One-Step Solid-State Reactions at Ambient Temperatures—A Novel Approach to Nanocrystal Synthesis

Ye, Xiang R.; Jia, Dian Zeng; Yu, Jinpu; Xin, Xin Q.; Chen, Xue-Tai

doi:10.1002/(sici)1521-4095(199908)11:11<941::aid-adma941>3.3.co;2-k

Cited by 51 publications

(67 citation statements)

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“…[15] Recently, we reported a simple direct method for the synthesis of nanostructured materials for use as cathodes in lithium cells. [16] The method produces nanometric oxalates [17] from highly hydrated salts ground in the presence of hydrated oxalic acid, which is followed by thermal decomposition of the precursors formed. The pyrolysis reaction preserves the nanometric size of the particles, even at high temperatures.…”

Section: Introductionmentioning

confidence: 86%

Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Arrebola

Caballero

Cruz

et al. 2006

Adv Funct Materials

222

128

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Li–Ni–Mn spinels of nominal composition LiNi0.5Mn1.5O4, which are functional materials for electrodes in high‐voltage lithium batteries, are prepared by thermal decomposition of mixed nanocrystalline oxalates obtained by grinding hydrated salts and oxalic acid in the presence of polyethyleneglycol 400. Their structure, microstructure, and texture are established from combined X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction, transmission electron microscopy (TEM), IR spectroscopy, and N2 absorption measurements. The polymer tailors the shape of particles, which adopt a nanorodlike morphology at low temperatures (400 °C). In fact, the nanorods consist of highly distorted oriented nanocrystals connected by a polymer‐based film as inferred from IR and XPS spectra. The electrochemical properties of spinels in this peculiar form are quite poor, mainly as a result of the high microstrain content of their nanocrystals. Raising the temperature up to 800 °C partially destroys the nanorods, which become highly crystalline nanoparticles approximately 80 nm in size. At this temperature, the polymer facilitates crystal growth; this leads to highly crystalline polyhedral nanoparticles as revealed from TEM images and microstrain data. Following functionalization as a cathode in lithium cells, this material exhibits a very good rate capability, coulombic efficiency, and capacity retention even upon cycling at voltages as high as 5 V. Moreover, it withstands fast‐charge–slow‐discharge processes, which is an important cycle‐life‐related property for commercial batteries.

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Section: Introductionmentioning

confidence: 86%

Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Arrebola

Caballero

Cruz

et al. 2006

Adv Funct Materials

222

128

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“…In 1998, this method was applied by our laboratory for the first time in the synthesis of various kinds of nanoparticles and for semiconductor materials in particular, including metal oxides, metal sulfides, etc. [11,12] At present, our group is interested in fabricating nanostructured materials with specific morphologies by using this convenient approach.…”

Section: Introductionmentioning

confidence: 99%

Rapid Synthesis of Amino Acid Polyoxometalate Nanotubes by One-Step Solid-State Chemical Reaction at Room Temperature

et al. 2006

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A novel and convenient method—solid‐state chemical reaction at room temperature—is reported for the synthesis of amino acid polyoxometalate nanotubes. As a convenient synthesis method for nanomaterials, it may open up a new pathway for the fabrication of organic–inorganic hybrid materials with nanotubular structure. Here, three novel tyrosine (Tyr) polyoxometalate nanotubes, (HTyr)3PMo12O40 · 3H2O, (HTyr)3PW12O40 · 3H2O, and (HTyr)4SiW12O40 · 5H2O are successfully synthesized via a one‐step solid‐state chemical reaction at room temperature. Elemental analysis confirms the rationality of composition for the samples. Infrared spectroscopy, X‐ray diffraction, and 31P magic‐angle spinning NMR results prove that the samples still possess Keggin‐type structures. Scanning and transmission electron microscopies suggest that the three samples are comprised of nanotubes with remarkably uniform shape and size, with diameters from 50 to 150 nm and lengths of up to several micrometers. Cyclic voltammograms of samples in 1 mol L–1 H2SO4 indicate that three redox waves correspond to three two‐electron processes resulting from the reduction/oxidation of the heteropoly anion.

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“…Others have attributed irregular particle shapes to the lack of solvent in this solid-state method that would promote diffusion-related crystal ripening. 20 After annealing, the MAZnO particle size increases relative to M-ZnO, and it also transforms into a rod-like shape (Fig. 3(b)).…”

Section: Resultsmentioning

confidence: 99%

“…16,20,30,[33][34][35][36][37] Since nanostructured materials made by solid-state metathesis have been utilized for solar cell, 35 cathode material, 38 UV-detector 36 and gas sensor 34,39,40 applications, it is important to recognize the tradeoffs between rapid production and long-term stability against atmospheric degradation.…”

Section: Discussionmentioning

confidence: 99%

Ambient Degradation of ZnO Powders: Does Surface Polarity Matter?

Cheng

Poduska

2014

ECS J. Solid State Sci. Technol.

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Comparing different synthesis methods to investigate ambient degradation differences among ZnO crystals with different crystal habits, we examined the effects of particle size, surface area, shape (surface polarity), and zeta (surface) potential. Neither surface polarity nor surface area, on their own, can account for the differences in the surface carbonation among differently synthesized ZnO samples. Our results demonstrate that surface dissolution and carbonation tendencies must be considered together, in the context of surface polarity, to explain different propensities toward degradation in ZnO powders.

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One-Step Solid-State Reactions at Ambient Temperatures—A Novel Approach to Nanocrystal Synthesis

Cited by 51 publications

References 0 publications

Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Rapid Synthesis of Amino Acid Polyoxometalate Nanotubes by One-Step Solid-State Chemical Reaction at Room Temperature

Ambient Degradation of ZnO Powders: Does Surface Polarity Matter?

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One-Step Solid-State Reactions at Ambient Temperatures—A Novel Approach to Nanocrystal Synthesis

Cited by 51 publications

References 0 publications

Crystallinity Control of a Nanostructured LiNi0.5Mn1.5O4 Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Crystallinity Control of a Nanostructured LiNi0.5Mn1.5O4 Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Rapid Synthesis of Amino Acid Polyoxometalate Nanotubes by One-Step Solid-State Chemical Reaction at Room Temperature

Ambient Degradation of ZnO Powders: Does Surface Polarity Matter?

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Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries

Crystallinity Control of a Nanostructured LiNi_0.5Mn_1.5O₄ Spinel via Polymer‐Assisted Synthesis: A Method for Improving Its Rate Capability and Performance in 5 V Lithium Batteries