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Preparation method for electrode with three-dimensional structure formed by coating nickel sulfide by fold graphene through self-repairing

A graphene and self-repairing technology, which is applied in the field of nanomaterials and electrochemistry, can solve the problems of excessive changes in electrode structure and low conductivity, and achieve the effect of fast charging and discharging with large currents

Active Publication Date: 2014-09-10
WUHAN UNIV OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Transition metal oxides, sulfides, and fluorides have been widely concerned and studied by scientists due to their ultra-high theoretical specific capacity (some up to 1000mAh / g). Nickel sulfide is a typical transition metal sulfide material. It is a promising electrode material for lithium-ion batteries, but its development is limited by its low electrical conductivity and excessive changes in electrode structure during charge-discharge cycles.

Method used

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  • Preparation method for electrode with three-dimensional structure formed by coating nickel sulfide by fold graphene through self-repairing
  • Preparation method for electrode with three-dimensional structure formed by coating nickel sulfide by fold graphene through self-repairing
  • Preparation method for electrode with three-dimensional structure formed by coating nickel sulfide by fold graphene through self-repairing

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Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: as Figure 6 shown

[0032] One, the preparation of graphene dispersion liquid:

[0033] a) Add 1g of graphite powder and 23ml of concentrated sulfuric acid in a 250ml Erlenmeyer flask, mix and stir at room temperature for 24 hours;

[0034] b) Put the Erlenmeyer flask into a constant temperature water bath, the reaction temperature is 40 degrees Celsius, and add 100mgNaNO to the dispersion obtained in step a) 3 , stirred for 5 minutes, then slowly added 1500mgKMnO 4 , and keep the solution temperature below 45 degrees Celsius, and stir for 30 minutes;

[0035] c) Add 3ml of deionized water to the dispersion obtained in step b), stir for 5 minutes, then add 3ml of deionized water, then stir for 5 minutes, then add 40ml of deionized water, and stir for 15 minutes;

[0036] d) Remove the Erlenmeyer flask from the water bath, add 140ml of deionized water and 10ml of 30% H 2 o 2 to stop the oxidation reaction;

[0037] e) The suspension obtained in step...

Embodiment 2

[0052] One, the preparation of graphene dispersion liquid: same as embodiment 1;

[0053] 2. Preparation of three-dimensional wrinkled graphene self-healing coated nickel sulfide structure electrode

[0054] 1) Prepare 50mL of NaOH solution with a mass fraction of 10%, add 0.25g S, 0.65g NaOH to it 2 S·9H 2 0, stirring in a water bath until an orange-yellow transparent solution is formed, and the temperature of the water bath is between 60 degrees Celsius;

[0055] 2) Add 10 mL of graphene oxide solution (concentration is about 4.7 mg / mL) to the solution obtained in step 1), and stir with magnetic force for 1 hour;

[0056] 3) Add about 72 mL of dilute hydrochloric acid with a mass fraction of 5% to the solution obtained in step 2), adjust the pH of the solution to 2, a white precipitate precipitates out, and stir magnetically for 1 hour;

[0057] 4) Suction filtration of the suspension obtained in step 3) to obtain graphene-coated sulfur particles, and drying in air at 70 ...

Embodiment 3

[0062] One, the preparation of graphene dispersion liquid: same as embodiment 1;

[0063] 2. Preparation of three-dimensional wrinkled graphene self-healing coated nickel sulfide structure electrode

[0064] 1) Prepare 50mL of NaOH solution with a mass fraction of 10%, add 0.25g S, 0.65g NaOH to it 2 S·9H 2 0, stirring in a water bath until an orange-yellow transparent solution is formed, and the temperature of the water bath is between 60 degrees Celsius;

[0065] 2) Add 5 mL of graphene oxide solution (concentration is about 4.7 mg / mL) to the solution obtained in step 1), and stir magnetically for 1 hour;

[0066] 3) Add about 72 mL of dilute hydrochloric acid with a mass fraction of 5% to the solution obtained in step 2), adjust the pH of the solution to 2, a white precipitate precipitates out, and stir magnetically for 1 hour;

[0067] 4) Suction filtration of the suspension obtained in step 3) to obtain graphene-coated sulfur particles, and drying in air at 70 degrees ...

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Abstract

The invention relates to a preparation method for an electrode with a three-dimensional structure formed by coating nickel sulfide by fold graphene through self-repairing. The preparation method comprises the following steps: (1) preparing NaOH solution, adding S and Na2S.9H2O into the NaOH solution, and stirring the mixture in a water bath; (2) adding a graphene dispersion liquid, and stirring by using magnetic force; (3) adding dilute hydrochloric acid, adjusting the pH of the solution, and stirring the solution by using the magnetic force; (4) performing suction and filtration to obtain graphene-coating sulfur particles, and drying the sulfur particles in air; (5) soaking the sulfur particles by using commercial nickel foam, and preserving for later use; (6) placing the soaked sulfur particles in a reaction kettle lining, adding de-ionized water into the sulfur particles, encapsulating and performing hydrothermal reaction on the mixture, and cooling a reaction product to room temperature; and (7) washing the reaction product by using alcohol and water once respectively, soaking the reaction product in hydrazine hydrate aqueous solution, and finally drying the soaked reaction product in the air. The preparation method has the beneficial effects that the electrode is prepared on the basis of a shrinkage strain drive mechanism; high-current fast charge and discharge can be realized; in addition, the cycling times can reach 1,000, and the capacity does not decay basically.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials and electrochemistry, and in particular relates to a preparation method of a three-dimensional wrinkled graphene self-repairing coated nickel sulfide structure electrode, and the material can be used as a negative electrode material of a lithium ion battery. Background technique [0002] With the increasing energy demand, energy storage devices play an increasingly important role in improving energy utilization efficiency. Recently, as an important component of energy storage devices, lithium-ion batteries are widely used in hybrid vehicles and portable devices due to their high energy density. Research on lithium-ion battery electrode materials with longer cycle life, higher reversible capacity, and lower production cost is one of the frontiers and hotspots of current research. Transition metal oxides, sulfides, and fluorides have been widely concerned and studied by scientists due t...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/62H01M4/1397
CPCY02E60/122H01M4/1397H01M4/5815H01M4/625H01M4/628H01M10/0525Y02E60/10
Inventor 麦立强刘学赵云龙黄磊石长玮
Owner WUHAN UNIV OF TECH
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