Saponites containing divalent transition metal cations in octahedral positions — Exploration of synthesis possibilities using microwave radiation and NMR characterization

Trujillano, Raquel; Rico, E.; Vicente, M.A.; Rives, V.; Sobrados, Isabel; Sanz, J.

doi:10.1016/j.clay.2015.07.023

Cited by 14 publications

(7 citation statements)

References 25 publications

(32 reference statements)

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“…These diffraction peaks are attributed to the (001), (100), (004), (110), (210), and (300) crystal planes, respectively, and the d -spacing of Fe–BEI calculated from the (001) crystal plane is 9.9 Å. As a kind of layered silicate, beidellite has a similar layered structure to saponite or montmorillonite. ,− They all have an intercalated structure composed of host laminate and interlayer metal ions (Na + , K + , Ca 2+ , Mg 2+ , etc.). However, their laminate structure is different: saponite is a type of trioctahedral smectite, while beidellite and montmorillonite belong to the dioctahedral structure.…”

Section: Resultsmentioning

confidence: 99%

Two-Dimensional Beidellite/Carbon Superlattice for Boosting Lithium-Ion Storage Performance

Zhang

et al. 2022

ACS Appl. Mater. Interfaces

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Two-dimensional Fe–beidellite/carbon (Fe–BEI@C) superlattice-like heterostructure was prepared by intercalation of glucose in the gallery of layered Fe–BEI followed by calcination. The interlaminar and superficial carbon coating enables Fe–BEI to have good rate performance, fast lithium-ion diffusion, and high pseudocapacitance contribution, leading to excellent lithium storage performance as anode material for lithium-ion batteries (LIBs). The Fe–BEI@C/Li half cell delivers a maximum specific capacity of 850 mAh·g–1 at 0.5 A·g–1 and has a 92.3% retention rate after 100 cycles along with a high-rate performance of 403 mAh·g–1 at 5 A·g–1. The reversible valence state change of Si2+/Si4+ and Fe0/Fe x+ (0 < x < 3) in electrochemical cycles are realized without collapse of layered structure. Additionally, the Fe–BEI@C heterostructure displays a high Li+ diffusion coefficient of 10–13∼10–10 cm2 s–1, illustrating fast Li+ transfer in the interlayer of Fe–BEI@C heterostructure. Dynamic analysis reveals that the Si redox reaction is almost dominated by surface control and that of Fe is mainly diffusion-controlled. This work has exploited a novel layered silicate as anode material for LIBs and developed a molecular-level carbon hybridization method to improve their electrochemical performance, which is meaningful for the application of layered silicate in the energy-storage field.

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Section: Resultsmentioning

confidence: 99%

Two-Dimensional Beidellite/Carbon Superlattice for Boosting Lithium-Ion Storage Performance

Zhang

et al. 2022

ACS Appl. Mater. Interfaces

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“…Saponite is a trioctahedral 2:1 smectite with the ideal composition M x Mg 3 Al x Si 4−x O 10 (OH,F) 2 , where M signifies the interlayer cation, e.g., Na + , K + , Rb + , NH 4 + , or 1/2Ca 2+ , 1/2Ba 2+ , l/2Mg 2+ , or even 1/3A1 3+ ; where x can range between approximately 0.3 and A number of different saponite synthesis methods with adjustable compositions and physicochemical properties have been described over the decades. These methods can be divided into sol-gel methods under mild temperatures and pressures [16][17][18][19][20], hydrothermal methods which are carried out at relatively higher temperatures and pressures [8,[21][22][23][24][25][26], and microwave-assisted hydrothermal synthesis [15,[27][28][29][30][31], which permits crystallization to take place at lower temperatures than typical for hydrothermal processes and with strongly reduced synthesis times. The hydrothermal methods are the most commonly used synthesis methods to form saponite.…”

Section: Introductionmentioning

confidence: 99%

Spectroscopic Studies of Synthetic and Natural Saponites: A Review

Kloprogge

Ponce

2021

Minerals

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Saponite is a trioctahedral 2:1 smectite with the ideal composition MxMg3AlxSi4−xO10(OH,F)2.nH2O (M = interlayer cation). Both the success of the saponite synthesis and the determination of its applications depends on robust knowledge of the structure and composition of saponite. Among the routine characterization techniques, spectroscopic methods are the most common. This review, thus, provides an overview of various spectroscopic methods to characterize natural and synthetic saponites with focus on the extensive work by one of the authors (JTK). The Infrared (IR) and Raman spectra of natural and synthetic saponites are discussed in detail including the assignment of the observed bands. The crystallization of saponite is discussed based on the changes in the IR and Raman spectra and a possible crystallization model is provided. Infrared emission spectroscopy has been used to study the thermal changes of saponite in situ including the dehydration and (partial) dehydroxylation up to 750 °C. 27Al and 29Si magic-angle-spinning nuclear magnetic resonance spectroscopy is discussed (as well as 11B and 71Ga for B- and Ga-Si substitution) with respect to, in particular, Al(IV)/Al(VI) and Si/Al(IV) ratios. X-ray photoelectron spectroscopy provides chemical information as well as some information related to the local environments of the different elements in the saponite structure as reflected by their binding energies.

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“…The development of microwave synthesis enables direct heating inside a reactor, which facilitates completing the reaction under a lower temperature and in a shorter time [9][10][11]. For example, Trujillano's group successfully synthesized saponite and saponite-like materials by using microwave irradiation at 180 • C [11][12][13][14].…”

Section: Introductionmentioning

confidence: 99%

Synthesis of Zn-Saponite Using a Microwave Circulating Reflux Method under Atmospheric Pressure

Hung

Fang³

et al. 2020

Minerals

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Smectite is a common clay mineral in nature. Due to its tendency to swell and its strong cation exchange capacity (CEC), smectite is prevalently used in industrial and technological applications. Numerous scholars have explored smectite synthesis, which usually involves autoclaving under high pressure. However, this approach requires an array of expensive equipment, and the process consumes time and energy. This study adopted self-developed equipment to synthesize zinc saponite (Zn-saponite), a type of trioctahedral smectite, using a microwave circulating reflux method under atmospheric pressure. Compared with the conventional hydrothermal methods, the proposed method entails fewer constraints regarding the synthesis environment and can be more easily applied to large-scale synthesis. The phase purity of the synthetic product was examined using X-ray diffraction and the CEC of the product was tested. The results revealed that the microwave circulating reflux method could synthesize Zn-saponite in 16 h under atmospheric pressure, and the CEC of the product reached 120 cmol(+)/kg. In addition, the product exhibited larger basal spacing and a 32% increase in CEC compared with Zn-saponite synthesized using a hot-plate under atmospheric pressure.

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Saponites containing divalent transition metal cations in octahedral positions — Exploration of synthesis possibilities using microwave radiation and NMR characterization

Cited by 14 publications

References 25 publications

Two-Dimensional Beidellite/Carbon Superlattice for Boosting Lithium-Ion Storage Performance

Two-Dimensional Beidellite/Carbon Superlattice for Boosting Lithium-Ion Storage Performance

Spectroscopic Studies of Synthetic and Natural Saponites: A Review

Synthesis of Zn-Saponite Using a Microwave Circulating Reflux Method under Atmospheric Pressure

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