In-Situ Corrosion Studies on Cast Steel for a High-Level Waste Packaging in a Rock Salt Repository

1988 ◽  
Vol 127 ◽  
Author(s):  
W. Schwarzkopf ◽  
E. Smailos ◽  
R. Koster

ABSTRACTPrevious corrosion studies performed on a number of materials have shown that unalloyed steels are promising materials for long-term resistant packagings to be used in disposal of heat-generating wastes in rock salt formations. This is the reason why those steels are the subject of more detailed investigations. This paper reports an in-situ experiment conducted in the Asse salt mine in which the influence of selected characteristics (welding, shape) of containers on the corrosion behaviour of cast steel was studied. The material was tested in NaCl brine which might intrude into an HLW borehole in an accident scenario. For this, an electron beam welded cast-steel tube was stored for 18 months in a 2-m deep heated borehole and the annular gap between the tube and the borehole wall was filled with saturated NaCl brine. The vertical temperature profile in the borehole was in the range from 90°C to 200°C; the maximum temperature occurred in the center of the heated zone and the minimum temperature in the upper parts of tube.Under the testing conditions cast steel was subjected to general corrosion at a maximum corrosion rate of 120 μm/a. Considering this magnitude of the corrosion rates, the resulting corrosion allowances are technically acceptable for a packaging having long service-lives. Pitting and crevice corrosion as well as stress-corrosion cracking did not occur in cast steel, and electron beam welding did not exert a noticeable influence on cast-steel corrosion. With these results available, cast steel continues to be considered as a promising HLW packaging material.

1991 ◽  
Vol 257 ◽  
Author(s):  
W. Schwarzkopf ◽  
E. Smailos ◽  
R. KÖster

ABSTRACTPrevious corrosion studies have shown that the passive alloys Ti 99.8-Pd and Hastelloy C4 are the most promising corrosion protection materials for long-term resistant carbon-steel containers for the disposal of heat-generating wastes in rock salt formations. Consequently, these materials are subject to more detailed investigations. The influence of selected container manufacturing characteristics (sealing technique, application mode of the corrosion protecting layer on the steel) on the corrosion behaviour of Ti 99.8-Pd and Hastelloy C4was studied using in-situ experiments. The corrosion resistance of the materials was examined both in NaCI brine and MgCl2-rich brine, which might enter into an HLW borehole under certain disposal conditions. Four electron-beam welded cast-steel tubes plated with corrosion protection layers made of Ti 99.8-Pd and Hastelloy C4, respectively, were stored for 18 months in 2-m deep heated boreholes in the Asse salt mine. The annular gap between the tubes and the borehole wall was filled with saturated NaCl-brine or Qbrine (MgCl2-rich). The vertical temperature profile in the boreholes ranged from 90°C to 200°CIn the cast-steel tube with a corrosion protection of Ti 99.8-Pd, no indication of corrosion was observed on the EB-welds or on the explosion plated material in both brines. The cast-steel tube with a corrosion protection of Hastelloy C4 also was found to be resistant to any kind of corrosion in the NaCl-brine. In the MgCl2-rich brine, however, small pitting corrosion of 15 pm was observed after 1.5 years on the passive surface layer that was formed.On the basis of these results, Ti 99.8-Pd continues to be considered as a promising corrosion protection material for long-lived HLW containers.


