Preparation method of lithium battery negative pole material

A negative electrode material, lithium battery technology, applied in the direction of battery electrodes, secondary batteries, nanotechnology for materials and surface science, etc., can solve the problems of unfavorable product consistency control, low cycle rate, and many processes, etc. To achieve the effect of facilitating industrial production promotion, simple process operation and simple operation

Active Publication Date: 2017-02-15
ZHEJIANG JILI POWER NEW ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Invention patent CN 102522534A discloses a high specific capacity silicon-carbon composite material and its preparation method, lithium-ion battery negative electrode material and lithium-ion battery. It uses porous carbon-based materials as the substrate, and nano-silicon particles are embedded in its pores to obtain silicon Carbon composite materials have high specific capacity, but they also have problems such as low cycle performance and low first effect
However, there are many processes and many control points, which is not conducive to the control of product consistency in the process of industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Preparation of graphene

[0029] Add 40mL H to a 500mL beaker 2 SO 4 and 6g (NH 4 ) 2 S 2 o 8 , stirred mechanically until (NH 4 ) 2 S 2 o 8 dissolved, to be (NH 4 ) 2 S 2 o 8 After dissolving, add 1.5g of graphite powder (32 mesh), stir mechanically for 30min, slowly add 5mL of H 2 o 2 , after standing for 8 hours at room temperature, the expanded graphene aggregates (expanded graphite) were obtained, washed with water until neutral, freeze-dried in a freeze dryer for 12 hours to obtain a powder; the powder was added to 150mL N-methylpyrrolidone (NMP) In the solution, under the condition of ultrasonic power of 500w, ultrasonically stir for 1 hour to obtain a graphene suspension, freeze-dry in a freeze dryer for 48 hours to obtain a graphene powder;

[0030] (2) Preparation of graphene / silicon / c-PAN / artificial graphite hybrid anode materials

[0031] Graphene in step (1) and nano-silicon (Si) powder, polyacrylonitrile (PAN), artificial graphite are a...

Embodiment 2

[0033] (1) Preparation of graphene

[0034] With embodiment 1;

[0035] (2) Preparation of graphene / silicon / c-PAN / artificial graphite hybrid anode materials

[0036] Graphene in step (1) and nano-silicon (Si) powder, polyacrylonitrile (PAN), artificial graphite are added to the container containing dimethylformamide (DMF) according to mass ratio 10:5:5:80 middle; put it under the ultrasonic crusher, ultrasonic power is 500w, and ultrasonically stir for 2h; wash with water, freeze-dry in a freeze dryer for 12h to obtain a graphene / silicon / PAN / artificial graphite mixture; place the mixture at a temperature of 350°C , N 2 In a sintering furnace protected by an atmosphere, calcined for 2 hours to obtain a graphene / silicon / c-PAN / artificial graphite composite; put the composite into a jet mill for fine crushing, and the jet mill feed pressure is 0.1Mpa, The working pressure is 0.8Mpa, and the working medium is compressed air. After crushing, a graphene / silicon / c-PAN / artificial gr...

Embodiment 3

[0038] (1) Preparation of graphene

[0039] With embodiment 1;

[0040] (2) Preparation of graphene / silicon / c-PAN / artificial graphite hybrid anode materials

[0041] Graphene in step (1) and nano-silicon (Si) powder, polyacrylonitrile (PAN), artificial graphite are added to the container containing dimethylformamide (DMF) according to mass ratio 10:5:5:80 middle; put it under the ultrasonic crusher, under the condition of ultrasonic power of 500w, ultrasonically stir for 2h; wash with water, and freeze-dry in the freeze dryer for 12h to obtain the graphene / silicon / PAN / artificial graphite mixture; place the mixture at a temperature of 400°C , N 2 In a sintering furnace protected by an atmosphere, calcined for 4 hours to obtain a graphene / silicon / c-PAN / artificial graphite composite; put the composite into a jet mill for fine crushing, and the jet mill feed pressure is 0.1Mpa, The working pressure is 0.8Mpa, and the working medium is compressed air. After crushing, a graphene / ...

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Abstract

The invention discloses a preparation method of a lithium battery negative pole material. The preparation method comprises the following steps: 1) preparing graphene nanoplatelets: stirring and mixing H2SO4 and (NH4)2S2O8, adding graphite powder after (NH4)2S2O8 is dissolved, further stirring, dropwisely adding H2O2, standing to obtain expanded graphene aggregate, washing with water to neutral, and drying; and adding the dried graphene aggregate into an N-methylpyrrolidone solution, pulverizing to obtain a graphene solution, centrifuging, washing with water, and freeze-drying to obtain graphene nanoplatelet powder; and 2) adding the graphene nanoplatelet powder prepared in the step 1) together with nano silicon powder, polyacrylonitrile and artificial graphite into a container containing dimethylformamide, performing ultrasonic dispersion, freeze-drying to obtain a graphene/nano silicon powder/polyacrylonitrile/artificial graphite mixture, calcining the mixture to obtain a graphene/nano silicon powder/cyclized polyacrylonitrile/artificial graphite compound, and crushing the compound to obtain the graphene/nano silicon powder/cyclized polyacrylonitrile/artificial graphite mixed negative pole material.

Description

technical field [0001] The invention belongs to the technical field of lithium battery materials and their manufacture, and in particular relates to a high specific capacity graphene / silicon / c-PAN / artificial graphite hybrid lithium battery negative electrode material manufacturing method. Background technique [0002] Silicon material has a high theoretical specific capacity (4200mAh / g), low potential for lithium intercalation and extraction, and is abundant in nature. It has become a research hotspot for the next generation of negative electrode materials. However, the silicon material expands in volume by more than 300% during the process of deintercalating lithium, causing electrode pulverization and collapse, resulting in a decrease in battery capacity. The preparation of modified silicon anode with good cycle performance and high specific capacity provides the possibility for industrial application. [0003] At present, the modification work of silicon materials mainly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/583H01M4/62H01M10/0525H01M4/36H01M4/38H01M4/60C01B32/182B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/364H01M4/386H01M4/583H01M4/602H01M4/625H01M10/0525Y02E60/10
Inventor 汪训国王斌
Owner ZHEJIANG JILI POWER NEW ENERGY
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