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Preparation method for nano multilayer nickelous hydroxide hollow tube

A multi-layer, hollow tube technology, applied in the field of nanomaterials, can solve the problems of difficult doping, low output, and difficult mass production, etc., and achieve the effect of simple experimental process, cheap and easy-to-obtain raw materials, and convenient operation

Inactive Publication Date: 2008-10-15
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhao et al. found that α-Ni(OH) could be successfully obtained by homogeneous precipitation in the presence of urea. 2 (ZhaoY L, Wang J M, Chen H, Pan T, Int.J.Hydrogen Energy 2004, 29, 889), but this method is difficult to accurately control the shape and size of the product
Indira et al. electrochemically synthesized doped Al 3+ 、Cr 3+ , Mn 3+ , Fe 3+ α-Ni(OH) 2 , found Al 3+ Substituted α-Ni(OH) 2 Coulombic efficiency is the highest (Indira L, Mridula D, Vishnu Kamath P.Journal of Power Sources1994, 52 (1), 93), but this method usually requires expensive equipment, and is limited by equipment, it is difficult to accurately determine the amount of doping Control, α-Ni(OH) 2 The output is low and it is not easy to produce in large quantities
As another example, Cao et al reported the preparation of dandelion-like α-Ni(OH) by inverse emulsion / microemulsion method 2 Structure (CaoM, He X, Chen J, Hu C.Cryst.Growth Des.2007, 7, 170), this method is influenced by various templates, the synthesized α-Ni(OH) 2 The purity of the product is limited, which affects the performance of the product
Although there are various morphologies of α-Ni(OH) 2 Nanostructures were prepared successfully, but about nanoscale multi-level α-Ni(OH) 2 Hollow tubes remain unreported

Method used

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  • Preparation method for nano multilayer nickelous hydroxide hollow tube
  • Preparation method for nano multilayer nickelous hydroxide hollow tube
  • Preparation method for nano multilayer nickelous hydroxide hollow tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare 0.001mol nickel chloride hexahydrate and 0.12mol ethylene glycol and put them into a 40mL stainless steel reaction kettle lined with polytetrafluoroethylene, add 0.45g sodium acetate, stir with a glass rod until completely dissolved, and form a light green transparent mixture solution. Close and tighten the reactor, put it into an oven, set the temperature at 190°C, take out the reactor after 3 hours of reaction, and let it cool naturally. Subsequently, the reaction precipitate was poured out, washed three times with distilled water, and then washed three times with absolute ethanol. Finally, it was dried in a vacuum oven at 60°C for 8 hours, and the samples were collected and stored in a desiccator. figure 1 The nano-multilayered α-Ni(OH) prepared for this embodiment 2 The X-ray diffraction spectrum of the hollow tube shows that the obtained powder is α-Ni(OH) with a hydrotalcite structure 2 , the diffraction peaks in the spectrogram correspond to the crysta...

Embodiment 2

[0023] Prepare the molar ratio of nickel chloride hexahydrate and ethylene glycol as 1:120, put it into a PTFE-lined stainless steel reaction kettle with a volume of 40mL, add 0.45g of sodium acetate, stir with a glass rod until completely dissolved, and form Light green transparent mixed solution. Close and tighten the reactor, put it into an oven, set the temperature at 170°C, take out the reactor after 6 hours of reaction, and let it cool naturally. Subsequently, the reaction precipitate was poured out, washed three times with distilled water, and then washed three times with absolute ethanol. Finally, it was dried in a vacuum oven at 70°C, and the collected samples were stored in a desiccator. TEM image ( Figure 4 a) shows that the outer diameter of the prepared nanotube is 1.6-1.9 μm, and the outer wall of the tube is made of a large amount of soft 30-40nm thick α-Ni(OH) 2 Composed of nanosheets, the aspect ratio can be as high as 10. Figure 4 The inset in a is a si...

Embodiment 3

[0025] Prepare the molar ratio of nickel chloride hexahydrate and ethylene glycol as 1:80, put it into a stainless steel reaction kettle with a polytetrafluoroethylene liner with a volume of 40mL, add 0.45g of sodium acetate, stir with a glass rod until it is completely dissolved, and form Light green transparent mixed solution. Close and tighten the reactor, put it into an oven, set the temperature at 160°C, take out the reactor after 6 hours of reaction, and let it cool naturally. Subsequently, the reaction precipitate was poured out, washed three times with distilled water, and then washed three times with absolute ethanol. Finally, it was dried in a vacuum oven at 70°C, and the collected samples were stored in a desiccator. TEM image ( Figure 4 b) It shows that the outer diameter of the prepared nanotube is 500-600nm, and the outer wall of the tube is composed of a large number of soft, interlaced ~20nm thick α-Ni(OH) 2 Nanosheets are self-assembled.

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Abstract

The invention provides a wet chemical method for preparing a nanometer multilayer structured nickel hydroxide hollow tube, which is mainly characterized in that the method takes inorganic salt containing nickel as a nickel source, and glycol as a complexing agent to obtain the nanometer multilayer structured Alpha-Ni(OH)2 hollow tube in one step through thermal reaction of the solvent; during the preparation process, neither templates nor surface active agents are needed; the Alpha-Ni(OH)2 hollow tube which is 0.3Mum to 2.5Mum in diameter and the outer wall of which is composed of a large quantity of soft and 20nm to 50nm thick Alpha-Ni(OH)2 nano-plates can be obtained through the thermal reaction of the solvent at the temperature of 150 to 190 DEG C for 3 to 8 hours. The preparation method adopts the environment-friendly glycol as the complexing agent to prepare the Alpha-Ni(OH)2 hollow tube that has a large specific surface and a hollow internal structure and is expected to be widely applied in such fields as battery, ultracapacitor materials and environment-friendly automobiles. The method is characterized in simple equipment and process, low production cost, suitability for industrialized production, environment-friendliness, etc.

Description

technical field [0001] The invention relates to a method for preparing a nanometer multilayer nickel hydroxide hollow tube, and the prepared hollow tube can be used for preparing electrodes and supercapacitor electronic devices. It belongs to the field of nanomaterials. Background technique [0002] Ni(OH) 2 It is an important alkaline battery (Ni / Cd, Ni / H 2 , Ni / Zn, Ni / MH, Ni / Fe) positive electrode active materials, which play a key role in the capacity, life and electrochemical performance of the battery. Nickel hydroxide has two crystal structures: α-Ni(OH) 2 and β-Ni(OH) 2 , and the corresponding charge states are γ-NiOOH and β-NiOOH, respectively. At present, the positive electrode of nickel-metal hydride batteries uses β-Ni(OH) 2 / β-NiOOH electric pair cycle, the theoretical electron transfer number of nickel atom in the electrochemical reaction process is 1, and the theoretical specific capacity is 289mAh g -1 . Due to β-Ni(OH) 2 The theoretical specific capa...

Claims

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Application Information

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IPC IPC(8): C01G53/04B82B1/00B82B3/00
Inventor 高濂宋雪峰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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