1988 ◽  
Vol 127 ◽  
Author(s):  
Martin A. Molecke ◽  
N. Rob Sorensen

ABSTRACTIn situ waste package performance experiments involving simulated (non-radioactive) defense high-level waste (DHLW) containers have been in progress since late 1984 at the Waste Isolation Pilot Plant (WIPP) facility. These experiments involve full-size, simulated DHLW containers of several metals and designs emplaced in the WIPP bedded rock salt. These test containers are surrounded by granular backfill (packing) materials, have in many cases been intentionally injected with brines, and are heavily instrumented. A majority of the test packages also contain nonradioactive DHLW borosilicate glass waste form, either within the container and/or outside of it. The primary purpose of these WIPP simulated DHLW experiments is to evaluate the in situ durability and performance of all waste package engineered barrier materials, and to perform package concept validation testing.Twelve of the test DHLW containers, emplaced in WIPP test Room B, have been in heated operation since 1985 and had a maximum surface temperature of about 190°C. These containers were recently retrieved, after about 3 years of heated exposure, for detailed posttest laboratory analyses of: general corrosion and metallurgical degradation, waste form and backfill materials alterations, and other rock salt-brine-barrier materials near-field interactions with the “repository” geochemical environment. Test canisters and overpacks made of ASTM Grade-12 titanium showed essentially no visible degradation in either the base metal or welds; cast mild steel A216/WCA over-packs have suffered some uniform corrosion. Significant degradation of the removed instruments and associated test apparatus has been found: pieces of stainless steel (both 304L and 316) apparatus have undergone extensive stress-corrosion cracking failure and non-uniform attack; Inconel 600-sheathed instruments have undergone both extensive uniform and localized (pitting) attack. Granular backfill materials have been significantly compacted by creep closure to about a density of 2 kg/m. Laboratory analyses are still in progress. Further details on these materials results plus instrumentation data and other in situ WIPP waste package test observations are discussed.


1991 ◽  
Vol 257 ◽  
Author(s):  
E. Smailos ◽  
W. Schwarzkopf ◽  
B. Kienzler ◽  
R. KÖster

ABSTRACTIn previous corrosion studies, carbon steels, especially the fine-grained steel TStE355, were identified as promising materials for heat-generating nuclear waste containers acting as a barrier in a rock-salt repository. In the present study detailed investigations have been performed on fine-grained steel to determine the influence of important parameters on its corrosion behaviour in disposal-relevant salt brines. These parameters are: brine composition (Mg Cl2-rich and NaCI-rich brines), temperature (90°C, 170°C), and salt impurities, such as H2S concentrations of 25 mg/I-200 mg/I salt brine.Under the conditions of the tests used here, carbon steel was subjected to general corrosion. Pitting and crevice corrosion or stress-corrosion cracking were not observed. The increase in temperature from 90°C to 170°C strongly enhanced the corrosion rate of the steel. In the MgCl2-rich brines, considerably higher rates (37-70 μm/a at 90°C, 200-300 °m/a at 170°C) were observed than in the NaCI-rich brine (5 μm/a at 90°C, 46 μm/a at 170°C). H2S concentrations in the MgCl2-rich Qbrine of up to 200 mg/l did not influence significantly the corrosion rate of the steel. The corrosion rates determined imply corrosion allowances that are technically acceptable for thick-walled containers. In view of these results, fine-grained steel continues to be considered as a promising material for long-lived HLW containers.


1988 ◽  
Vol 127 ◽  
Author(s):  
J. P. Simpson ◽  
R. Schenk

ABSTRACTHydrogen evolution from anoxic corrosion of cast steel overpacks in high-level waste repositories is an important issue for design if, as has been estimated, the hydrogen is prevented from escaping by diffusion by a low permeability compacted bentonite backfill.Evaluation of the corrosion results showed three basic types of corrosion behaviour: general corrosion with oxide layer formation, unstable corrosion behaviour with pitting or macro-element formation and stable passive behaviour.Cast steel containers under Swiss repository conditions are expected to suffer general corrosion with oxide layer formation. This behaviour gives the highest long term corrosion rates (2–5 μm/a) without local attack, above the 0.03–0.8 μm/a tolerated for hydrogen escape by diffusion but below the 20 μm/a assumed for overpack design.


2011 ◽  
Vol 383-390 ◽  
pp. 4678-4682
Author(s):  
N. Arivazhagan ◽  
S Narayanan ◽  
Singh Surendra ◽  
Prakash Satya ◽  
G. M. Reddy

In the present work hot corrosion studies were carried out on electron beam welded AISI 304 and AISI 4140 dissimilar weldment in molten salt (K2SO4-60% NaCl) environment at 800 °C for 50 cycles. The weight gain follows parabolic law in all the cases. It is observed that the scale formation was maximum on 4140 side as compared on 304 side. Moreover higher content of Fe2O3 and Cr2O3 on scale over weld zone may be due to enrichment of this zone with Fe and Cr. This could be attributed to diffusion of chromium towards AISI 4140 from the AISI 304 and diffusion of iron from AISI 4140 side towards AISI 304. Furthermore weld interface suffered accelerated corrosion behavior in the chloride and sulfate mixed molten salt environment in the form of intense spalling and sputtering of its scale. The cracking of oxide scale on the weldment might be attributed to different composition of base metals, weld metal and oxide formed.


