Chronopotentiometric Analysis in Fused Lithium Chloride-Potassium Chloride

Laitinen, Herbert A.; Ferguson, W. S.

doi:10.1021/ac60121a002

Cited by 74 publications

(44 citation statements)

References 20 publications

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“…The apparatus used in this work includes the fol- (4)(5)(6). The microelectrodes used consisted of 26 gauge Pt wire sealed into Corning 0120 glass with about 1 mm of the wire projecting (total electrode area of 1.4 mm ~) or 18 gauge tungsten wire sealed into Pyrex glass with the wire ground flush to the glass (total electrode area of 0.8 mm~).…”

Section: Methodsmentioning

confidence: 99%

Preparation of Pure Fused Lithium Chloride-Potassium Chloride Eutectic Solvent

Laitinen¹,

Ferguson²,

Osteryoung³

1957

J. Electrochem. Soc.

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169

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Hydrolytic decomposition occurs during the fusion of a eutectic mixture of lithium chloride-potassium chloride containing traces of moisture if the fusion conditions are not controlled. The resultant contamination by hydroxyl ion greatly lowers the utility of this mixture as a fused salt solvent. The effectiveness of various procedures used for preparation of the fused salt solvent was followed by observation of the characteristic polarographic residual current using a platinum microelectrode. A preparative method is described which involves drying the mixture under moderate vacuum, fusion under anhydrous hydrogen chloride, and removal of the hydrogen chloride from the melt.

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Section: Methodsmentioning

confidence: 99%

Preparation of Pure Fused Lithium Chloride-Potassium Chloride Eutectic Solvent

Laitinen¹,

Ferguson²,

Osteryoung³

1957

J. Electrochem. Soc.

Self Cite

169

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“…However, to date there has been a significant technological barrier to the development of microelectrode sensors for reproducible and quantitative MS analysis and monitoring. For example, microelectrodes fabricated by metal wire drawing, glass encapsulation and cleavage to expose the metal wire end with surrounding glass insulation as a disk microelectrode have been employed with limited success, as this has been shown to result in both initial and time-dependent variation of response [24][25][26][27][28] . The initial variability can be attributed to differences in the wire size and cross section due to variation in the wire drawing process, which as a result requires optical and/or electrochemical characterization of electrode size and shape.…”

Section: Introductionmentioning

confidence: 99%

Enhanced Electroanalysis in Lithium Potassium Eutectic (LKE) Using Microfabricated Square Microelectrodes

et al. 2014

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Molten salts (MSs) are an attractive medium for chemical and electrochemical processing and as a result there is demand for MS-compatible analysis technologies. However, MSs containing redox species present a challenging environment in which to perform analytical measurements because of their corrosive nature, significant thermal convection and the high temperatures involved. This paper outlines the fabrication and characterization of microfabricated square microelectrodes (MSMs) designed for electrochemical analysis in MS systems. Their design enables precise control over electrode dimension, the minimization of stress because of differential thermal expansion through design for high temperature operation, and the minimization of corrosive attack through effective insulation. The exemplar MS system used for characterization was lithium chloride/potassium chloride eutectic (LKE), which has potential applications in pyrochemical nuclear fuel reprocessing, metal refining, molten salt batteries and electric power cells. The observed responses for a range of redox ions between 400 and 500 °C (673 and 773 K) were quantitative and typical of microelectrodes. MSMs also showed the reduced iR drop, steady-state diffusion-limited response, and reduced sensitivity to convection seen for microelectrodes under ambient conditions and expected for these electrodes in comparison to macroelectrodes. Diffusion coefficients were obtained in close agreement with literature values, more readily and at greater precision and accuracy than both macroelectrode and previous microelectrode measurements. The feasibility of extracting individual physical parameters from mixtures of redox species (as required in reprocessing) and of the prolonged measurement required for online monitoring was also demonstrated. Together, this demonstrates that MSMs provide enhanced electrode devices widely applicable to the characterization of redox species in a range of MS systems.

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“…46 Fig. 8 illustrates a series of chronopotentiograms obtained on a tungsten electrode at 1023 K under the different current intensities in LiCl−KCl−MgCl 2 −AlCl 3 −LaCl 3 melts.…”

Section: Resultsmentioning

confidence: 99%

Study on Electrochemical Behavior of La(III) and Preparation of Al−La Intermetallic Compound Whiskers in Chloride Melt

Yan

Zhang

et al. 2015

J. Electrochem. Soc.

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This paper exhibits a novel method to prepare the Al−La intermetallic compound whiskers on the liquid magnesium electrode at 1023 K. The electrochemical behavior of La (III) on a tungsten electrode in LiCl−KCl−MgCl 2 −AlCl 3 −LaCl 3 melts was investigated by different electrochemical measurements. The result from chronopotentiometry shows that co-deposition of Mg(II), Li(I), Al(III) and La(III) ions occurs when the current intensity more than −190 mA. Quarternary Mg-Li-Al-La alloy was prepared by galvanostatic electrolysis, and the Al 4 La intermetallic compound was identified via X-ray diffraction (XRD). The microstructure and micro−zone chemical analysis of Mg−Li−Al−La alloy were accomplished by scanning electron microscopy (SEM) with energy dispersive spectrometry (EDS). The results illustrate that lots of needle-like precipitates are synthesized on magnesium substrate. The crystal structure of needle-like precipitates was certified by transmission electron microscopy (TEM) with electron diffraction pattern. The result exhibits that the needle-like precipitates are Al−La intermetallic compound whiskers. The micro hardness of Mg−Li−Al−La alloy is remarkable improved with the help of Al−La intermetallic compound whiskers. Along with the development of the economy, the energy consumption issue and environmental protection have become the theme of the world. With this problem, the superlight materials have attracted much attention. Magnesium−lithium alloys are considered to the most promising new energy materials, which have drawn more and more attention by the industry of aerospace and microelectronic because of the advantages of the low density, high specific strength, good machinability, damping ability and high energetic particle penetration resistance.1-4 Nevertheless, the widespread use of magnesium−lithium alloys is limited by the poor mechanical properties of alloy, especially the hardness.The definition of the whisker was given by Cevans et al.: 5 the crystal structure of the whisker is single-crystal structure, the ratio of the length to diameter is between 5 and 1000. The diameter of whisker is falling in 20 to 100 nanometer. Many researchers [6][7][8][9] have adopted the whiskers to improve the mechanical properties of magnesium−lithium alloys. On account of the binding force between the whisker and the magnesium−lithium alloys substrate is limited by the adscititious whisker, the mechanical properties of the magnesium−lithium alloy are not likely to see a great promotion. In our prior work, for the extraction of europium and formation of Al−Li−Eu alloy, most of needle-like precipitates can be formed in aluminum substrate.10 The needle-like precipitates grow through several grains and across grain boundaries. Such long needle-like precipitates should act as pins to increase the boundary strength and improve the properties of alloy. Therefore, the thought of whether the mechanical properties of the magnesium−lithium alloys can be improved by the formation of Al−RE intermetallic compound whiskers in mag...

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Chronopotentiometric Analysis in Fused Lithium Chloride-Potassium Chloride

Cited by 74 publications

References 20 publications

Preparation of Pure Fused Lithium Chloride-Potassium Chloride Eutectic Solvent

Preparation of Pure Fused Lithium Chloride-Potassium Chloride Eutectic Solvent

Enhanced Electroanalysis in Lithium Potassium Eutectic (LKE) Using Microfabricated Square Microelectrodes

Study on Electrochemical Behavior of La(III) and Preparation of Al−La Intermetallic Compound Whiskers in Chloride Melt

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