scholarly journals In-Situ Imaging of Molten High-Entropy Alloys Using Cold Neutrons

2019 ◽  
Vol 5 (2) ◽  
pp. 29 ◽  
Author(s):  
Nicholas Derimow ◽  
Louis Santodonato ◽  
Benjamin MacDonald ◽  
Bryan Le ◽  
Enrique Lavernia ◽  
...  

Real-time neutron imaging was utilized to produce a movie-like series of radiographs for in-situ observation of the remixing of liquid state immiscibility that occurs in equiatomic CoCrCu with the addition of Ni. A previous neutron imaging study demonstrated that liquid state immiscibility can be observed in-situ for the equiatomic CoCrCu alloy. In this follow-up study, equiatomic buttons of CoCrCu were placed alongside small Ni buttons inside an alumina crucible in a high-temperature vacuum furnace. The mass of the Ni buttons was specifically selected such that when melted in the same crucible as the CoCrCu buttons, the overall composition would become equiatomic CoCrCuNi. Neutron imaging was simultaneously carried out to capture 10 radiographs in 20 °C steps from 1000 °C to 1500 °C and back down to 1000 °C. This, in turn, produced a movie-like series of radiographs that allow for the observation of the buttons melting, the transition from immiscible to miscible as Ni is alloyed into the CoCrCu system, and solidification. This novel imaging process showed the phase-separated liquids remixing into a single-phase liquid when Ni dissolves into the melt, which makes this technique crucial for understanding the liquid state behavior of these complex alloy systems. As metals are not transparent to X-ray imaging techniques at this scale, neutron imaging of melting and solidification allows for the observation of liquid state phase changes in real time. Thermodynamic calculations of the isopleth for CoCrCuNix were carried out to compare the observed results to the predictions resulting from the current Thermo-Calc TCHEA3 thermodynamic database. The calculations show a very good agreement with the experimental results, as the calculations indicate that the CoCrCuNix alloy solidifies from a single-phase liquid when x ≥ 0.275, which is close to the nominal concentration of the CoCrCuNi alloy (x = 0.25). The neutron imaging shows that the solidification of CoCrCuNi results from a single-phase liquid. This is evident as no changes in the neutron attenuation were observed during the solidification of the CoCrCuNi alloy.

1989 ◽  
Vol 167 ◽  
Author(s):  
Seyong Oh ◽  
Igor Y. Khandros ◽  
Janet L. Poetzinger

AbstractA real-time x-ray analysis technique has been developed and employed for in-situ investigation of solid and liquid state reactions in Au-Sn/Cu system as a function of temperature. Typically, 1 μm eutectic Au-Sn films were deposited on 1.5 μm Cu layers on Si wafers. Phase changes in Au-Sn films on Cu from ambient to above the eutectic temperature have been investigated. Cu diffusion into Au-Sn film above 250 °C resulted in a ternary Au-Sn-Cu compound and raised the melting temperature of the structure to about 325 °C. This affects joining characteristics of the Au-Sn metallization.


2018 ◽  
Vol 25 (6) ◽  
pp. 1673-1682 ◽  
Author(s):  
Adam S. Hoffman ◽  
Joseph A. Singh ◽  
Stacey F. Bent ◽  
Simon R. Bare

In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer–Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer–Tropsch catalysis using syngas, H2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.


2017 ◽  
Vol 17 (12) ◽  
pp. 6372-6381 ◽  
Author(s):  
Anton S. Tremsin ◽  
Didier Perrodin ◽  
Adrian S. Losko ◽  
Sven C. Vogel ◽  
Takenao Shinohara ◽  
...  

2021 ◽  
Author(s):  
Jean-Michel Lellouche ◽  
Romain Bourdalle-Badie ◽  
Eric Greiner ◽  
Gilles Garric ◽  
Angelique Melet ◽  
...  