CORROSION ◽  
10.5006/3548 ◽  
2021 ◽  
Author(s):  
Sheyla de Carvalho ◽  
Richard Barker ◽  
MARIANA FOLENA ◽  
Mohaamed Al-Khateeb ◽  
JOSE ANTONIO PONCIANO GOMES ◽  
...  

<i>This paper presents an experimental and theoretical investigation into water condensation and corrosion under non-corrosion product forming conditions at the top of line in a static, CO<sub>2 </sub>environment. An experimental test cell is developed to measure droplet lifetimes, condensation rates, as well as in situ and integrated corrosion rates (using miniature electrodes and mass loss specimens, respectively), as a function of the surface and gas temperatures, when the gas flow is dominated by natural convection. Experimental results show clearly that that water condensation rate (WCR) is not very influential on corrosion rate at low surface temperatures (T<sub>s</sub>) (particularly below 25<sup>o</sup>C) but becomes much more important at higher surface temperatures (>40<sup>o</sup>C). These findings are summarised in a new empirical correlation for TLC rate as a function of the condensation rate and surface temperature. A model for condensation at the top of the line for static, buoyancy-driven conditions is also presented and is shown to predict dropwise condensation rates accurately for a range of experimental conditions. The developed miniature electrodes for in situ electrochemical measurement are shown to provide an accurate interpretation of the transient response in general corrosion behaviour by giving real-time corrosion rates to complement the mass loss measurement.</i>


Author(s):  
Dudley M. Sherman ◽  
Thos. E. Hutchinson

The in situ electron microscope technique has been shown to be a powerful method for investigating the nucleation and growth of thin films formed by vacuum vapor deposition. The nucleation and early stages of growth of metal deposits formed by ion beam sputter-deposition are now being studied by the in situ technique.A duoplasmatron ion source and lens assembly has been attached to one side of the universal chamber of an RCA EMU-4 microscope and a sputtering target inserted into the chamber from the opposite side. The material to be deposited, in disc form, is bonded to the end of an electrically isolated copper rod that has provisions for target water cooling. The ion beam is normal to the microscope electron beam and the target is placed adjacent to the electron beam above the specimen hot stage, as shown in Figure 1.


Author(s):  
J. I. Bennetch

In a recent study of the superplastic forming (SPF) behavior of certain Al-Li-X alloys, the relative misorientation between adjacent (sub)grains proved to be an important parameter. It is well established that the most accurate way to determine misorientation across boundaries is by Kikuchi line analysis. However, the SPF study required the characterization of a large number of (sub)grains in each sample to be statistically meaningful, a very time-consuming task even for comparatively rapid Kikuchi analytical techniques.In order to circumvent this problem, an alternate, even more rapid in-situ Kikuchi technique was devised, eliminating the need for the developing of negatives and any subsequent measurements on photographic plates. All that is required is a double tilt low backlash goniometer capable of tilting ± 45° in one axis and ± 30° in the other axis. The procedure is as follows. While viewing the microscope screen, one merely tilts the specimen until a standard recognizable reference Kikuchi pattern is centered, making sure, at the same time, that the focused electron beam remains on the (sub)grain in question.


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.


Author(s):  
Gunnar Zimmermann ◽  
Richard Chapman

Abstract Dual beam FIBSEM systems invite the use of innovative techniques to localize IC fails both electrically and physically. For electrical localization, we present a quick and reliable in-situ FIBSEM technique to deposit probe pads with very low parasitic leakage (Ipara < 4E-11A at 3V). The probe pads were Pt, deposited with ion beam assistance, on top of highly insulating SiOx, deposited with electron beam assistance. The buried plate (n-Band), p-well, wordline and bitline of a failing and a good 0.2 μm technology DRAM single cell were contacted. Both cells shared the same wordline for direct comparison of cell characteristics. Through this technique we electrically isolated the fail to a single cell by detecting leakage between the polysilicon wordline gate and the cell diffusion. For physical localization, we present a completely in-situ FIBSEM technique that combines ion milling, XeF2 staining and SEM imaging. With this technique, the electrically isolated fail was found to be a hole in the gate oxide at the bad cell.


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