Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8

A self-assembly, nanosheet technology, applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of few reports and few electrochemical performances, and achieve good electrochemical performance, low preparation cost, and cheap raw materials. easy-to-get effect

Active Publication Date: 2016-09-07
SHAANXI UNIV OF SCI & TECH
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AI Technical Summary

Problems solved by technology

(NH 4 ) 2 V 3 o 8 It belongs to the tetragonal crystal system and has a typical two-dimensional layered structure [Liu G, Greedan J E. Magnetic properties offresnoite-type vanadium oxides: A 2 V 3 o 8 (A=K,Rb,NH 4 )[J].Journal of Solid State Chemistry,1995,114(2):499–505], but there are few reports about its liquid phase, especially hydrothermal synthesis, and even fewer reports about its electrochemical performance

Method used

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  • Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8
  • Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8

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preparation example Construction

[0020] A nanosheet self-assembled prism (NH 4 ) 2 V 3 o 8 The preparation method comprises the following steps:

[0021] (1) Dissolve the vanadium source in deionized water to prepare a suspension A. At this time, the concentration of vanadium is 0.108-1mol / L, then add ammonia water and organic alcohol to the suspension A in turn, and stir until the vanadium source is completely dissolved. , to obtain solution B. The vanadium source is vanadium pentoxide, sodium metavanadate or ammonium metavanadate; the organic alcohol is ethylene glycol, ethanol or isopropanol.

[0022] Further, the stirring method is magnetic stirring or ultrasonic vibration. The speed of the magnetic stirring is 400-900 r / min; the ultrasonic vibration time is 10-60 min.

[0023] (2) Put solution B into a hydrothermal reaction kettle, place it in a homogeneous reactor, and react for 6-24 hours at a temperature of 120-200°C.

[0024] (3) Cool naturally after the reaction is complete, and then use suct...

Embodiment 1

[0027] Step 1: Put 1gV 2 o 5 Dissolve in deionized water to prepare suspension A. At this time, the concentration of vanadium is 0.3mol / L, then add 9mL ammonia water to suspension A and ultrasonically vibrate for 10min, then add 10mL ethylene glycol and ultrasonically vibrate for 30min until V 2 o 5 Completely dissolved to obtain solution B. Vanadium pentoxide can be replaced by sodium metavanadate or ammonium metavanadate; ethylene glycol can be replaced by ethanol or isopropanol.

[0028] Step 2: Put solution B into a hydrothermal reaction kettle, place it in a homogeneous reactor, and react for 12 hours at a temperature of 160°C.

[0029]Step 3: Cool naturally after the reaction is complete, then wash the product 3 times with water and 3 times with alcohol, then collect the washed product and place it in an oven, and dry it at 60°C for 12 hours to obtain nanosheets Self-assembled prisms (NH 4 ) 2 V 3 o 8 .

[0030] From figure 1 It can be seen that the (NH 4 ) 2...

Embodiment 2

[0033] step one:

[0034] Will 0.5g V 2 o 5 Dissolve in deionized water to prepare suspension A. At this time, the concentration of vanadium is 0.108mol / L, then add 3mL ammonia water to suspension A and stir magnetically for 5min, then add 5mL ethylene glycol and magnetically stir for 10min until V 2 o 5 Completely dissolved to obtain solution B. The rotating speed of magnetic stirring is 400r / min~600r / min. Vanadium pentoxide can be replaced by sodium metavanadate or ammonium metavanadate; ethylene glycol can be replaced by ethanol or isopropanol.

[0035] Step 2: Put solution B into a hydrothermal reaction kettle, place it in a homogeneous reactor, and react for 6 hours at a temperature of 120°C.

[0036] Step 3: Cool naturally after the reaction is complete, then wash the product twice with water and twice with alcohol, then collect the washed product, place it in an oven, and dry it at 80°C for 6 hours to obtain nanosheets Self-assembled prisms (NH 4 ) 2 V 3 o 8 ....

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Abstract

The invention provides a preparation method of a nanosheet self-assembled frustum-shaped (NH4)2V3O8. The preparation method comprises the following steps of firstly, dissolving vanadium pentoxide in deionized water to prepare a suspension liquid A, afterwards adding ammonia water and ethylene glycol to the suspension liquid A, and magnetically stirring the suspension liquid until the suspension liquid is clear to obtain a solution B; secondly, loading the solution B in a hydrothermal reaction kettle, placing the hydrothermal reaction kettle in a homogeneous reaction device, and naturally cooling the homogeneous reaction device after hydrothermal reaction; and finally, washing the product with water and alcohol, collecting and drying the product to obtain the nanosheet self-assembled frustum-shaped (NH4)2V3O8. The method process is simple and is easy to control, and the prepared (NH4)2V3O8 is uniform in microcrystal chemical constitution and relatively high in purity, and shows favorable electrochemical performance when taken as a positive electrode material of a lithium ion battery. Further, by the method, a large-size device and a severe reaction condition are not needed, the raw material is low in cost and is available, the preparation cost is low, the yield is high, subsequent processing is not needed, and the method is friendly to an environment and can be suitable for mass production.

Description

【Technical field】 [0001] The invention relates to a preparation method of an ion secondary battery cathode material, in particular to a nanosheet self-assembled prism (NH 4 ) 2 V 3 o 8 method of preparation. 【Background technique】 [0002] Lithium-ion secondary batteries have the advantages of high voltage, large specific energy, long cycle life, stable discharge performance, good safety, no pollution, and wide operating temperature range, and have become a research hotspot in recent years [Tarascon J M, Armand M. Issues and challenges facing rechargeable lithium batteries [J]. Nature, 2001, 414(6861): 359-367]. Cathode materials account for 35-40% of the cost of the entire lithium-ion battery, which is the key to development. Commercial cathode materials (such as LiCoO 2 , LiMn 2 o 4 、LiFePO 4 ) capacity is generally less than 150mAh·g -1 , far from meeting the requirements of high-energy and high-power batteries in the future. LiV 3 o 8 With high capacity (the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525B82Y30/00B82Y40/00C01G31/00
CPCB82Y30/00B82Y40/00C01G31/00H01M4/58H01M10/0525Y02E60/10
Inventor 黄剑锋李文斌王海静李瑞梓费杰曹丽云任一杰闻稼宝程呈罗晓敏
Owner SHAANXI UNIV OF SCI & TECH
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