Tuning Nanomaterials' Characteristics by a Miniaturized In‐Line Dispersion–Precipitation Method: Application to Hydrotalcite Synthesis

Abelló, Sònia; Pérez‐Ramírez, Javier

doi:10.1002/adma.200600673

Cited by 56 publications

(38 citation statements)

References 16 publications

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“…[52] Briefly, aqueous solutions MgA C H T U N G T R E N N U N G (NO 3 ) 2 ·6 H 2 O (0.75 m) and AlA C H T U N G T R E N N U N G (NO 3 ) 3 ·9 H 2 O (0.25 m) and the precipitating agent (NaOH + Na 2 CO 3 , each 1 m ) were fed continuously at room temperature by means of peristaltic pumps into a home-made micro-reactor (effective volume % 6 cm 3 ). The pH was kept at 10 by using an in-line probe that measured the pH of the slurry directly at the outlet of the micro-reactor and was connected to one of the pumps for pH control.…”

Section: Methodsmentioning

confidence: 97%

Memory Effect of Activated Mg–Al Hydrotalcite: In Situ XRD Studies during Decomposition and Gas‐Phase Reconstruction

Pérez‐Ramírez

Abelló

Pers

2007

Chemistry A European J

138

109

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The thermal decomposition of Mg-Al hydrotalcite and the subsequent reconstruction of the decomposed products in the presence of water vapor (2 vol. % H(2)O in N(2)) have been investigated by in situ XRD. Thermographic analysis and temperature-programmed desorption MS results complemented the diffraction data. Valuable mechanistic and kinetic insights into these processes, which are of prime importance for optimal activation of this type of material for catalytic applications, were obtained. Hydrotalcite decomposition to the mixed oxide proceeds via formation at 423-473 K of an intermediate phase, consisting of a highly disordered, dehydrated, layered structure. The latter evolves by removal of interlayer water on heating, causing a shrinking of the interlayer space (it is up to 45 % smaller than in the as-synthesized hydrotalcite). Above 623 K, Mg(Al)O(x) oxide with the periclase structure is formed. Reversion of the intermediate dehydrated structure to hydrotalcite upon contact with water vapor is complete and very fast at room temperature. Recovery of hydrotalcite from the oxide calcined at 723 K is two orders of magnitude slower than rehydration of the intermediate layered structure and one order of magnitude slower than the typically practiced liquid-phase reconstruction. In contrast to the decomposition, the reconstruction mechanism does not involve an intermediate phase. The gas-phase rehydration and reconstruction was interrupted above 303 K. This is attributed to the poor wetting of the surface of the decomposed materials induced by hampered H(2)O adsorption above room temperature at the water vapor pressure applied. The Avrami-Erofe'ev model describes the reconstruction kinetics well.

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Section: Methodsmentioning

confidence: 97%

Memory Effect of Activated Mg–Al Hydrotalcite: In Situ XRD Studies during Decomposition and Gas‐Phase Reconstruction

Pérez‐Ramírez

Abelló

Pers

2007

Chemistry A European J

138

109

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“…[ 29 ] The above comparisons suggest that the precipitation of Al nanograins and amorphization of Li 3 AlH 6 matrix in the SSPP Li‐Al‐H anode is mainly attributed to the synergetic effect of fast short‐circuited electrochemical reaction (fast nucleation) and slow solid‐state long‐distance diffusion (slow growth). [ 30,31 ]…”

Section: Resultsmentioning

confidence: 99%

Solid‐State Prelithiation Enables High‐Performance Li‐Al‐H Anode for Solid‐State Batteries

Pang

Wang

Shi

et al. 2020

Advanced Energy Materials

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Lithium alanates exhibit high theoretical specific capacities and appropriate lithiation/delithiation potentials, but suffer from poor reversibility, cycling stability, and rate capability due to their sluggish kinetics and extensive side reactions. Herein, a novel and facile solid‐state prelithiation approach is proposed to in situ prepare a Li3AlH6‐Al nanocomposite from a short‐circuited electrochemical reaction between LiAlH4 and Li with the help of fast electron and Li‐ion conductors (C and P63mc LiBH4). This nanocomposite consists of dispersive Al nanograins and an amorphous Li3AlH6 matrix, which enables superior electrochemical performance in solid‐state cells, as much higher specific capacity (2266 mAh g−1), Coulombic efficiency (88%), cycling stability (71% retention in the 100th cycle), and rate capability (1429 mAh g−1 at 1 A g−1) are achieved. In addition, this nanocomposite works well in the solid‐state full cell with LiCoO2 cathode, demonstrating its promising application prospects. Mechanism analysis reveals that the dispersive Al nanograins and amorphous Li3AlH6 matrix can dramatically enhance the lithiation and delithiation kinetics without side reactions, which is mainly responsible for the excellent overall performance. Moreover, this solid‐state prelithiation approach is general and can also be applied to other Li‐poor electrode materials for further modification of their electrochemical behavior.

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“…4(a)]. XRD analysis and SEM observation confirmed the formation of LDH nanocrystals Until now, the preparation of nano LDH has been performed by specific synthesis steps, such as a colloid mill process followed by aging, 39) controlled hydrothermal treatment, 40) in-line dispersionprecipitation, 41) and hydrothermal treatment with a continuous flow. 42) More recently, an aqueous synthesis of nano-LDH suspension by using micelles as a nano reaction-pool was reported.…”

Section: Scheme Ii: Hydroxide Nanoclusters and Their Use As Nanobuildmentioning

confidence: 99%

Aqueous synthesis of metal hydroxides with controllable nano/macro architectures

Tokudome

2017

J. Ceram. Soc. Japan

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This review briefly describes recent advances on the synthesis of metal hydroxide nanomaterials and their assembly into 3D architectures toward applications of catalysis, adsorption, and energy conversion. The discussion is mainly dedicated to the synthesis strategies toward nanohydroxide-based functional materials. A special attention is focused on two reaction schemes for the preparations of: (1) macroporous (hydr)oxides monoliths and (2) monodispersed hydroxide nanoclusters and mesoporous hydroxides.

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Tuning Nanomaterials' Characteristics by a Miniaturized In‐Line Dispersion–Precipitation Method: Application to Hydrotalcite Synthesis

Cited by 56 publications

References 16 publications

Memory Effect of Activated Mg–Al Hydrotalcite: In Situ XRD Studies during Decomposition and Gas‐Phase Reconstruction

Memory Effect of Activated Mg–Al Hydrotalcite: In Situ XRD Studies during Decomposition and Gas‐Phase Reconstruction

Solid‐State Prelithiation Enables High‐Performance Li‐Al‐H Anode for Solid‐State Batteries

Aqueous synthesis of metal hydroxides with controllable nano/macro architectures

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