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Preparation and stripping methods of mesoporous cobaltosic oxide nanosheet

A nano and mesoporous technology of cobalt tetroxide, applied in the directions of cobalt oxide/cobalt hydroxide, nanotechnology, nanotechnology, etc., can solve the problems of less active sites, increase the interlayer spacing, agglomeration, etc., and achieve large lamellar structure and interlayer spacing. Enlarged, homogeneous effect

Active Publication Date: 2015-12-30
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cobalt tetroxide with a layered structure has been discovered and studied in recent years due to its excellent performance as a supercapacitor electrode. During the research process, people found a problem: the layered material is too small, and it is prone to agglomeration, which leads to hydrogen The conduction between oxygen radicals and electrons between layers is difficult, the contact area between the electrolyte and the material is small, and the exposed active sites are less. In this case, the material cannot fully function, so the interlayer distance is increased to increase the charge transfer rate of the material. It is a key problem that needs to be solved. As the ion exchange reaction proceeds, the interlayer spacing changes with the size of ions or molecules in the layer. When the interlayer spacing increases to a certain extent, the interaction force between the layers gradually weakens until it disappears completely. , the layered compound dissociates and exists in the form of two-dimensional ultrathin sheets
Although this method has obtained cobalt tetraoxide nanosheets, the products are stacked on each other and have a small specific surface area, which hinders the ion exchange of the electrolyte.

Method used

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  • Preparation and stripping methods of mesoporous cobaltosic oxide nanosheet
  • Preparation and stripping methods of mesoporous cobaltosic oxide nanosheet
  • Preparation and stripping methods of mesoporous cobaltosic oxide nanosheet

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1) Preparation of layered precursor

[0029] Prepare 70mL cobalt ion concentration of 0.1mol / L cobalt nitrate hexahydrate, triton mixed solution, its molar ratio is 2:1, after stirring evenly, add urea again, make its molar ratio with cobalt nitrate hexahydrate be 2 : 1, then continue to stir; transfer the resulting mixed solution into a 100mL polytetrafluoroethylene liner, put the liner in a reactor, and place it in a 120°C oven for constant temperature reaction for 24h. After the reaction, cool, centrifuge, wash, and dry , after drying completely, the pink layered precursor nanosheets were obtained.

[0030] 2) Preparation of Mesoporous Layered Cobalt Tetroxide Nanosheets

[0031] Put the layered precursor obtained in step 1) into a crucible, put it into a muffle furnace, burn it at 300° C. for 3 hours, and cool it to room temperature to obtain mesoporous black cobalt tetraoxide nanosheets.

[0032] 3) Exfoliation of Mesoporous Co3O3 Nanosheets

[0033] The layered...

Embodiment 2

[0035] 1) Preparation of layered precursor

[0036] Prepare 70mL cobalt ion concentration of 0.2mol / L cobalt nitrate hexahydrate, triton mixed solution, its molar ratio is 2:1; after stirring evenly, add urea again, make it and cobalt nitrate hexahydrate molar ratio be 2 : 1, then continue to stir; The resulting mixed solution is transferred to a 100mL polytetrafluoroethylene liner, the liner is placed in a reaction kettle, and placed in a 120°C oven for constant temperature reaction for 24h. After the reaction is over, it is cooled, centrifuged, washed, After drying, after the drying is complete, a pink layered precursor nanosheet is obtained.

[0037] 2) Preparation of Mesoporous Layered Cobalt Tetroxide Nanosheets

[0038] Put the layered precursor obtained in step 1) into a crucible, put it into a muffle furnace, burn it at 300° C. for 3 hours, and cool it to room temperature to obtain mesoporous black cobalt tetraoxide nanosheets.

[0039] 3) Exfoliation of Mesoporous C...

Embodiment 3

[0042] 1) Preparation of layered precursor

[0043] Prepare 70mL cobalt ion concentration of 0.1mol / L cobalt nitrate hexahydrate, triton mixed solution, its molar ratio is 2:1; after stirring evenly, add urea again, make it and cobalt nitrate hexahydrate molar ratio be 2 : 1, then continue to stir; The resulting mixed solution is transferred to a 100mL polytetrafluoroethylene liner, the liner is placed in a reaction kettle, and placed in a 120°C oven for constant temperature reaction for 24h. After the reaction is over, it is cooled, centrifuged, washed, After drying, after the drying is complete, a pink layered precursor nanosheet is obtained.

[0044] 2) Preparation of Mesoporous Layered Cobalt Tetroxide Nanosheets

[0045] Put the layered precursor obtained in step 1) into a crucible, put it into a muffle furnace, burn it at 300° C. for 3 hours, and cool it to room temperature to obtain mesoporous black cobalt tetraoxide nanosheets.

[0046] 3) Exfoliation of Mesoporous C...

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Abstract

The invention provides preparation and stripping methods of a mesoporous cobaltosic oxide nanosheet. According to the method, urea is added into a solution with the Co<2+> concentration being 0.01 to 0.5 mol / L; constant-temperature reaction is performed for 24h at 120 DEG C; cooling, centrifugation, washing and drying are performed; after the drying is completed, a pink lamellar precursor nanosheet is obtained; the lamellar precursor nanosheet is calcined at the temperature being 200 to 400 DEG C to obtain a mesoporous black cobaltosic oxide nanosheet. The mesoporous black cobaltosic oxide nanosheet is dissolved in an ammonium nitrate solution for pretreatment; after centrifugation, supernatant liquid is dissolved in formamide; mixed liquid is subjected to water bath ultraphonic treatment for 1 to 2h at 100 to 200W at the room temperature; constant-temperature oscillation is performed for 3d in a constant-temperature oscillator at a rotating speed being 100 to 300r / min; supernatant obtained after centrifugation is a striped single lamellar cobaltosic oxide nanosheet. Obtained cobaltosic oxide inherits excellent properties of matrixes; the crystallinity is high; a larger lamellar structure is used; meanwhile, the surface also has the obvious mesoporous features.

Description

technical field [0001] The invention relates to a preparation method of nano inorganic functional materials, in particular to a preparation and stripping method of cobalt trioxide mesoporous nanosheets used for supercapacitors. Background technique [0002] Cobalt tetroxide has the advantages of highly reversible redox reaction, large specific surface area, high electrical conductivity, good long-term performance, and corrosion resistance. Therefore, it is considered as an alternative electrode material for supercapacitors. Cobalt tetroxide with a layered structure has been discovered and studied in recent years due to its excellent performance as a supercapacitor electrode. During the research process, people found a problem: the layered material is too small, and it is prone to agglomeration, which leads to hydrogen The conduction between oxygen radicals and electrons between layers is difficult, the contact area between the electrolyte and the material is small, and the e...

Claims

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Application Information

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IPC IPC(8): C01G51/04B82Y40/00B82Y30/00
Inventor 李占双朱会敏刘琦王君刘婧媛张宏森李茹民刘连河
Owner HARBIN ENG UNIV
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