Synthesis of nanolayered ternary borides powders (MAB phases) by sustainable molten salt shielded synthesis/sintering (MS3) process

Dey, Maharshi; Javaid, Sabah; Clifford, Dustin M.; Sharma, Vaibhav; Barua, Radhika; Gupta, Surojit

doi:10.1007/s10853-021-06779-0

Cited by 12 publications

(8 citation statements)

References 41 publications

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“…Based on the aforementioned results, it is reasonable to conclude that even at 1200°C, the reaction is still in progress. Knowing that the synthesis of single-phase Fe 2 AlB 2 requires a very long time to be achieved [31], according to the present XRD results, as shown in Fig. 2a, the sample synthesized by adding Sn powder was nearly single-phase Fe 2 AlB 2 .…”

Section: Resultssupporting

confidence: 53%

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Molten salt shielded synthesis of the nanolaminated transition metal boride Fe2AlB2

Benamor

Benamor²,

Chiker³

et al. 2023

Int J Adv Manuf Technol

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Fe 2 AlB 2 is one of many ternary transition metal borides called MAB phases, which attracted interest owing to its magnetocaloric effect and magnetic properties. Herein, the molten salt shielded synthesis (MS 3 ) of Fe 2 AlB 2 powder is studied using potassium bromide "KBr" in an open-air atmosphere. The synthesis process of the MAB phase, from Fe, Al, and B elemental powders, was studied with and without Sn additive in the temperature range of 900-1200°C. The obtained powders were analyzed using XRD, TDA, GTA and SEM analysis. The corresponding results revealed a successful synthesis of nearly-pure Fe 2 AlB 2 phase at 1000°C for only one hour of holding time, beyond which FeB impurities form. These results show the e ciency of KBr (with Sn as a synthesis aid 'additive') in increasing the reactivity of this MAB phase in terms of the lowest synthesis temperature and time reported to date.

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Section: Resultssupporting

confidence: 53%

“…They were able to synthesize different ternary transition metal compounds (Ti 3 SiC 2 , Ti 2 AlN, TiC, and MoAlB) as well as pure Ti. Recently, M. Dey et al [31] synthesized Fe 2 AlB 2 , Mn 2 AlB 2 , and MoAlB powders by molten salt shielded synthesis with different salts (NaCl, KBr, and eutectic NaCl-KCl).…”

Section: Introductionmentioning

confidence: 99%

Molten salt shielded synthesis of the nanolaminated transition metal boride Fe2AlB2

Benamor

Benamor²,

Chiker³

et al. 2023

Int J Adv Manuf Technol

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“…To target Fe 2 AlB 2 from FeB phases, we have modified a recent synthesis in molten salts, using the LiCl/KCl eutectic mixture as solvent, NaAlCl 4 as an Al source, NaH as a reducing agent to generate in situ Al 0 (eqs and ), and α or β-FeB with molar ratios FeB:Al:NaH = 2:1.5:10. The large NaH excess ensures fast delivery of Al atoms, while the excess of Al vs FeB fastens its incorporation, as previously reported. ,, To favor the Al incorporation, we have increased the surface of the FeB particles exposed to the reaction medium by developing an impregnation protocol. The particles were dispersed in methanol and then abruptly mixed with a previously ground LiCl/KCl eutectic salt mixture to avoid reaggregation.…”

Section: Resultsmentioning

confidence: 99%

“…The large NaH excess ensures fast delivery of Al atoms, while the excess of Al vs FeB fastens its incorporation, as previously reported. 37,38,70 To favor the Al incorporation, we have increased the surface of the FeB particles exposed to the reaction medium by developing an impregnation protocol. The particles were dispersed in methanol and then abruptly mixed with a previously ground LiCl/KCl eutectic salt mixture to avoid reaggregation.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…Overall, comparing the reactivity of α-FeB and β-FeB could highlight interesting effects of nanoscale domains and crystal defects. We have then To target Fe 2 AlB 2 from FeB phases, we have modified a recent synthesis in molten salts, 70 using the LiCl/KCl eutectic mixture as solvent, NaAlCl 4 as an Al source, NaH as a reducing agent to generate in situ Al 0 (eqs 4 and 5), and α or β-FeB with molar ratios FeB:Al:NaH = 2:1.5:10. The large NaH excess ensures fast delivery of Al atoms, while the excess of Al vs FeB fastens its incorporation, as previously reported.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

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Revealing the Elusive Structure and Reactivity of Iron Boride α-FeB

et al. 2023

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Crystal structures can strongly deviate from bulk states when confined into nanodomains. These deviations may deeply affect properties and reactivity and then call for a close examination. In this work, we address the case where extended crystal defects spread through a whole solid and then yield an aperiodic structure and specific reactivity. We focus on iron boride, α-FeB, whose structure has not been elucidated yet, thus hindering the understanding of its properties. We synthesize the two known phases, α-FeB and β-FeB, in molten salts at 600 and 1100 °C, respectively. The experimental X-ray diffraction (XRD) data cannot be satisfactorily accounted for by a periodic crystal structure. We then model the compound as a stochastic assembly of layers of two structure types. Refinement of the powder XRD pattern by considering the explicit scattering interference of the different layers allows quantitative evaluation of the size of these domains and of the stacking faults between them. We, therefore, demonstrate that α-FeB is an intergrowth of nanometer-thick slabs of two structure types, β-FeB and CrB-type structures, in similar proportions. We finally discuss the implications of this novel structure on the reactivity of the material and its ability to perform insertion reactions by comparing the reactivities of α-FeB and β-FeB as reagents in the synthesis of a model layered material: Fe 2 AlB 2 . Using synchrotron-based in situ X-ray diffraction, we elucidate the mechanisms of the formation of Fe 2 AlB 2 . We highlight the higher reactivity of the intergrowth α-FeB in agreement with structural relationships.

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Low temperature atmospheric synthesis of WAlB and Mn2AlB2 MAB phases by modified molten salt shielded synthesis method

Roy

Mondal

Banerjee

et al. 2023

Advanced Powder Technology

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Synthesis of nanolayered ternary borides powders (MAB phases) by sustainable molten salt shielded synthesis/sintering (MS3) process

Cited by 12 publications

References 41 publications

Molten salt shielded synthesis of the nanolaminated transition metal boride Fe2AlB2

Molten salt shielded synthesis of the nanolaminated transition metal boride Fe2AlB2

Revealing the Elusive Structure and Reactivity of Iron Boride α-FeB

Low temperature atmospheric synthesis of WAlB and Mn2AlB2 MAB phases by modified molten salt shielded synthesis method

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