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Transition metal tri-stibide/graphene composite material and preparation method thereof

A technology of composite materials and transition metals, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of poor electrochemical stability of antimony-based alloy materials, large volume changes of antimony-based alloys, and increased preparation costs, so as to improve electrochemical performance. Stability, low cost, evenly distributed effect

Inactive Publication Date: 2013-04-10
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, these antimony-based alloys are generally prepared by solid-state sintering method, which is expensive in equipment, complicated in process, and requires high raw materials, which greatly increases the preparation cost.
In addition, due to the large volume change of antimony-based alloys during charging and discharging, and the large particle size and uneven distribution of the material prepared by the solid-state method, the electrochemical stability of the obtained antimony-based alloy materials is poor.

Method used

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  • Transition metal tri-stibide/graphene composite material and preparation method thereof
  • Transition metal tri-stibide/graphene composite material and preparation method thereof
  • Transition metal tri-stibide/graphene composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1) The analytically pure SbCl 3 and CoCl 2 ·6H 2 O, according to the ratio of Co:Sb atomic ratio of 1:3, mixed in absolute ethanol to obtain CoSb 3 The meter concentration is the mixed solution of 0.2mol / L, and the mixed solution volume is 80 milliliters.

[0031] 2) After adding 130 mg of GO and 1.2 g of CTAB to the mixed solution in step 1), place it in an autoclave with a capacity of 100 ml (filling degree 80%, volume percentage), and add 8.5 g of reducing agent NaBH to the solution 4 , then seal immediately.

[0032] 3) Heating the reactor to 180°C and reacting for 24 hours.

[0033] 4) Naturally cool to room temperature after the reaction, collect the powdery reaction product at the bottom of the kettle, wash it with deionized water and absolute ethanol alternately and repeatedly for several times, then vacuum dry the powder at 110°C for 12 hours to obtain a composite material powder , the weight percent of graphene in the composite is 0.8%.

[0034] The X-ra...

Embodiment 2

[0037] 1) Analytical pure Sb(NO 3 ) 3 and CoCl 2 ·6H 2 O, NiSO 4 ·7H 2 O, according to the ratio of Co: Ni: Sb atomic ratio 0.9: 0.1: 3, mixed in deionized water to obtain Co 0.9 Ni 0.1 Sb 3 The meter concentration is the mixed solution of 0.05mol / L, and the mixed solution volume is 80 milliliters.

[0038] 2) Add 50 mg of GO and 0.5 g of PVP to the mixed solution in step 1) and place it in a high-pressure reactor with a capacity of 100 ml (filling degree 80%, volume percentage), and add 2 g of reducing agent to the solution KBH 4 , then seal immediately.

[0039] 3) Heating the reactor to 160°C and reacting for 48 hours.

[0040] 4) Naturally cool to room temperature after the reaction, collect the powdery reaction product at the bottom of the kettle, wash it with deionized water and absolute ethanol alternately and repeatedly for several times, then vacuum dry the powder at 110°C for 12 hours to obtain a composite material powder , the weight percent of graphene in ...

Embodiment 3

[0043] 1) The analytically pure SbCl 3 , NiSO 4 ·7H 2 O and FeSO 4 ·7H 2 O is mixed in anhydrous ethylene glycol according to the ratio of Ni:Fe:Sb atomic ratio of 0.5:0.5:3 to obtain Ni 0.5 Fe 0.5 Sb 3 The meter concentration is the mixed solution of 0.15mol / L, and the mixed solution volume is 80 milliliters.

[0044] 2) Add 200 mg of GO and 1.3 g of SDS to the mixture in step 1) and place it in a 100 ml autoclave (filling degree 80%, volume percentage), and add 9 g of reducing agent to the solution NaBH 4 , then seal immediately.

[0045] 3) Heating the reactor to 200°C and reacting for 36 hours.

[0046] 4) Naturally cool to room temperature after the reaction, collect the powdery reaction product at the bottom of the kettle, wash it with deionized water and absolute ethanol alternately and repeatedly for several times, then vacuum dry the powder at 110°C for 12 hours to obtain a composite material powder , the weight percent of graphene in the composite is 1.66%....

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Abstract

The invention discloses a transition metal tri-stibide / graphene composite material, which has the composition of MxSb3 / G, wherein M represents a transition metal element from a VIIIB group, x is more than or equal to 0.95 and is less than or equal to 1.05, and G represents graphene. Because of the dispersing and loading effects of the graphene, the transition metal tri-stibide in the composite material can be distributed uniformly, and the stability of the transition metal tri-stibide in the process of charging and discharging can be effectively improved. The invention also discloses a preparation method of the composite material through a one-step hydro-thermal method or one-step solvent thermal method, which has the advantages of simple process, low cost, short cycle, low energy consumption and the like.

Description

technical field [0001] The invention relates to the field of composite materials for lithium ion batteries, in particular to a transition metal antimonide / graphene composite material and a one-step preparation method thereof. Background technique [0002] Lithium-ion batteries have the advantages of high working voltage, high energy density, and good safety performance. Therefore, they are widely used in portable electronic products such as digital cameras, mobile phones, and notebook computers. They also have application prospects for electric bicycles and electric vehicles. The anode materials of current commercial lithium-ion batteries are graphite and other forms of carbon materials. Since the theoretical capacity of graphite is only 372mAh g -1 , and the lithium intercalation potential is low, which limits its application range. Compared with carbon materials such as graphite, some antimony-based alloys have better lithium intercalation potential and higher mass ratio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/48H01M4/62H01M4/1391H01M4/131
CPCY02E60/12Y02E60/122Y02E60/10
Inventor 谢健郑云肖刘双宇宋文涛曹高劭赵新兵
Owner ZHEJIANG UNIV