Kinetics of thermal decomposition of niobium hydride

High-purity niobium powders can be obtained from the well-known hydride-dehydride (HDH) process. The aim of this work was the investigation of the structural phase transition of the niobium hydride to niobium metal as function of temperature, heating rate and time. The niobium powder used in this work was obtained by high-temperature hydriding of niobium machining chips followed by conventional ball milling and sieving. X-ray diffraction measurements were carried out in vacuum using a high-temperature chamber coupled to an X-ray diffractometer. During the dehydriding process, it is possible to follow the phase transition from niobium hydride to niobium metal starting at about 380 degrees C for a heating rate of 20 degrees C/min. The heating rate was found to be an important parameter, since complete dehydriding was obtained at 490 degrees C for a heating rate of 20 degrees C/min. The higher dehydriding rate was found at 500 degrees C. Results contribute to a better understanding of the kinetics of thermal decomposition of niobium hydride to niobium metal. (C) 2011 Elsevier Ltd. All rights reserved.CNPq (Brazil)CNPq (Brazil

SEM/EDX and XPS studies of niobium after electropolishing

The studies of niobium after electrochemical polishing EP in sulfuric-methanesulfonic acid mixture were performed. The NbOx/Nb surface was studied by SEM/EDX and XPS methods to find out the chemical composition of the oxygen-induced structures. Specifically the XPS results obtained after EP treatment indicate prevailing part of oxygen with niobium oxides on the sample surface. In order to correctly interpret these structures the photoelectron spectra of main niobium oxides were analyzed, and the spectra of internal Nb 3d and O 1s electronic states and valence band spectra were measured for them. (C) 2012 Elsevier B. V. All rights reserved

Kinetics of thermal decomposition of titanium hydride powder using in situ high-temperature X-ray diffraction (HTXRD)

The thermal decomposition of titanium hydride powder (delta-phase) to titanium (alpha-phase) was investigated by means of thermogravimetric analysis (TGA) and high-temperature X-ray diffraction (HTXRD) in high vacuum. The delta-to-alpha phase transformation was followed in situ by HTXRD at temperatures varying from room temperature up to 1000 °C. The transformation was also analyzed as a function of time at isothermal conditions from 450 to 650 °C. The results of TGA show that the decomposition of the titanium hydride becomes significant at about 450 °C. Above 500 °C the decomposition is completed in times shorter than 50 minutes. The apparent activation energy for hydrogen desorption was found to be 63 ± 6 kJ.mol-1

XPS and GDOES characterization of porous coating enriched with copper and calcium obtained on tantalum via plasma electrolytic oxidation

XPS and GDOES characterizations of porous coatings on tantalum after Plasma Electrolytic Oxidation (PEO) at 450 V for 3 minutes in electrolyte containing concentrated (85%) phosphoric acid with calcium nitrate and copper (II) nitrate are described. Based on the obtained data, it may be concluded that the PEO coating consists of tantalum (Ta5+), calcium (Ca2+), copper (Cu2+  and Cu+), and phosphates (). It has to be pointed out that copper and calcium are distributed throughout the volume. The authors also propose a new model of PEO, based on the derivative of GDOES signals with sputtering time

XPS and GDOES Characterization of Porous Coating Enriched with Copper and Calcium Obtained on Tantalum via Plasma Electrolytic Oxidation

XPS and GDOES characterizations of porous coatings on tantalum after Plasma Electrolytic Oxidation (PEO) at 450 V for 3 minutes in electrolyte containing concentrated (85%) phosphoric acid with calcium nitrate and copper (II) nitrate are described. Based on the obtained data, it may be concluded that the PEO coating consists of tantalum (Ta5+), calcium (Ca2+), copper (Cu2+  and Cu+), and phosphates (PO43-). It has to be pointed out that copper and calcium are distributed throughout the volume. The authors also propose a new model of PEO, based on the derivative of GDOES signals with sputtering time

Three-dimensional characterization of pores in Ti-6Al-4V alloy

The direct three-dimensional characterization of opaque materials through serial sectioning makes possible to visualize and better quantify a material microstructure, using classical metallographic techniques coupled with computer-aided reconstruction. Titanium alloys are used as biomaterials for bone implants because of its excellent mechanical properties, biocompatibility and enhanced corrosion resistance. The Ti-6Al-4V alloy (in wt. (%)) with porous microstructure permits the ingrowths of new-bone tissues improving the fixation bone/implant. This is important to understand connectivity, morphology and spatial distribution of pores in microstructure. The Ti-6Al-4V alloy compacts were produced by powder metallurgy and sintered at three distinct temperatures (1250, 1400 and 1500 °C) to obtain distinct microstructures in terms of residual porosity. The visualization of the reconstructed 3D microstructure provides a qualitative and quantitative analysis of the porosity of Ti6Al4V alloy (volume fraction and pore morphology)