, and polymers in contact with liquids could be studied. Preliminary tests have been performed in two theta – theta geometry on metal plates in contact with acid solutions to simulate accelerated corrosion. However a large variety of experiments with other geometries, (grazing incidence) could be carried out and of course this assembly could be used on SIRIUS with better time resolution.

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  • IPEN-DOC 25848

    ICHIKAWA, R.U. ; LINHARES, H.M.S.M.D.; SILVA, A.S.B. da ; TEIXEIRA, M.I. ; RANIERI, I.M. ; TURRILLAS, X.; MARTINEZ, L.G. . X-ray diffraction analysis of KY3F10 nanoparticles doped with Nd and preliminary studies for its use in high-dose radiation dosimetry. Brazilian Journal of Radiation Sciences, v. 7, n. 2A, p. 1-13, 2019. DOI: 10.15392/bjrs.v7i2A.586

    Abstract: In this work, the structure and microstructure of Nd:KY3F10 nanoparticles was probed using X-ray synchrotron diffraction analysis. Rietveld refinement was applied to obtain cell parameters, atomic positions and atomic dis-placement factors to be compared with the ones found in literature. X-ray line profile methods were applied to determine mean crystallite size and crystallite size distribution. Thermoluminescent (TL) emission curves were measured for different radiation doses, from 0.10 kGy up to 10.0 kGy. Dose-response curves were obtained by area integration beneath the peaks from TL. The reproducibility of the results in this work has shown that this material can be considered a good dosimetric material.

    Palavras-Chave: nanoparticles; x-ray diffraction; radiation doses; doped materials; thermoluminescence; neodymium; yttrium fluorides; critical size; dose-response relationships; dosimetry

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Operando, inicialmente como uma base de dados referencial o Repositório foi disponibilizado na atual plataforma, em junho de 2015. No Repositório está disponível o acesso ao conteúdo digital de artigos de periódicos, eventos, nacionais e internacionais, livros, capítulos, dissertações, teses e relatórios técnicos.

A elaboração do projeto do RI do IPEN foi iniciado em novembro de 2013, colocado em operação interna em julho de 2014 e disponibilizado na Internet em junho de 2015. Utiliza o software livre Dspace, desenvolvido pelo Massachusetts Institute of Technology (MIT). Para descrição dos metadados adota o padrão Dublin Core. É compatível com o Protocolo de Arquivos Abertos (OAI) permitindo interoperabilidade com repositórios de âmbito nacional e internacional.

O gerenciamento do Repositório está a cargo da Biblioteca do IPEN. Constam neste RI, até o presente momento 20.950 itens que tanto podem ser artigos de periódicos ou de eventos nacionais e internacionais, dissertações e teses, livros, capítulo de livros e relatórios técnicos. Para participar do RI-IPEN é necessário que pelo menos um dos autores tenha vínculo acadêmico ou funcional com o Instituto. Nesta primeira etapa de funcionamento do RI, a coleta das publicações é realizada periodicamente pela equipe da Biblioteca do IPEN, extraindo os dados das bases internacionais tais como a Web of Science, Scopus, INIS, SciElo além de verificar o Currículo Lattes. O RI-IPEN apresenta também um aspecto inovador no seu funcionamento. Por meio de metadados específicos ele está vinculado ao sistema de gerenciamento das atividades do Plano Diretor anual do IPEN (SIGEPI). Com o objetivo de fornecer dados numéricos para a elaboração dos indicadores da Produção Cientifica Institucional, disponibiliza uma tabela estatística registrando em tempo real a inserção de novos itens. Foi criado um metadado que contém um número único para cada integrante da comunidade científica do IPEN. Esse metadado se transformou em um filtro que ao ser acionado apresenta todos os trabalhos de um determinado autor independente das variáveis na forma de citação do seu nome.