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Nickel-cobalt selenide with organic metal frame structure, preparation method and application thereof

A framework structure, organometallic technology, applied in selenium/tellurium compounds, chemical instruments and methods, elemental compounds other than selenium/tellurium, etc., can solve problems such as low electrical conductivity, and achieve improved electrical conductivity and high porosity , the effect of structural optimization

Pending Publication Date: 2021-11-19
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Description
  • Claims
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Problems solved by technology

Among them, the negative electrode materials that make up the battery are the research hotspots in recent years. However, the negative electrode materials have a series of problems such as large volume change and low conductivity during charging and discharging.

Method used

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  • Nickel-cobalt selenide with organic metal frame structure, preparation method and application thereof
  • Nickel-cobalt selenide with organic metal frame structure, preparation method and application thereof
  • Nickel-cobalt selenide with organic metal frame structure, preparation method and application thereof

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preparation example Construction

[0027] A preparation method of an organometallic framework structure nickel cobalt selenide, comprising the steps of:

[0028] 1) Preparation of nickel-cobalt-selenide precursor: Dissolve nickel source, cobalt source and carbon source in dimethyl phthalate, deionized water, N,N-dimethylformamide methanol and ethylene glycol in a certain proportion In the mixed solution of alcohol, stir well.

[0029] Wherein, the nickel source is at least one of nickel acetate, nickel nitrate and nickel sulfate, and the total amount is between 0.015-0.025 mol. The cobalt source is at least one of cobalt acetate, cobalt nitrate and cobalt sulfate, and the total amount is between 0.015-0.025mol. The carbon source is at least one of 1,3,5-tribenzenetricarboxylic acid, polyvinylpyrrolidone (PVP), sucrose, and ascorbic acid, and the amount of the added carbon source is 7-14wt% of the total mass of the cobalt source and the nickel source.

[0030] In the mixed solution, the volume ratio of dimethy...

Embodiment 1

[0035] Weigh 2.63g of nickel sulfate, 1.244g of nickel acetate, 1.454g of nickel nitrate, 2.81g of cobalt sulfate, and 0.53g of PVP with a balance. Move it into a beaker with a volume of 200mL, then add 30mL of deionized water, 20mL of DMP, 20mL of ethylene glycol, 10mL of N,N-dimethylformamide methanol, at a speed of 120r / min, Stir magnetically for 30 min. Then the mixture was transferred to a 100 mL reactor lining and reacted at 180 °C for 10 h. After the reaction, the reactor was left to stand, and the supernatant liquid was removed. The centrifuge was used to wash three times with deionized water and twice with ethanol at a speed of 8000 r / min, and then dried in a vacuum oven at 80°C for 12 hours.

[0036] The above-mentioned product 300mg is placed on one side of the corundum ark, and the selenium powder of 800mg is placed on the other side of the small ark. In an argon flow with a flow rate of 50mL / min, at 850°C, the heating rate was set to 4°C / min, and after calcinati...

Embodiment 2

[0040] Weigh 1.244g of nickel acetate, 2.81g of cobalt sulfate, 1.455g of cobalt nitrate, 2.49g of cobalt acetate, and 0.96g of sucrose with a balance. Move it into a beaker with a volume of 200mL, then add 40mL of deionized water, 10mL of DMP, 10mL of ethylene glycol, and 20mL of N,N-dimethylformamide methanol, at a speed of 150r / min, Stir magnetically for 20 min. Then the mixture was transferred to a 100 mL reactor lining and reacted at 150 °C for 18 h. After the reaction, the reactor was left to stand, and the supernatant liquid was removed. The centrifuge was used to wash three times with deionized water and twice with ethanol at a speed of 8000 r / min, and then dried in a vacuum oven at 80°C for 12 hours.

[0041] Place 400 mg of the above product on one side of the corundum ark, and place 1000 mg of selenium powder on the other side of the small ark. In an argon flow at a flow rate of 25mL / min, at 750°C, the heating rate was set to 4°C / min, and after calcination at high...

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Abstract

The invention relates to the technical field of preparation of new energy electrode materials, in particular to nickel-cobalt selenide with an organic metal frame structure, a preparation method and application thereof. The preparation method comprises the following steps: 1) dissolving a nickel source, a cobalt source and a carbon source in a mixed solution, uniformly stirring, transferring the mixture into a reaction container, reacting for 6-18 hours at 150-200 DEG C, and after the reaction is finished, centrifuging, washing and drying a product to obtain a nickel cobalt selenide precursor NiCo-MOF with an organic metal frame structure; and 2) placing the nickel cobalt selenide precursor NiCo-MOF and selenium powder in a corundum ark, and carrying out high-temperature calcination in argon flow for a period of time to obtain a target product. According to the invention, the obtained product has a large specific surface area, the reaction interface is increased, and the volume change of the active material in the charging and discharging process can be effectively buffered through proper carbon coating; and compared with the prior art, the material has the characteristics of high conductivity, long cycle life, environmental protection, simple preparation and excellent performance.

Description

technical field [0001] The invention relates to the technical field of preparation of new energy electrode materials, in particular to an organometallic framework structure nickel-cobalt selenide and its preparation method and application. Background technique [0002] Lithium-ion batteries have attracted widespread attention due to their high energy density, good safety, stability, and cycle life. Among them, the negative electrode materials that make up the battery are the research hotspots in recent years. However, the negative electrode materials have a series of problems such as large volume changes and low electrical conductivity during charging and discharging. Therefore, in order to develop suitable anode materials suitable for lithium-ion batteries, it is necessary to optimize the anode materials. Binary transition metal selenides have higher electrical conductivity and more active sites for electrochemical reactions than single metal selenides, so they are often s...

Claims

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Application Information

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IPC IPC(8): C01B19/00C01B32/05H01M4/58H01M4/62H01M10/0525
CPCC01B19/002C01B32/05H01M4/581H01M4/625H01M10/0525C01P2004/03C01P2002/72C01P2006/40C01P2004/80Y02E60/10
Inventor 李俊哲孙文超汪超李林玮孔祥升
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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