Hydrogen-Induced Phase Separation of Palladium-Rhodium Alloys Using an Environmental Cell TEM

1997 ◽  
Vol 3 (S2) ◽  
pp. 591-592
Author(s):  
D.F. Teter ◽  
R.D. Field ◽  
D.J. Thoma

The palladium-rhodium system has been extensively studied for its hydrogen absorption characteristics. However, the phase diagram of the palladium-rhodium system has not been conclusively determined below 800 K. Shield and Williams have experimentally determined the incoherent miscibility gap in Pd-Rh alloys using electrical resistivity studies, however the coherent miscibility gap and spinodal have not been determined. Recently work by Noh and Flanagan has suggested that hydrogen enhances metal atom mobility and may increase the kinetics of phase separation in Pd-Rh alloys. Field and Thoma found that hydrogen causes a Pd-10%Rh alloy to decompose during an in situhydrogen charging experiment in an environmental cell TEM. According to the calculations by Gonis et al. of the miscibility gap for the palladium-rhodium system, the Pd-10%Rh alloy may be within the chemical spinodal at room temperature.In this work, two palladium-rhodium compositions were investigated. The first was a Pd-10 at.% Rh alloy produced by melt-spinning, and the second was a Pd-30at.%Rh alloy which had been arc-melted and cold rolled followed by an annealing treatment to homogenize the material. TEM specimens were prepared by punching 3 mm disks from the material.

2014 ◽  
Vol 1645 ◽  
Author(s):  
Romain VAUCHY ◽  
Renaud.C. BELIN ◽  
Anne-Charlotte ROBISSON ◽  
Fiqiri HODAJ

ABSTRACTUranium-plutonium mixed oxides incorporating high amounts of plutonium are considered for future nuclear reactors. For plutonium content higher than 20%, a phase separation occurs, depending on the temperature and on the oxygen stoichiometry. This phase separation phenomenon is still not precisely described, especially at high plutonium content. Here, using an original in situ fast X-ray diffraction device dedicated to radioactive materials, we evidenced a phase separation occurring during rapid cooling from 1773 K to room temperature at the rate of 0.05 and 2 K per second for a (U0.55Pu0.45)O2-x compound under a reducing atmosphere. The results show that the cooling rate does not impact the lattice parameters of the obtained phases at room temperature but their fraction. In addition to their obvious fundamental interest, these results are of utmost importance in the prospect of using uranium-plutonium mixed oxides with high plutonium content as nuclear fuels.


Author(s):  
J. Drucker ◽  
R. Sharma ◽  
J. Kouvetakis ◽  
K.H.J. Weiss

Patterning of metals is a key element in the fabrication of integrated microelectronics. For circuit repair and engineering changes constructive lithography, writing techniques, based on electron, ion or photon beam-induced decomposition of precursor molecule and its deposition on top of a structure have gained wide acceptance Recently, scanning probe techniques have been used for line drawing and wire growth of W on a silicon substrate for quantum effect devices. The kinetics of electron beam induced W deposition from WF6 gas has been studied by adsorbing the gas on SiO2 surface and measuring the growth in a TEM for various exposure times. Our environmental cell allows us to control not only electron exposure time but also the gas pressure flow and the temperature. We have studied the growth kinetics of Au Chemical vapor deposition (CVD), in situ, at different temperatures with/without the electron beam on highly clean Si surfaces in an environmental cell fitted inside a TEM column.


2011 ◽  
Vol 347-353 ◽  
pp. 3420-3424
Author(s):  
Yang Huan Zhang ◽  
Xiao Gang Liu ◽  
Le Le Chen ◽  
Hui Ping Ren ◽  
Guo Fang Zhang ◽  
...  

The nanocrystalline and amorphous Mg2Ni-type Mg20Ni10-xMnx (x = 0, 1, 2, 3, 4) alloys were synthesized by melt-spinning technique. The structures of the as-cast and spun alloys were characterized by XRD, SEM and HRTEM. The hydrogen absorption and desorption kinetics of the alloys were measured. The results show that the substitution of Mn for Ni, instead of changing the major phase Mg2Ni, leads to the formation of Mg and MnNi phases. No amorphous phase is detected in the as-spun Mn-free alloy, but the as-spun alloys substituted by Mn display the presence of an amorphous phase, suggesting that the substitution of Mn for Ni enhances the glass forming ability of the Mg2Ni-type alloy. The hydrogen absorption capacity of the as-cast alloys first increases and then decreases with the variation of the amount of Mn substitution. The hydrogen desorption capacity of the alloys markedly increases with growing Mn content.


