RODRIGO UCHIDA ICHIKAWA

RODRIGO UCHIDA ICHIKAWA

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Thickness estimation of TiO2-based nanotubes using X-ray diffraction techniques
2020 - FARIA, MARCELA E.M.; LEITE, MARINA M.; ICHIKAWA, RODRIGO U.; VICHI, FLAVIO M.; TURRILLAS, X.; MARTINEZ, L.G.
TiO2-based nanotubes are a very promising material with many applications in solar cells, biomedical devices, gas sensors, hydrogen generation, supercapacitors, and lithium batteries, among others. Nanotube thickness is a very important property since it is related to electronic and surface mechanics. In this sense, transmission electron microscopy (TEM) can be used. However, it can be difficult to acquire a good TEM image because the transversal section of the nanotubes needs to be visible. In this work, TiO2-based nanotubes obtained via hydrothermal synthesis were studied using X-ray line profile analysis. Scherrer and Single-Line methods provided consistent results for the thickness of the nanotubes (≃ 5 nm) when compared with TEM. Additionally, Single-Line method was also applied to estimate the microstrain. The advantage of using XRD is given by the fact that it is a quick and statistically significant analysis when compared with TEM. The results show that XRD can be used as a rapid and reliable alternative for the thickness estimation of nanotubes.
Characterization of nanostructured Mn-Zn ferrites synthesized by coprecipitation method using CTAB
2020 - MARANHAO, W.C.A.; ICHIKAWA, R.U.; TURRILLAS, X.; YOSHITO, W.K.; SAEKI, M.J.; ORLANDO, M.T.D.; MARTINEZ, L.G.
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.
In situ hydration of sulfoaluminate cement mixtures monitored by synchrotron X-Ray diffraction
2018 - ROSSETTO, CLEUSA M.; ICHIKAWA, RODRIGO U.; MARTINEZ, LUIS G.; CAREZZATO, GERALDO L.; CARVALHO, ALEXANDRE M.G.; TURRILLAS, XAVIER
Mixtures of calcium sulfoaluminate and Portland clinkers with gypsum were hydrated with deionized water. The pastes were introduced in 0.7 mm borosilicate capillary tubes and kept at 40 ºC while diffraction patterns were collected every 35 s for approximately 3 hours with a monochromatic radiation of 12 keV at the XRD1 beamline of the Laboratório Nacional de Luz Síncrotron (LNLS) in Campinas, SP - Brazil. The main crystalline phases (C2S, C3S, ettringite, ye’elemite and gypsum) involved in the hydration were quantified by Rietveld analysis. The most noticeable fact was the absence of portlandite as a crystalline precipitate, most likely due to the capture of calcium ions to form ettringite.
Characterization of Mn0.67Zn0.33Fe2O4 nanoparticles synthesized under different pH
2017 - ICHIKAWA, RODRIGO U.; YOSHITO, WALTER K.; SAEKI, MARGARIDA J.; MARANHAO, WILLIAN C.A.; GOULART, FATIMA; MARTINEZ, LUIS G.
Nanostructured Mn-Zn ferrites were synthesized using co-precipitation in alkaline solution with different pH. The samples were characterized using X-ray diffraction (XRD), X-ray fluorescence (XRF), thermal analysis (TG-DTA), dynamic light scattering (DLS) and scanning electron microscopy (SEM) techniques. Monophasic nanoparticles were formed when synthesized with pH 10.5. This sample was heat-treated and its XRD data was refined by the Rietveld method. Mean crystallite sizes and microstrains were determined from X-ray line profile analysis using Single-Line and Warren-Averbach methods, which revealed a mean crystallite size of approximately 10 nm and negligible microstrains. Zn content was estimated using refined cell parameters, giving a value of 33 at %, in accordance with XRF result. TG-DTA revealed that the incorporation of α-Fe2O3 occurs around 1130 °C and 1200 °C with recrystallization of the Mn-Zn ferrite spinel phase. DLS showed that mean particle size increase with temperature up to 1159 nm at 800 °C. SEM analysis showed the samples agglomerate and present similar morphology with negligible size changing when calcined between 280 °C and 800 °C. However, the sample calcined at 1200 °C presents larger agglomerates due to the sintering process.
Synthesis of TiFe compound from ball milled TiHsub(2) and Fe powders mixtures
2014 - FALCAO, RAILSON B.; DAMMANN, EDGAR D.C.C.; ROCHA, CLAUDIO J. da; ICHIKAWA, RODRIGO U.; DURAZZO, MICHELANGELO; MARTINEZ, LUIS G.; LEAL NETO, RICARDO M.
TiFe compound was produced by high-energy ball milling of TiH2 and Fe powders, followed by heating under vacuum. TiH2 was used instead of Ti in order to avoid the strong particles adhesion to grinding balls and vial walls. Mixtures of TiH2 and Fe powders were drymilled in a planetary mill for times ranging from 5 to 40 hours. The amount of sample, number and diameter of the balls were kept constant in all experiments. After milling, samples were heated under dynamic high-vacuum for the synthesis reaction. As-milled and heat-treated materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analysis (DTA). The mean crystallite sizes and microstrains were determined by XRD line profile analysis using the Warren-Averbach method. As-milled materials presented only Fe and TiH2 phases. Nanostructured TiFe compound was formed after heat treatment. TiH2 was effective for providing low adherence of the powders during milling.