<p>The GLORYS12V1 system is a global eddy-resolving physical ocean and sea ice reanalysis at 1/12° resolution covering the 1993-present altimetry period, designed and implemented in the framework of the Copernicus Marine Environment Monitoring Service (CMEMS). All the essential ocean physical variables from this reanalysis are available with free access through the CMEMS data portal.</p><p>The GLORYS12V1 reanalysis is based on the current CMEMS global real-time forecasting system, apart from a few specificities that are detailed in this manuscript. The model component is the NEMO platform driven at the surface by atmospheric conditions from the ECMWF ERA-Interim reanalysis. Ocean observations are assimilated by means of a reduced-order Kalman filter. Along track altimeter sea level anomaly, satellite sea surface temperature and sea ice concentration data and in situ temperature and salinity (T/S) vertical profiles are jointly assimilated. A 3D-VAR scheme provides an additional correction for the slowly-evolving large-scale biases in temperature and salinity.</p><p>The performance of the reanalysis is first addressed in the space of the assimilated observations and shows a clear dependency on the time-dependent in situ observation system, which is intrinsic to most reanalyses. The general assessment of GLORYS12V1 highlights a level of performance at the state-of-the-art and the reliability of the system to correctly capture the main expected climatic interannual variability signals for ocean and sea ice, the general circulation and the inter-basins exchanges. In terms of trends, GLORYS12V1 shows a higher than observed  warming trend together with a lower than observed global mean sea level rise.</p><p>Comparisons made with an experiment carried out on the same platform without assimilation show the benefit of data assimilation in controlling water masses properties and their low frequency variability. Examination of the deep signals below 2000 m depth shows that the reanalysis does not suffer from artificial signals even in the pre-Argo period.</p><p>Moreover, GLORYS12V1 represents particularly well the small-scale variability of surface dynamics and compares well with independent (non-assimilated) data. Comparisons made with a twin experiment carried out at ¼° resolution allows characterizing and quantifying the strengthened contribution of the 1/12° resolution onto the downscaled dynamics.</p><p>In conclusion, GLORYS12V1 provides a reliable physical ocean state for climate variability and supports applications such as seasonal forecasts. In addition, this reanalysis has strong assets to serve regional applications and should provide relevant physical conditions for applications such as marine biogeochemistry. In a near future, GLORYS12V1 will be maintained to be as close as possible to real time and could therefore provide a relevant reference statistical framework for many operational applications.</p>


2018 ◽  
Vol 28 (42) ◽  
pp. 1804039 ◽  
Author(s):  
Tae Woong Kim ◽  
Naoyuki Shibayama ◽  
Ludmila Cojocaru ◽  
Satoshi Uchida ◽  
Takashi Kondo ◽  
...  

2013 ◽  
Vol 52 (40) ◽  
pp. 10541-10544 ◽  
Author(s):  
Ranjit Thakuria ◽  
Mark D. Eddleston ◽  
Ernest H. H. Chow ◽  
Gareth O. Lloyd ◽  
Barry J. Aldous ◽  
...  

2006 ◽  
Vol 9 (01) ◽  
pp. 7-14 ◽  
Author(s):  
Chengli Dong ◽  
Peter S. Hegeman ◽  
Andrew J.G. Carnegie ◽  
Hani Elshahawi

