Nitrogen and sulfur co-doped graphene-loaded cobalt selenide-coated positive electrode material and preparation method thereof

A nitrogen-sulfur co-doping, cathode material technology, applied in battery electrodes, electrochemical generators, electrical components, etc., can solve the problem that lithium-ion batteries cannot have good rate performance and structural stability at the same time, and achieve good coating Protection effect, improve stability, improve transmission rate effect

Inactive Publication Date: 2019-05-17
GEM WUXI ENERGY MATERIAL CO LTD
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Problems solved by technology

[0003] In view of the above problems, the object of the present invention is to provide a nitrogen-sulfur co-doped graphene-supported cobalt selenide-coated positive electrode material and a preparation me...
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Abstract

The invention is applicable to the technical field of a lithium battery technology, and provides a nitrogen and sulfur co-doped graphene-loaded cobalt selenide-coated positive electrode material and apreparation method thereof. During the preparation process, cobalt nelenide is loaded onto a graphene material, the mutual effect between the graphene material and Li can be improved due to presenceof a group containing elements N and S, a good coating protection effect is achieved, the mutual effect between the positive electrode material and an electrolyte is prevented, the volume effect generated by the material during the charge-discharge process can be effectively reduced by a hole structure of the graphene body, and the stability of the material structure is improved; and meanwhile, graphene has favorable conductivity, the cobalt selenide is a negative electrode material and is a lithium ion conductor, the lithium ion transmission rate can be improved by synergic effect of the graphene and the cobalt selenide, and finally, the lithium ion battery has excellent rate performance and cycle property and also has favorable safety.

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  • Nitrogen and sulfur co-doped graphene-loaded cobalt selenide-coated positive electrode material and preparation method thereof
  • Nitrogen and sulfur co-doped graphene-loaded cobalt selenide-coated positive electrode material and preparation method thereof

Examples

  • Experimental program(2)
  • Comparison scheme(1)

Example Embodiment

[0022] In this embodiment, the preparation method of the nitrogen-sulfur co-doped graphene-supported cobalt selenide-coated cathode material includes:
[0023] Step S1, adding graphite oxide to an aqueous solution of a compound containing nitrogen and sulfur, and ultrasonically dispersing to obtain a uniformly mixed aqueous solution.
[0024] In this step, the ultrasonic dispersion time is 20-60 min, the concentration of graphite oxide in the uniformly mixed aqueous solution is 5g/L, the concentration of the nitrogen- and sulfur-containing compound is 0.025mol/L, and the nitrogen- and sulfur-containing The element compound is one or more of L-cysteine, thiourea, mercaptoethylamine, glutathione or methionine.
[0025] Step S2: The aqueous solution is reacted at a certain temperature to obtain nitrogen-sulfur co-doped graphene hydrogel, and then freeze-dried to obtain nitrogen-sulfur co-doped graphene.
[0026] In this step, the reaction temperature is 60-90°C, and the reaction time is 30-90 min.
[0027] Step S3: Disperse the obtained nitrogen and sulfur co-doped graphene in a diethylene triamine solution containing a compound of cobalt and a compound of selenium to obtain an aqueous solution of doped graphene, which is then ultrasonically dispersed, and then transferred to a high pressure reaction Reaction in the kettle, after cooling, suction filtration and washing with water to remove impurities, followed by freeze drying, to obtain nitrogen-sulfur co-doped graphene supporting cobalt selenide material.
[0028] In this step, the cobalt compound is Co(OAc) 2 ·H 2 O. The compound of selenium is Na 2 SeO 3 , The Co(OAc) 2 ·H 2 O and Na 2 SeO 3 The concentration in the diethylene triamine solution is 50 mmol/L, the concentration of nitrogen and sulfur co-doped graphene in the doped graphene aqueous solution is 5 g/L, the ultrasonic dispersion time is 20-60 min, and the reaction The temperature is 120-160°C, the reaction time is 12-20h, and the number of washing times is three times.
[0029] Step S4, mixing the obtained nitrogen-sulfur co-doped graphene-supported cobalt selenide material with the nickel-cobalt-manganese ternary material in a certain proportion, and the mixture is uniformly calcined under a protective gas atmosphere, and finally cooled to obtain nitrogen-sulfur co-doped graphite The ene-supported cobalt selenide coated cathode material.
[0030] In this step, the addition amount of the nitrogen-sulfur co-doped graphene-supported cobalt selenide material is 0.05-0.5% of the mass of the nickel-cobalt-manganese ternary material, the calcination temperature is 300-600°C, and the calcination time is 2-6 hours.
[0031] The following is described through specific implementation.

Example Embodiment

[0032] Example one:
[0033] 1) Add graphite oxide to the L-cysteine ​​aqueous solution containing 0.025mol/L, the graphite oxide concentration is 5g/L, and ultrasonically disperse for 30 minutes to obtain a uniformly mixed aqueous solution, and react at 80°C for 1 hour to obtain nitrogen and sulfur. Doped graphene hydrogel, freeze-dried to obtain nitrogen and sulfur co-doped graphene;
[0034] 2) Disperse the nitrogen and sulfur co-doped graphene in step 1 in Co(OAc) containing 50mmol/L 2 ·H 2 O and 50mmol/L Na 2 SeO 3 In the diethylene triamine solution, the doped graphene concentration is 5g/L. After ultrasonic for 30min, it is transferred to the autoclave and reacted at 140℃ for 18h. After cooling, it is suction filtered and washed with water three times to remove impurities, and freeze-dried Then obtain the nitrogen-sulfur co-doped graphene loaded cobalt selenide material;
[0035] 3) Mix the nitrogen-sulfur co-doped graphene-supported cobalt selenide material in step 2 with the high-nickel nickel-cobalt-manganese ternary material. The supported graphene content is 0.1%, and the mixture is evenly mixed in an argon atmosphere muffle It is calcined in a furnace at 400°C for 4 hours, and after cooling, a cathode material coated with a cobalt selenide material coated with nitrogen and sulfur co-doped graphene is obtained.
[0036] 4) The cathode material obtained in step 3 is formed into a button battery by slurrying, coating, and drying, and the battery charge and discharge test is performed.
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