Flake MoS2/graphene composite aerogel and preparation method thereof

A graphene airgel and graphene composite technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low electronic conductivity and poor cycle stability

Inactive Publication Date: 2015-05-06
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Molybdenum disulfide is used as the negative electrode material of the battery. Although it has a high capacity, due to the obvious deformation when lithium ions are intercalated and extracted, the capacity decays quickly after multiple charges and discharges, and the cycle stability is not good. At the same time, due to the two Molybdenum sulfide is a semiconductor material, and its electronic conductivity is relatively low. Therefore, it is necessary to select a material that can not only enhance the structural stability of molybdenum disulfide to alleviate the deformation during lithiation and delithiation, but also have higher electrical conductivity for compounding.

Method used

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  • Flake MoS2/graphene composite aerogel and preparation method thereof
  • Flake MoS2/graphene composite aerogel and preparation method thereof
  • Flake MoS2/graphene composite aerogel and preparation method thereof

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Embodiment 1

[0029] Used graphene oxide is to adopt traditional process method to make, and its preparation method is as follows:

[0030] Potassium persulfate (K 2 S 2 o 8 ) 2.5g, phosphorus pentoxide (P 2 o 5 ) 2.5g, dissolved in 12mL of concentrated sulfuric acid, heated to 80°C; then 3g of natural graphite was added to the above solution, kept at 80°C for 4.5 hours; cooled to room temperature, diluted with 500mL of deionized water, and left standing overnight; filtered, Use a 0.2mm filter to float the residual acid; dry it in a vacuum oven at 60°C; add the obtained preoxide to 120mL of ice-bathed concentrated sulfuric acid, and slowly add 15g of KMnO under stirring 4 , Keep the temperature below 20°C during the addition process. Then the temperature was controlled at 35°C and stirred for 2h. Add 250mL deionized water to dilute, and keep the temperature below 50°C in an ice bath during the dilution process. Stir for another 2 h, add 0.7 L of deionized water, and immediately add 2...

Embodiment 2

[0042] The preparation method of graphene oxide is the same as embodiment 1.

[0043] Preparation of flake MoS 2 / Graphene composite airgel material:

[0044] 1) Measure 25mL of graphene oxide solution with a concentration of 3mg / mL and pour it into a 100mL beaker, add 20mL of deionized water and magnetically stir for 30min to mix well;

[0045] 2) Weigh 0.45g ammonium molybdate and dissolve it in 15mL deionized water, stir it magnetically for 20min, and pour it into the graphene oxide solution in step 1);

[0046] 3) Weigh 0.57g of thiourea and dissolve it in 15mL of deionized water. Thiourea is both a sulfur source and a reducing agent. Stir magnetically for 20 minutes, pour into the solution obtained in step 2), and stir magnetically for 1 hour;

[0047] 4) Measure 1 mL of ethylenediamine solution and pour it into the mixed solution in step 3), and stir magnetically for 20 minutes;

[0048] 5) Transfer the mixed solution obtained in step 4) into a polytetrafluoroh...

Embodiment 3

[0052] The preparation method of graphene oxide is the same as embodiment 1.

[0053] Preparation of flake MoS 2 / Graphene composite airgel material:

[0054] 1) Measure 50mL graphene oxide solution with a concentration of 3mg / mL and pour it into a 100mL beaker, add 40mL deionized water and magnetically stir for 30min to mix well;

[0055] 2) Weigh 0.91g sodium molybdate and dissolve it in 15mL deionized water, stir it magnetically for 20min, and pour it into the graphene oxide solution in step 1);

[0056] 3) Weigh 1.14g of thiourea and dissolve it in 15mL of deionized water. Thiourea is both a sulfur source and a reducing agent. Stir magnetically for 20 minutes, pour into the solution obtained in step 2), and stir magnetically for 1 hour;

[0057] 4) Measure 3 mL of triethylamine solution and pour it into the mixed solution in step 3), and stir magnetically for 20 minutes;

[0058] 5) Transfer the mixed solution obtained in step 4) into a polytetrafluorohydrotherma...

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Abstract

The invention relates to a flake MoS2/graphene composite aerogel and a preparation method thereof and belongs to the technical field of anode materials of lithium ion batteries. The preparation method comprises the following steps: ultrasonically dispersing a certain quantity of graphene oxide solution into deionized water, adding a certain quantity of water-soluble molybdate and thiourea, then adding 0.1-3mL organic amine solution, taking out a cylindrical product after hydrothermal reaction at the temperature of 160-240 DEG C, freeze-drying, and then carrying out thermal treatment for 2h in the mixed atmosphere of argon and hydrogen at the temperature of 800 DEG C to obtain the flake MoS2/graphene composite aerogel. According to the flake MoS2/graphene composite aerogel and the preparation method thereof disclosed by the invention, thin layers of graphene are connected with one another in a staggering mode to form a three-dimensional ordered conductive network and form micron pore canals, MoS2 is uniformly dispersed on the ultra-large superficial area, and thus, the problems of volume expansion and crushing materials are effectively solved; meanwhile, the structure stability and the cycle performance of the flake MoS2/graphene composite aerogel, serving as the anode material, are improved.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion battery negative electrode material, in particular to a flake MoS 2 The invention discloses a graphene composite airgel and a preparation method thereof, belonging to the technical fields of inorganic composite nanometer materials and lithium ion battery electrode materials. Background technique [0002] A chemical power source is a device that realizes mutual conversion between electrical energy and chemical energy, and is an important medium for more rational use of energy. The new generation of lithium-ion batteries have excellent properties such as high working voltage, small size, high specific capacity, light weight, and no memory effect. Commercial lithium-ion batteries mostly use carbon materials as negative electrodes. Graphite has good cycle stability due to its structural characteristics, but its shortcomings cannot be ignored. First, the limitation of theoretical capacity canno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/62H01M4/1393H01M4/1397H01M4/133H01M4/136
CPCY02E60/10
Inventor 蒋永赵兵陆孟娜阮仲英陈卢焦正吴明红
Owner SHANGHAI UNIV
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