Dilson Silva dos Santos

Mg alloy for hydrogen storage processed by SPD

Abstract Mg-based nanocomposites are promising candidates for hydrogen storage applications exhibiting fast H-sorption kinetics at reasonably low temperatures when processed by high-energy ball milling techniques. However, since compaction of the highly reactive nanometric powder is desirable before application, the search for other effective processing routes for the preparation of Mg-based nanocomposites is relevant. In this work, we have used a combination of equal channel angular pressing, cold rolling and high-energy ball milling in the processing of the commercial AZ31 extruded alloy to evaluate its use as a hydrogen storage material. Severe plastic deformation carried out at different temperatures, combined with further mechanical processing resulted in a controlled texture and signifiant grain refinement, which are desirable microstructural characteristics for hydrogen storage applications.

Mechanical and Reactive Milling of a TiCrV BCC Solid Solution

Nowadays, many efforts have been concentrated in research and development of hydrogen absorbing materials due to a possible application as electrode for rechargeable batteries, on board hydrogen storage systems, getters, catalysts, etc. Novel technologies for materials processing have been used to generate new alloys with metastable structures, such as amorphous and/or nanocrystalline alloys. In this context, mechanical milling or mechanical alloying is a very attractive way to produce this alloys, specially when carried out under hydrogen atmosphere (reactive milling). In this work, we have studied the structural evolution of a TiCrV bcc solid solution during mechanical and reactive milling. The process parameters analyzed were: milling atmosphere (argon and hydrogen), milling time and gas pressure into the vials (in the case of reactive milling). Structural evolution was investigated by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM). Hydrogen contents of the reactive milled alloys were determined using a Leco analyzer. Differential scanning calorimetry (DSC) was used to determine the hydrogen desorption temperature and the stability of the alloys.

Hydrogen Diffusivity and Hydride Formation in Rich-Zirconium Alloys Used in Nuclear Reactors

Hydrogen gas permeation tests were performed on two Nb-modified Zr alloys used in the nuclear industry. The influence of the microstructure on hydrogen diffusivity in each alloy is discussed and a mechanism of hydride formation is presented. The hydrogen binding energy for different trap sites was calculated in the M5 alloy as well as hydrogen diffusivity value in the Zirlo alloy at 300oC, D = 2.5 x 10-13 m2/s.

Hydrogen Absorption Study of Ti-based Alloys Performed by Melt-spinning

The hydrogen absorption and desorption of Ti53Zr27Ni20 icosahedral quasicrystal (ICQ) and Ti50Ni50 shape memory alloy (SMA) melt-spun ribbons was studied. Samples were exposed to hydrogen gas at 623 K and 4 MPa for 1000 minutes. The total capacity of hydrogen obtained for Ti53Zr27Ni20 and Ti50Ni50 was 3.2 and 2.4 wt. % respectively. The Thermal Desorption Spectrometry (TDS) of the hydrogenated alloys shows that both alloys start to desorb hydrogen around 750 K. X-ray diffraction (XRD) patterns, performed after hydrogenation, indicate a complete amorphization of the Ti53Zr27Ni20 i-phase alloy, while the Ti50Ni50 alloy remained crystalline after hydride formation.

Hydrogen absorption/desorption properties in the TiCrV based alloys

Three different Ti-based alloys with bcc structure and Laves phase were studied. The TiCr1.1V0.9, TiCr1.1V0.45Nb0.45 and TiCr1.1V0.9 + 4%Zr7Ni10 alloys were melted in arc furnace under argon atmosphere. The hydrogen absorption capacity was measured by using aparatus type Sieverts. Crystal structures, and the lattice parameters were determined by using X-ray diffraction, XRD. Microestructural analysis was performed by scanning electron microscope, SEM and electron dispersive X-ray, EDS. The hydrogen storage capacity attained a value of 3.6 wt. (%) for TiCr1.1V0.9 alloy in a time of 9 minutes, 3.3 wt. (%) for TiCr1.1V0.45Nb0.45 alloy in a time of 7 minutes and 3.6 wt. (%) TiCr1.1V0.9 + 4%Zr7Ni10 with an increase of the hydrogen absorption kinetics attained in 2 minutes. This indicates that the addition of Nb and 4%Zr7Ni10 to the TiCrV alloy acts as catalysts to accelerate the hydrogen absorption kinetics.

