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Preparation method of nitrogen-doping carbon substrate-supported Fe3O4 composite material sodium-ion battery negative electrode material

A sodium ion battery and ferric oxide technology, applied in the field of electrochemistry, can solve the problems of poor conductivity, unstable cycle performance, low current capacity, etc., to improve stability, maintain the original shape, and relieve volume expansion. Effect

Active Publication Date: 2017-03-22
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims at the problems in the prior art, and the purpose is to propose a method for preparing a nitrogen-doped carbon matrix supporting ferric oxide composite material sodium ion battery negative electrode material, which can effectively solve the problem of Fe 3 o 4 Poor conductivity, unstable cycle performance due to large volume expansion during charging and discharging, and also solves the problem of low high-current capacity. The preparation method is simple and easy to operate, does not add any organic matter, and is low in cost and environmentally friendly. , is expected to realize industrial production

Method used

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  • Preparation method of nitrogen-doping carbon substrate-supported Fe3O4 composite material sodium-ion battery negative electrode material
  • Preparation method of nitrogen-doping carbon substrate-supported Fe3O4 composite material sodium-ion battery negative electrode material
  • Preparation method of nitrogen-doping carbon substrate-supported Fe3O4 composite material sodium-ion battery negative electrode material

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 1) Weigh urea and ammonium ferric citrate with a mass ratio of 4:1, dissolve the urea and ammonium ferric citrate in deionized water, and ultrasonicate for 30 minutes at a power of 300W to make ammonium ferric citrate with a concentration of 0.8mg / mL suspension A;

[0025] 2) Adjust the pH value of the suspension A to 3, then pour it into a watch glass, put it in the refrigerator and freeze it at -20°C for 12 hours to obtain a solid solid B;

[0026] 3) Put the frozen solid B into a freeze dryer and dry at -50°C for 12 hours to obtain a completely dried product C;

[0027] 4) Pour product C into a quartz crucible, wrap the quartz crucible with tin foil, then put it into a glass tube for oxides, set the temperature and holding time of the vacuum tube furnace to 5°C min -1 The heating rate was increased to 500 °C, and pyrolysis was carried out for 2 h to obtain the final product nitrogen-doped carbon matrix supported Fe 3 o 4 Composite sodium ion battery anode material...

Embodiment 2

[0030] 1) Weigh urea and ferric acetate with a mass ratio of 4:3, dissolve the urea and ferric acetate in deionized water, and ultrasonicate for 30 min at a power of 300W to prepare a suspension with a ferric acetate concentration of 0.8 mg / mL. Turbid liquid A;

[0031] 2) Adjust the pH value of the suspension A to 3, then pour it into a watch glass, put it in the refrigerator and freeze it at -20°C for 12 hours to obtain a solid solid B;

[0032] 3) Put the frozen solid B into a freeze dryer and dry at -50°C for 12 hours to obtain a completely dried product C;

[0033] 4) Pour the product C into a quartz crucible, wrap the quartz crucible with tin foil, then put it into a glass tube for oxides, set the vacuum tube furnace temperature and holding time at 5°C min -1 The heating rate was increased to 500 °C, and pyrolysis was carried out for 2 h to obtain the final product nitrogen-doped carbon matrix supported Fe 3 o 4 Composite sodium ion battery anode material.

[0034] T...

Embodiment 3

[0036] 1) Dissolve urea and soluble trivalent complex iron salt in deionized water at a mass ratio of 4:1 to 4:4, and sonicate for 10 minutes at a power of 300W to make a soluble trivalent complex iron salt with a concentration of 2mg / mL Suspension A; wherein, the soluble trivalent complex iron salt is ferric ammonium oxalate.

[0037] 2) Adjust the pH value of the suspension A to 5 and freeze it in the refrigerator at -20°C for 24 hours to obtain the solid B;

[0038] 3) freeze-dry solid B in a freeze dryer at -50°C for 24 hours to obtain product C;

[0039] 4) Pour the product C into a quartz crucible, wrap the quartz crucible with tin foil, and then heat it in a vacuum tube furnace at 10°C min -1 The heating rate was increased from room temperature to 400 °C and pyrolyzed for 2 h to obtain a nitrogen-doped carbon matrix supported Fe 3 o 4 Composite sodium ion battery anode material.

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Abstract

A preparation method of a nitrogen-doping carbon substrate-supported Fe3O4 composite material sodium-ion battery negative electrode material comprises the steps of dissolving urea and a soluble trivalent complexing ferric salt in deionized water according to a mass ratio being (4:1)-(4:4), and uniformly mixing the urea and the soluble trivalent complexing ferric salt to prepare a solution A; freezing the solution A to obtain a solid B after a pH value of the solution A is adjusted to 3-7; and pyrolyzing the solid B under a temperature of 400-700 DEG C after the solid B is frozen and dried. The raw material adopted by the preparation method has the advantages of environmental friendliness, wide source, low cost and the like, and the preparation method is easy to operate; the trivalent ferric salt is used as an iron source and a nitrogen-doping nitrogen source, active sites on a Fe3O4 electrode material are increased due to nitrogen doping, and intercalation and de-intercalation of sodium ions are facilitated; any surfactant is not added, reaction is completed at one time, and subsequent processing is not needed; and the nitrogen-doping carbon substrate-supported Fe3O4 composite material prepared according to the method is stable in cycle performance, and the conductivity of the nitrogen-doping carbon substrate-supported Fe3O4 composite material is improved.

Description

technical field [0001] The invention belongs to the technical field of electrochemistry, and in particular relates to a preparation method of a nitrogen-doped carbon matrix supporting ferric oxide composite material sodium ion battery negative electrode material. Background technique [0002] In chemical energy storage, compared with lithium-ion batteries, the raw material cost of sodium-ion batteries is lower than that of lithium-ion batteries, and the half-cell potential is higher than that of lithium-ion batteries. It is suitable to use electrolytes with lower decomposition voltages, so the safety performance is significantly better than that of lithium-ion batteries. Lithium Ion Battery. Studies have shown that the transition metal oxide Fe 3 o 4 As a negative electrode material, the theoretical capacity is as high as 926mAhg -1 , and Fe 3 o 4 Wide distribution, low cost, non-toxic and environmental protection. Therefore, Fe 3 o 4 It is a very promising anode mat...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/52H01M4/62H01M10/054
CPCH01M4/364H01M4/523H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 曹丽云党欢黄剑锋齐慧李嘉胤周磊程娅伊罗艺佳
Owner SHAANXI UNIV OF SCI & TECH
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