2016 ◽  
Vol 8 (23) ◽  
pp. 14548-14551 ◽  
Author(s):  
Tengfei Zhang ◽  
Yuki Nakagawa ◽  
Takenobu Wakasugi ◽  
Shigehito Isobe ◽  
Yongming Wang ◽  
...  

2018 ◽  
Vol 921 ◽  
pp. 231-235
Author(s):  
Ke Bin Sun ◽  
Yan Feng Li ◽  
Ye Xin Jiang ◽  
Guo Jie Huang ◽  
Xue Shuai Li ◽  
...  

Copper foils with 91% cold rolled deformation annealed at temperature between 140°C and 170 °C.The microstructures were observed by EBSD. The mechanical properties were measured at room temperature by tensile test machine and the fracture morphologies observed by SEM. After annealed at 150 °C, recrystallization begins to occur, while the elongation increases evidently and tensile strength decreases sharply. When the temperature rises to 170 °C, recrystallization is complete and the grain starts to grow. When the foils are annealed at 140 °C, it exhibits a strong cold rolling textures characterized by Brass {011}<211> and Cu {112}<111>. After annealed at 170 °C, there are olny weak Brass {011}<211> texture.


1982 ◽  
Vol 21 ◽  
Author(s):  
S. S. Brenner ◽  
P. P. Camus ◽  
M. K. Miller ◽  
W. A. Soffa

Continuous phase separation or spinodal decomposition occurs within a miscibility gap through the selective amplification of long wavelength concentration waves to produce a two-phase modulated microstructure. To comprehensively study the formation of these modulated microstructures and the kinetics of continuous phase separation the behavior of the composition fluctuations in the decomposing material should be monitored directly. The atom probe field-ion microscope is an ideal instrument for this type of investigation of fine-scale microstructures because of its ultra-high spatial resolution and microchemical analysis capability.


1999 ◽  
Vol 77 (5-6) ◽  
pp. 550-556 ◽  
Author(s):  
Andrew P Munro ◽  
D Lyn H. Williams

TheS-nitrosothiols 2-acetamido-2-deoxy-S-nitroso-1-thio-β-D-glucopyranose 3,4,6-triacetate (GPSNO) and S-nitroso-N-carbamyl-D,L-penicillamine (SNCP) were synthesized by S-nitrosation of the corresponding thiols, isolated, and fully characterized. The nitrosothiol (TGSNO) from 1-thioglycerol was obtained as a red gelatinous liquid, which decomposed rapidly at room temperature and so was not characterized. The kinetics of decomposition of GPSNO showed that there is a surprisingly large thermal pathway overlaid with a Cu2+/RS- catalyzed reaction. The results strongly suggest that the product disulfide complexes Cu2+ (for which there is some spectral evidence), leading to incomplete conversion by that route. Ascorbate also acts as a Cu2+ reductant. Another S-nitroso sugar, S-nitroso-1-thio-β-D-glucose (SNTG), behaved very similarly from solutions generated and used in situ. The decomposition of TGSNO shows induction periods suggesting that slow initial generation of Cu+ (the true catalyst) is taking place. There appears to be also a significant alternative pathway (analogous to that found for GPSNO), where the rate appears to be independent of [Cu2+], but very unusually this pathway is effectively halted by addition of EDTA either at the start of the reaction or at a later time. Reaction schemes are put forward to account for these unusual reaction characteristics.Key words: S-nitrosothiols, nitric oxide, ascorbate, copper catalysis.


1999 ◽  
Vol 06 (05) ◽  
pp. 929-934 ◽  
Author(s):  
H. OUGHADDOU ◽  
B. AUFRAY ◽  
J. M. GAY

We present one of the first experimental studies of the formation of an ordered surface alloy of a semiconductor, Ge, and a metal, Ag, with bulk tendency to phase separation. The kinetics of growth at room temperature as well as the surface segregation of Ge have been investigated for the (111) orientation using Auger Electron Spectroscopy (AES) and Low Electron Energy Diffraction (LEED). The growth mode of Ge on Ag(111) is layer-by-layer like up to at least two layers. An unexpected ordered surface alloy forming a [Formula: see text] superstructure is observed during the growth at 1/3 germanium monolayer, followed by a p(7× 7) superstructure at one-monolayer coverage. The surface Ge segregation studied via both dissolution and segregation kinetics shows the particular stability of the ordered [Formula: see text] surface alloy.


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