The effect of TTNT nanotubes on hydrogen sorption using MgH2

-TTNT composite, respectively. The Differential Scanning Calorimetry (DSC) examination provided some evidence with the shifting of the peaks obtained when the amount of TTNT is increased. The hydrogen absorption/desorption kinetics tests showed that the TTNT nanotubes can enhance hydrogen sorption effectively and the total hydrogen capacity obtained was 6.5 wt. (%).

Hydrogen Trap on the Microstructure of Cr-Mo Type Steels

Microstructure influence on hydrogen trapping in a Cr-Mo type steels −2.25Cr 1Mo and 2.25Cr 1Mo 0.25V− was studied by means of electrochemical permeation test, thermal desorption spectrometry, scanning and transmission electron microscopy analysis. Both steels, used in hydrogenation reactors, in as received and artificial aged conditions exhibit a bainitic microstructure with CrxMoy and CrxMoyVz carbides finely dispersed. The hydrogen diffusivity for the 2.25Cr-1Mo-0.25V is lower than 2.25Cr-1Mo due to its higher carbide precipitation. At aged conditions TDS on samples cathodically charged with hydrogen showed an increase on the hydrogen trapping capacity for 2.25Cr-1Mo and a reduction for the vanadium modified steel, compared with the as-received state.

Effects of the Microstructure on the Hydrogen Diffusivity in Ni-Based Superalloy 718

In some applications involving aggressive environments, common in oil and gas industries, superalloys 718 may suffer hydrogen embrittlement, resulting in degradation of mechanical properties. The aim of this work is to study the interaction of hydrogen with different microstructures in a 1 mm thick plate, annealed and age hardened superalloy 718. In this way, the effects of hydrogen interaction on microstructure were studied via thermal programmed desorption (TPD), tensile tests and scanning electron microscopy (SEM). Samples were studied in as-received, artificially aged and overaged conditions. Hydrogenated samples submitted to tensile tests presented ductility loss when compared to hydrogen free samples, showing the hydrogen embrittlement sensitivity of this alloy. The influence of  phase precipitation on hydrogen diffusivity, as a result of aging treatment, was also discussed in this work.

Characterization of amorphous Nb oxide and its influence on Mg hydrogen sorption

Abstract Amorphous Nb2O5 was synthesized by combining niobium ethoxide with an amine surfactant. The material turned out to have a high surface area, 287 m2 g−1, and a homogeneous structure. The material was shown to be amorphous despite the heat treatment performed within a range of 150 to 550°C. The surface area of Nb2O5 reduced to 105 m2 g−1 after heat treating at 350°C. The activation energy of the Nb2O5 crystallization reaction was found to be 327 kJ mol−1. The surface area of Nb2O5 reduced significantly with heat treatment but it still improved the hydrogen kinetics since the desorption rate was 1.5 wt.% min−1. The addition of a small amount of amorphous Nb2O5 to magnesium hydride, throughout milling, helped overcoming limitations inherent to solid hydrogen storage.

Mechanical Alloying of Zr-Nb5%at. Powders: Microstructural Evolution and Hydrogenation Properties

Zircaloy is commonly applied as structural element in nuclear reactors owing to the gamma radiation transparency of Zr. One of the research interests in Zr-Nb alloys is related to its behavior in H2O-rich environments due to hydrogen embrittlement. In the present work the microstructural evolution (crystallite size and microhardness), crystallography and hydrogenation behavior (after milling) due to mechanical alloying (MA) are studied for the Zr-Nb5%at and pure Zr. The MA study of Zr and the Zr-Nb system showed that frequency of rotation in a planetary mill and alloy composition play a major role on the evolution of crystallite size and microhardness. Nb addition was found to induce a partial allotropic transformation of the Zr structure (α→ω) during MA. Indeed, for milling experiments with significant Fe contamination the formation of an fcc phase was observed. Further, MA for extended times (over 5 hours) was found to reduce the hydrogen absorption capacity of Zr and the Zr-Nb system studied.