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Hard carbon material and preparation method and application thereof

A hard carbon and pre-oxidation technology, which is applied in the preparation/purification of carbon, electrical components, electrochemical generators, etc., can solve the problems of poor cycle stability, low first-cycle coulombic efficiency, and low reversible specific capacity, and achieve mild conditions Controllable, conducive to diffusion and transport, and increase the effect of specific surface area

Active Publication Date: 2021-01-15
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] ...The present invention provides a hard carbon material obtained by pre-oxidizing and carbonizing phenolic resin as a raw material, which overcomes the defects of low first cycle coulombic efficiency, low reversible specific capacity and poor cycle stability of current sodium battery negative electrode materials

Method used

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  • Hard carbon material and preparation method and application thereof
  • Hard carbon material and preparation method and application thereof
  • Hard carbon material and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] (1) phenolic resin pretreatment: get 10g phenolic resin (specific surface area 2m 2 / g) was completely dissolved in absolute ethanol, added conductive carbon black with 5wt% of phenolic resin and stirred for 2 hours, and then placed in an oven at 70° C. for 12 hours to obtain the treated phenolic resin.

[0048] (2) Pre-oxidation treatment: 5g of the treated phenolic resin was first heated to 200°C for 1 hour at a heating rate of 12°C / min in an air atmosphere, and then heated to 300°C for 1 hour at a heating rate of 8°C / min. Finally, the temperature was raised to 400° C. at a heating rate of 5° C. / min, and calcined for 0.5 h.

[0049] (3) Cooling: the pre-oxidized particles were rapidly cooled to 150°C at 20°C / min, kept for 20 seconds, and then naturally cooled to 30°C.

[0050] (4) Carbonization: After taking it out, the particles are ball-milled into powder, and the obtained powder is put into a tube furnace, and carbonized at 1250°C for 6 hours in a 20% Ar / N2 atmosp...

Embodiment 2

[0053] (1) phenolic resin pretreatment: get 10g phenolic resin (specific surface area 2m 2 / g) was completely dissolved in absolute ethanol, added conductive carbon black with 5wt% of phenolic resin and stirred for 2 hours, and then placed in an oven at 70° C. for 12 hours to obtain the treated phenolic resin.

[0054] (2) Pre-oxidation treatment: 5g of the treated phenolic resin was first heated to 250°C for 2 hours at a heating rate of 15°C / min in an air atmosphere, and then heated to 350°C for 2 hours at a heating rate of 10°C / min. Finally, the temperature was raised to 450° C. at a heating rate of 7° C. / min, and calcined for 1 hour.

[0055] (3) Cooling: the pre-oxidized particles were rapidly cooled to 150°C at 20°C / min, kept for 20 seconds, and then naturally cooled to 30°C.

[0056] (4) Carbonization: after taking out, ball mill the particles into powder, put the obtained powder into a tube furnace, carbonize at 1200°C for 6 hours in a 20% Ar / N2 atmosphere at a heating...

Embodiment 3

[0059] (1) phenolic resin pretreatment: get 10g phenolic resin (specific surface area 2m 2 / g) was completely dissolved in absolute ethanol, added conductive carbon black with 5wt% of phenolic resin and stirred for 2 hours, and then placed in an oven at 70° C. for 12 hours to obtain the treated phenolic resin.

[0060] (2) Pre-oxidation treatment: 5g of the treated phenolic resin was first heated to 200°C for 1 hour at a heating rate of 11°C / min in an air atmosphere, and then heated to 300°C at a heating rate of 9°C / min for 2 hours. Finally, the temperature was raised to 400° C. at a heating rate of 5° C. / min, and calcined for 1 h.

[0061] (3) Cooling: the pre-oxidized particles were rapidly cooled to 150°C at 20°C / min, kept for 20 seconds, and then naturally cooled to 30°C.

[0062] (4) Carbonization: After taking it out, the particles are ball-milled into powder, and the obtained powder is put into a tube furnace, and carbonized at 1300°C for 6 hours in a 20% Ar / N2 atmosph...

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Abstract

The invention relates to a hard carbon material as well as a preparation method and application thereof. A conductive additive is introduced into the hard carbon material precursor to improve the conductivity of an obtained material, and a large number of oxygen-containing functional groups are introduced in combination with variable-speed heating pre-oxidation, so that the crosslinking degree ofa material skeleton is increased, the strength of the material is improved, and the sodium storage specific capacity, the first-circle coulombic efficiency and the rate capability are remarkably improved. The hard carbon material has the advantages of high reversible capacity, high first-circle coulombic efficiency, good cycling stability and the like when being used for the sodium ion battery. The material has the characteristics of simple preparation method and cheap and easily available raw materials, and provides more choices for the negative electrode of the sodium-ion battery.

Description

technical field [0001] The invention relates to the field of batteries, more specifically to a preparation method of a hard carbon material and its application in a negative electrode of a sodium ion battery. Background technique [0002] Due to the shortage of oil resources and the aggravation of environmental pollution, it is increasingly important to vigorously develop clean energy. Lithium-ion batteries have outstanding advantages such as no pollution, long service life, and fast charging and discharging, and have been widely used in portable electronic devices and electric vehicles. However, with the continuous expansion of application fields and the sharp increase in usage, the price of lithium-ion batteries is relatively high due to the limited and uneven distribution of metal lithium resources. Sodium, which belongs to the same main group as lithium and has similar physicochemical properties, is very rich in resources. The price of raw materials is low, and it is di...

Claims

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Application Information

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IPC IPC(8): C01B32/05H01M4/587H01M4/62H01M10/054
CPCC01B32/05H01M4/587H01M4/625H01M10/054Y02E60/10
Inventor 殷雅侠魏峥牛玉斌郭玉国
Owner INST OF CHEM CHINESE ACAD OF SCI
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