CLAUDIO JOSE DA ROCHA
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Resumo IPEN-doc 26833 Mechanical activation of TiFe for hydrogen storage2019 - LEAL NETO, RICARDO M.; VEGA, LUIS E.R.; FALCÃO, RAILSON B.; LEIVA, DANIEL R.; ROCHA, CLAUDIO J.; ISHIKAWA, TOMAZ T.; KIMINAMI, CLAUDIO S.; BOTTA, WALTER J.The aim of this work is to report some recent developments on the synthesis of TiFe by high energy ball milling and cold rolling, concerning hydrogen storage. Ball-milled TiFe was produced by two procedures, both under inert atmosphere and with various milling times. In the first one a powder mixture of TiH2 an Fe was milled, followed by a vacuum heat treatment to promote the reaction synthesis of TiFe compound [1]. Second procedure consisted of milling Ti and Fe powders with stearic acid (as a process control agent) after a pre-milling operation (with the same powders and without PCA) to prepare the surface of milling media. Both methods were conceived for avoiding strong adherence of the powders to the milling balls and vial, impairing the mechanical alloying. Cold rolling was performed on a ground TiFe ingot produced by arc melting [2]. After 20 to 40 passes under inert atmosphere, powder particles and thin cracked flakes were produced. Results showed that both milling procedures succeeded in avoiding unacceptable adherence to the milling media, with high loose powder yields. Whatever the route, nanostructured TiFe was obtained with no need of further thermal activation for the first hydrogenation. Hydrogen absorption capacities of about 1.0 wt% at room temperature was obtained with both milling procedures. Higher capacity (1.4wt%) was obtained with cold rolled TiFe (powder and flakes) after 40 passes. Some possible explanations for this difference are presented and discussed.Artigo IPEN-doc 25090 An alternative route to produce easily activated nanocrystalline TiFe powder2018 - FALCAO, R.B.; DAMMANN, EDGAR D.C.C.; ROCHA, C.J.; DURAZZO, M.; ICHIKAWA, R.U.; MARTINEZ, L.G.; BOTTA, W.J.; LEAL NETO, R.M.In this paper, an alternative process route to produce active nanocrystalline TiFe compound was investigated. First, TiH2 and Fe powders were dry co-milled in a planetary ball mill for 5e40 h. TiH2 was selected as precursor powder, instead of Ti powder, due its fragility, which has proved to be beneficial to decrease powders adherence on milling tools. In terms of loose powder mass, milling yields ranged from 90 to 95 wt.%. Next, milled powders were post-heated at 873 K under dynamic high-vacuum for TiFe synthesis reaction. First hydrogen absorption was verified in situ during the cooling process of samples (until the room temperature), being the amount of hydrogen absorbed and desorbed by this samples measured by automated Sievert's apparatus, under constant hydrogen flow rate of 9 cm3. min-1 (dynamic measurements). Besides to allowing the first absorption in situ, the investigated process route also allowed the production of the non-stoichiometric TiFe compound (rich in Ti) in samples milled for shorter times (5 and 10 h), both characteristics associated with maintaining the mechanical compound activity. Each sample absorbed hydrogen at 2 MPa during the cooling process, requiring no additional thermal activation cycles, since the samples milled for shorter times (mainly for 10 h) could absorb hydrogen for the first time more easily. However, the samples milled for longer times (25 and 40 h) shown better results in terms of reversible and storage capacities (0.73 and 0.94 wt.%, respectively).