Summary Formation fluid sampling early in the life of a well ensures that vital information is available for timely input to field planning decisions. For example, in subsea wells, flow assurance is a major concern, and formation fluid samples from openhole logging help operators optimize investment in both upstream and downstream facilities. When a formation fluid sample is taken from a well drilled with oil-based mud (OBM), sample contamination by the OBM filtrate is a critical factor for the accurate measurement of the sample pressure/volume/temperature (PVT) properties. A technique of monitoring sample contamination from OBM filtrate uses optical means to monitor the buildup of both color- and methane-absorption signals during sampling. The technique provides real-time analysis of sample contamination. Methane detection is essential for condensates and lightly colored crude oils; for such fluids, the color buildup becomes difficult to detect, but the high methane content of these fluids makes possible a reliable methane-based OBM-contamination monitoring algorithm. Gas/oil ratio (GOR) is an important property of crude oil, and it is a vital input to the design of production facilities. Conventionally, GOR is measured at a PVT laboratory, and it may take many weeks before the laboratory can provide this critical information. In this paper, we describe the development of an in-situ GOR measurement technique, which uses the optical properties of methane and oil components in crude oil. With this technique, GOR can be measured downhole in real time, when the sample is taken, and without requiring phase separation. Downhole GOR has many advantages over the conventional GOR measurement techniques. It does not require tampering with the sample, which helps the operator maintain the fluid in a single phase during and after sampling. It also can aid in fingerprinting oils from different layers and provides early indications of GOR that can be compared to PVT lab results. Both the OBM contamination monitoring and the GOR algorithms work well for most crude oils. However, for heavy (dark) oils, the contamination prediction from the methane component and the GOR prediction become unreliable because of the color effect. In this paper, we describe the methodology for downhole GOR measurement, and we provide details of a decolorization technique to remove the color effect of dark oils from the methane, oil, and base channels in a downhole optical fluid analyzer tool. This technique significantly improves real-time contamination monitoring and GOR prediction results for dark oils. Introduction Real-time estimation of sample contamination by drilling-mud filtrate is critical for the collection of representative hydrocarbon-fluid samples in wells drilled with OBM. The hydrocarbon sample may become useless if the contamination is too high (typically above 10 to 15% for crude oils or 1 to 3% for gas condensates). In-situ sample OBM contamination can be predicted in real time by a downhole optical fluid analyzer tool, which is used as a module of a formation testing tool (Mullins and Schroer 2000; Smits et al. 1995; and Crombie et al. 1998). This is accomplished by using a technique of monitoring OBM contamination, which is based on measuring the change of methane content and color in the flowline as cleanup with the downhole pump proceeds and progressively larger fractions of formation fluid replace the OBM filtrate. An accurate value of the GOR is important for many applications, including crude-oil typing and production facilities design. Conventionally, GOR is measured in a PVT laboratory by flashing the crude oil and then measuring the volumes of the gaseous and liquid phases at standard conditions (1 atm and 60°F). It may take many weeks before the laboratory can provide this critical information. The downhole optical fluid analyzer tool has a methane channel and an oil channel, which cover the methane absorption peak and oil absorption peak, respectively. We have developed an in-situ GOR measurement technique that derives GOR from the optical density (OD) ratio of the methane channel and the oil channel. Thus, GOR can be measured downhole in real time, when the sample is taken, and while keeping the sample intact. Downhole GOR is valuable in providing an early confirmation check for subsequent laboratory PVT analysis. The downhole GOR measurement also aids fingerprinting oils from different layers and helps the operator maintain the fluid in a single phase during sampling. Both the OBM contamination monitoring and the downhole GOR techniques work well for the majority of light- to medium-colored crude oils. However, when these two techniques are applied to heavy oils, the color absorption of the crude extends to the near-infrared region (NIR) and covers the methane and oil molecular-vibration peaks. If not corrected for, this would result in errors in the methane-based contamination prediction and GOR prediction. This paper describes a decolorization algorithm to remove the color effect from the methane and the oil channels. This algorithm is based on the exponential decay of color absorption toward the longer wavelengths in the NIR region. After decolorization, the methane and oil channels contain only the molecular-vibration absorptions of methane and oil, which are then used to derive an accurate crude-oil contamination value and GOR. The examples described here involved OBM. It should be noted that all the techniques for GOR calculation mentioned in this paper can be, and have been, applied successfully to sampling in wells drilled with water-based mud.


2004 ◽  
Vol 808 ◽  
Author(s):  
Charles W. Teplin ◽  
Dean H. Levi ◽  
Qi Wang ◽  
Eugene Iwaniczko ◽  
Kim M. Jones ◽  
...  

ABSTRACTWe use in-situ real-time spectroscopic ellipsometry to observe the breakdown of silicon epitaxy during growth by hot-wire chemical vapor deposition (HWCVD) on Si (100) substrates. Representative data is presented for the two types of epitaxy breakdown that we have observed: 1) an immediate transition to hydrogenated amorphous silicon (a-Si:H), and 2) a slower transition where a-Si:H cones nucleate and grow until they eclipse further epitaxial growth. Simple models, consistent with transmission-electron and atomic-force micrographs, describe the evolution of both types of breakdown showing that real-time spectroscopic ellipsometry is a useful tool for monitoring the growth of epitaxial silicon.


2015 ◽  
Vol 754-755 ◽  
pp. 508-512
Author(s):  
M.A.A. Mohd Salleh ◽  
A. Sugiyama ◽  
Hideyuki Yasuda ◽  
Stuart D. McDonald ◽  
Kazuhiro Nogita

This paper demonstrates the development of an experimental technique of in-situ observation for soldering of Sn-0.7wt%Cu lead-free solder on a Cu substrate which was achieved for the first time by synchrotron X-ray imaging. Reactions between liquid solder and Cu substrate during a soldering process were able to be recorded in real-time. Individual stages of the soldering process consisted of flux activation in removal of Cu oxide, solder melting and contact with the Cu substrate (wetting) and intermetallic compound (IMC) and void formation between the solder and Cu substrate. The technique development which includes experimental setup with calculated optimum beam energy in the range of 20 – 30 keV appears to result in a clear observation of real-time X-ray imaging of the soldering process. This technique provides a key method to understand the mechanism of formation of micro-electronic inter-connects for future electronic packaging applications.


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