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One-Step Synthesis of Titanium Oxyhydroxy-Fluoride Rods and Research on the Electrochemical Performance for Lithium-ion Batteries and Sodium-ion Batteries.

Li B, Gao Z, Wang D, Hao Q, Wang Y, Wang Y, Tang K - Nanoscale Res Lett (2015)

Bottom Line: Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method.Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions.Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemistry and Hefei National Laboratory for Physical Science at Microscale, University of Science and Technology of China, Hefei, Anhui, 230026, People's Republic of China.

ABSTRACT
Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method. The structure, morphology, and component of the products were characterized by X-ray powder diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), ion chromatograph, energy-dispersive X-ray (EDX) analyses, and so on. Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions. With one-dimension channels for Li/Na intercalation/de-intercalation, the electrochemical performance of titanium oxyhydroxy-fluoride for both lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs) was also studied. Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

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SEM images of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O with different morphologies: long rods (a), short rods (b) and hexagonal rods (c); TEM image (d), HRTEM image (e) and the corresponding FFT image (f) of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods; the arrows in the HRTEM image (e) indicate the 0.38 nm interfringe spacing, and the arrows in the corresponding FFT image (f) indicate the spots which represent different lattice planes of the product
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Fig3: SEM images of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O with different morphologies: long rods (a), short rods (b) and hexagonal rods (c); TEM image (d), HRTEM image (e) and the corresponding FFT image (f) of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods; the arrows in the HRTEM image (e) indicate the 0.38 nm interfringe spacing, and the arrows in the corresponding FFT image (f) indicate the spots which represent different lattice planes of the product

Mentions: The morphology and structure features of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O particles are also investigated through the analyses of scanning electron microscopy (SEM), TEM, HRTEM images and the corresponding FFT image. The size of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods (Fig. 3a) is approx 2 μm long and 100–500 nm in diameter; the typical long rod with the regular shape is shown in Fig. 3d. For short TiO0.9(OH)0.9F1.2 · 0.59H2O rods (Fig. 3b), the length ranges from 700 to 1300 nm and the diameter ranges from 250 to 400 nm. All the TiO0.9(OH)0.9F1.2 · 0.59H2O rods with different morphologies are synthesized under the same condition with the only difference of the ethanol volume. Actually, if only the volume of deionized water is changed (from 1.20 mL to 0.15 mL), another compound hexagonal TiOF2 is synthesized. The sole difference between the synthesis of TiO0.9(OH)0.9F1.2 · 0.59H2O and hexagonal TiOF2 ,i.e., the volume of deionized water indicates that during the synthesis of TiO0.9(OH)0.9F1.2 · 0.59H2O, more hydrolysis reactions of TiF4 occur and Ti4+ binds the generated hydroxy to form the final product with the HTB structure. In other words, the hydroxy groups are considered to be very important for the firm HTB structure. It can also be concluded that the deionized water volume of reaction decides the structure of the products while the ethanol volume plays a significant role in affecting the morphology. The 0.38-nm interfringe spacing in Fig. 3e corresponds to the (002) lattice plane of TiO0.9(OH)0.9F1.2 · 0.59H2O. The vertical (120) and (002) lattice plane in Fig. 3e are also confirmed by the FFT image (Fig. 3f).Fig. 3


One-Step Synthesis of Titanium Oxyhydroxy-Fluoride Rods and Research on the Electrochemical Performance for Lithium-ion Batteries and Sodium-ion Batteries.

Li B, Gao Z, Wang D, Hao Q, Wang Y, Wang Y, Tang K - Nanoscale Res Lett (2015)

SEM images of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O with different morphologies: long rods (a), short rods (b) and hexagonal rods (c); TEM image (d), HRTEM image (e) and the corresponding FFT image (f) of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods; the arrows in the HRTEM image (e) indicate the 0.38 nm interfringe spacing, and the arrows in the corresponding FFT image (f) indicate the spots which represent different lattice planes of the product
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Related In: Results  -  Collection

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Fig3: SEM images of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O with different morphologies: long rods (a), short rods (b) and hexagonal rods (c); TEM image (d), HRTEM image (e) and the corresponding FFT image (f) of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods; the arrows in the HRTEM image (e) indicate the 0.38 nm interfringe spacing, and the arrows in the corresponding FFT image (f) indicate the spots which represent different lattice planes of the product
Mentions: The morphology and structure features of titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O particles are also investigated through the analyses of scanning electron microscopy (SEM), TEM, HRTEM images and the corresponding FFT image. The size of long TiO0.9(OH)0.9F1.2 · 0.59H2O rods (Fig. 3a) is approx 2 μm long and 100–500 nm in diameter; the typical long rod with the regular shape is shown in Fig. 3d. For short TiO0.9(OH)0.9F1.2 · 0.59H2O rods (Fig. 3b), the length ranges from 700 to 1300 nm and the diameter ranges from 250 to 400 nm. All the TiO0.9(OH)0.9F1.2 · 0.59H2O rods with different morphologies are synthesized under the same condition with the only difference of the ethanol volume. Actually, if only the volume of deionized water is changed (from 1.20 mL to 0.15 mL), another compound hexagonal TiOF2 is synthesized. The sole difference between the synthesis of TiO0.9(OH)0.9F1.2 · 0.59H2O and hexagonal TiOF2 ,i.e., the volume of deionized water indicates that during the synthesis of TiO0.9(OH)0.9F1.2 · 0.59H2O, more hydrolysis reactions of TiF4 occur and Ti4+ binds the generated hydroxy to form the final product with the HTB structure. In other words, the hydroxy groups are considered to be very important for the firm HTB structure. It can also be concluded that the deionized water volume of reaction decides the structure of the products while the ethanol volume plays a significant role in affecting the morphology. The 0.38-nm interfringe spacing in Fig. 3e corresponds to the (002) lattice plane of TiO0.9(OH)0.9F1.2 · 0.59H2O. The vertical (120) and (002) lattice plane in Fig. 3e are also confirmed by the FFT image (Fig. 3f).Fig. 3

Bottom Line: Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method.Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions.Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemistry and Hefei National Laboratory for Physical Science at Microscale, University of Science and Technology of China, Hefei, Anhui, 230026, People's Republic of China.

ABSTRACT
Titanium oxyhydroxy-fluoride, TiO0.9(OH)0.9F1.2 · 0.59H2O rods with a hexagonal tungsten bronze (HTB) structure, was synthesized via a facile one-step solvothermal method. The structure, morphology, and component of the products were characterized by X-ray powder diffraction (XRD), thermogravimetry (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), inductively coupled plasma optical emission spectroscopy (ICP-OES), ion chromatograph, energy-dispersive X-ray (EDX) analyses, and so on. Different rod morphologies which ranged from nanoscale to submicron scale were simply obtained by adjusting reaction conditions. With one-dimension channels for Li/Na intercalation/de-intercalation, the electrochemical performance of titanium oxyhydroxy-fluoride for both lithium-ion batteries (LIBs) and sodium-ion batteries (SIBs) was also studied. Electrochemical tests revealed that, for LIBs, titanium oxyhydroxy-fluoride exhibited a stabilized reversible capacity of 200 mAh g(-1) at 25 mA g(-1) up to 120 cycles in the electrode potential range of 3.0-1.2 V and 140 mAh g(-1) at 250 mA g(-1) up to 500 cycles, especially; for SIBs, a high capacity of 100 mAh g(-1) was maintained at 25 mA g(-1) after 115 cycles in the potential range of 2.9-0.5 V.

No MeSH data available.


Related in: MedlinePlus