Intercalation of barium into graphite by molten salts method: Synthesis of massive samples for crystal structure determination of BaC6

Hajj, Inass El; Speyer, Lucie; Cahen, Sébastien; Herbuvaux, L.; Lagrange, Philippe; Medjahdi, Ghouti; Hérold, Claire

doi:10.1016/j.carbon.2021.09.073

Cited by 11 publications

(10 citation statements)

References 18 publications

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“…Thus, this synthesis method had shown remarkable results allowing the intercalation of metals into graphite, as firstly verified by the synthesis of bulk binary EuC6 compound [7]. Thereafter, several fully intercalated compounds have been synthesized including, either binary ones like SrC6 [8], BaC6 [9] or even novel quaternary compounds such as Li0.2K0.75Ba0.6C6 [10]. This last one has given the opportunity to explore the co-intercalation of different alkali metals in the van der Waals gaps.…”

Section: Introductionmentioning

confidence: 91%

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Simultaneous intercalation of lithium, potassium and strontium into graphite in molten salts medium

Hajj

Speyer

Cahen

et al. 2023

Journal of Solid State Chemistry

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Section: Introductionmentioning

confidence: 91%

“…The experiments are carried out in a glove box under argon atmosphere to avoid the reactivity towards air and moisture of the used reactants and reaction products. The novel Sr-based GIC is synthesized by adding 2 at.% of strontium in a LiCl-KCl eutectic medium as described in previous works [8][9][10].…”

Section: Synthesismentioning

confidence: 99%

Simultaneous intercalation of lithium, potassium and strontium into graphite in molten salts medium

Hajj

Speyer

Cahen

et al. 2023

Journal of Solid State Chemistry

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“…However, only a few applications of GICs have been realized thus far, except for the use of Li-intercalated graphite in secondary batteries. [10] For the synthesis of GICs, several methods, involving vapor-phase reaction, [2,11,12] solid-state reaction, [13] high-pressure reaction, [14] reactions in liquid reaction media, such as molten salts, [15][16][17][18] molten alloys [19,20] among others, have been developed. The vapor-phase reaction is the standard GIC synthesis method, in which GICs are synthesized by the contact of graphite with the intercalate vapor.…”

Section: Introductionmentioning

confidence: 99%

Dramatically Accelerated Formation of Graphite Intercalation Compounds Catalyzed by Sodium

2023

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by direct contact between the solid metal and graphite. Although relatively large GIC amounts can be synthesized using this method, the simultaneous production of undesirable carbides is also expected due to the high reaction temperature of ≈500 °C. [12,14,21] In a newly developed synthesis method using LiCl-KCl molten salts, GICs are synthesized by immersing graphite sheets in the molten salts containing dissolved intercalants. [15,16] To date, bulk BaC 6 and SrC 6 have been successfully synthesized using this method. However, sample synthesis is relatively time-(up to several days) and energy-consuming. [18] Accordingly, it is desirable to develop an innovative method to efficiently synthesize large quantities of homogeneous GIC samples.Coincidentally, while searching for new superconductors, we discovered that the formation of CaC 6 was significantly enhanced in samples containing a combination of Ca, C, and Na. To clarify the universality of this phenomenon, the effect of Na addition on the formation of GICs was studied for donor-type intercalants with alkali metals (A M ) = Li, Na, K, and alkaline earth metals (A E ) = Ca, Sr, Ba. Consequently, Na addition was found to be highly effective in the synthesis of A M -GICs and A E -GICs. Since the experimental evidence indicated that Na acts as a catalyst, the GIC synthesis method developed in this study will be referred to as the Na-catalyzed method.This article begins with a detailed description of the LiC 6 synthesis process at a room temperature (RT) of ≈25 °C as a typical demonstration of the effect of Na addition. Then, we propose a method for simultaneously reducing the amount of Na in the sample and fabricating sintered pellets. Next, the effectiveness of the Na-catalyzed method for the synthesis of K-GICs with controlled staging and Na-GIC itself is described. Moreover, it is demonstrated that Na acts as a potent catalyst for the synthesis of A E -GIC. Finally, we discuss the catalytic function of Na and present the merits and limitations of the proposed Na-catalyzed method for GIC applications as well as future challenges.

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“…The alkaline-earth metal expels the intercalated lithium and replaces it in the graphitic galleries. Following this mechanism, it has been possible to prepare SrC6, BaC6, EuC6 as bulk compounds [9][10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Co-intercalation into graphite of lithium, potassium and barium using LiCl–KCl molten salt

et al. 2022

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The synthesis of a novel first stage GIC containing simultaneously lithium, potassium and barium through a solid-liquid reaction by molten salts method is described. Such a route has been largely developed in our laboratory for intercalation of metals into graphite. The interplanar distance of this quaternary compound reaches 950 pm and exhibits poly-layered intercalated sheets defined by X-ray measurements. The Li0.2K0.75Ba0.6C6 chemical formula of the compound is determined by ion beam analysis and this GIC is remarkably homogeneous. This GIC is the first poly-layered one containing barium.

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Intercalation of barium into graphite by molten salts method: Synthesis of massive samples for crystal structure determination of BaC6

Cited by 11 publications

References 18 publications

Simultaneous intercalation of lithium, potassium and strontium into graphite in molten salts medium

Simultaneous intercalation of lithium, potassium and strontium into graphite in molten salts medium

Dramatically Accelerated Formation of Graphite Intercalation Compounds Catalyzed by Sodium

Co-intercalation into graphite of lithium, potassium and barium using LiCl–KCl molten salt

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