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Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery

A molybdenum dioxide and octahedral technology, which is applied in the field of new energy materials, can solve the problems of difficult control of synthesis conditions, difficult control of morphology and structure, and difficulty in mass production, so as to reduce structural changes and performance deterioration, improve cycle stability, Beneficial to industrial production

Inactive Publication Date: 2016-09-28
CENT SOUTH UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

Shi et al. (Nano Letters, 2009, 9, 4215.) reported using silicon dioxide as a template to prepare nanometer mesoporous molybdenum dioxide by gas phase technology under 10% hydrogen atmosphere conditions. When applied to lithium-ion batteries Exhibited 750nAhg -1 specific capacity, but the preparation method is expensive, the synthesis conditions are harsh, and hydrogen gas with potential safety hazards is required, so it is difficult to achieve mass production; Zhao et al. (J.Mater.Chem., 2012, 22, 13334.) reported a Molybdenum dioxide with a core-shell structure synthesized by a solvothermal method, and applied to the negative electrode of lithium-ion batteries, its first-cycle specific capacity is 749.3mAhg -1 , reduced to 623.8mAhg after 50 laps -1 , although the performance is relatively good, but the core-shell structure is relatively complex, and the morphology structure is not easy to control, which limits its large-scale application; Chinese patent CN 102815749A discloses a method for preparing molybdenum dioxide nanorods by co-precipitation method, which The synthesis conditions of this method are difficult to control, and the uniformity of the material morphology is poor.
[0005] Most of the above-mentioned preparation methods of molybdenum dioxide have the disadvantages of harsh synthesis conditions and difficult control of morphology and material uniformity. When they are used as lithium-ion battery negative electrode materials, some have poor cycle stability and some have unsatisfactory high-current performance. Therefore, there is an urgent need to explore a negative electrode material for lithium-ion batteries with good capacity performance, good cycle and rate performance, and simple preparation methods in this field.

Method used

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  • Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery
  • Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery
  • Preparation method of octahedral porous molybdenum dioxide and application of octahedral porous molybdenum dioxide in lithium-ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] According to the molar ratio of copper source and molybdenum source being 9:1, 1 mmol of copper nitrate and 0.11 mmol of phosphomolybdic acid were weighed respectively, and added to 10 mL of deionized water successively, and 1 mmol of trimesic acid and 1 mmol of tetramethylene tricarboxylic acid were continuously added under magnetic stirring conditions. Methylammonium hydroxide, after fully stirring for 0.5h, transfer the mixed solution into a hydrothermal reaction kettle, conduct a hydrothermal reaction at 180°C for 48h, wash the product with distilled water, dry it in an oven, and place it In a quartz crucible, argon gas was introduced to conduct high-temperature heat treatment at 850°C for 8 hours. The product was washed with ferric chloride solution and dried to obtain an octahedral porous molybdenum dioxide material.

[0037] Using the octahedral porous molybdenum dioxide material prepared in this embodiment, the molybdenum dioxide nanoparticles are constructed to ...

Embodiment 2

[0044] According to the molar ratio of copper source and molybdenum source as 8:1, 1 mmol of copper nitrate and 0.125 mmol of phosphomolybdic acid were weighed respectively, and added to 10 mL of deionized water successively, and 0.5 mmol of trimesic acid and 0.5 mmol tetramethylammonium hydroxide, after fully stirring for 0.5h, transfer the mixed solution into a hydrothermal reaction kettle, carry out a hydrothermal reaction at 180°C for 36h, wash the product with distilled water, place it in an oven and dry it. It is placed in a quartz crucible, fed with argon gas for high-temperature heat treatment at 800°C for 6 hours, washed with ferric chloride solution, and dried to obtain an octahedral porous molybdenum dioxide material.

[0045] Using the octahedral porous molybdenum dioxide material prepared in this example, molybdenum dioxide nanoparticles are constructed to form a uniform octahedral structure rich in pores, and the particle size is 5-7 μm.

[0046] The electrode co...

Embodiment 3

[0048] According to the molar ratio of copper source and molybdenum source being 8:1, 1 mmol of copper nitrate and 0.125 mmol of phosphomolybdic acid were weighed respectively, and successively added to 10 mL of deionized water, and 1 mmol of trimesic acid and 1 mmol of tetramethylene tricarboxylic acid were continuously added under magnetic stirring conditions. Methylammonium hydroxide, after fully stirring for 0.5h, transfer the mixed solution into a hydrothermal reaction kettle, conduct a hydrothermal reaction at 180°C for 48h, wash the product with distilled water, dry it in an oven, and place it In a quartz crucible, argon gas is introduced to conduct high-temperature heat treatment at 800°C for 10 hours. The product is washed with ferric chloride solution and dried to obtain an octahedral porous molybdenum dioxide material.

[0049] Using the octahedral porous molybdenum dioxide material prepared in this embodiment, the molybdenum dioxide nanoparticles are constructed to ...

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Abstract

The invention discloses a preparation method of octahedral porous molybdenum dioxide and an application of the octahedral porous molybdenum dioxide in a lithium-ion battery. The preparation method comprises the steps of: adding trimesic acid and tetramethyl ammonium hydroxide to a solution containing a copper salt and a phosphomolybdic acid and / or phosphomolybdate for stirring to form an emulsion; transferring the emulsion into a hydrothermal reaction kettle for hydrothermal reaction to obtain a precursor compound; and putting the precursor compound into a protective atmosphere, carrying out thermal treatment at a high temperature and then washing the product to obtain a porous octahedral molybdenum dioxide material which is formed by stacking and assembling ultrafine nanoparticles, is uniform in shape and form and good in stability and has a porous characteristic. The molybdenum dioxide material is applied to the lithium-ion battery as a negative electrode material, so that the rate capability and the cycling stability of the electrode material are improved under the premise of ensuring the specific capacity; the preparation technology of the molybdenum dioxide material is simple; the cost is low; and the molybdenum dioxide material has a relatively good research prospect.

Description

technical field [0001] The invention relates to a preparation method of a negative electrode material of a lithium ion battery, in particular to the preparation of an octahedral porous molybdenum dioxide and its application in a lithium ion battery, belonging to the field of new energy materials. Background technique [0002] As an electrochemical energy storage device that occupies a dominant position in society, lithium-ion batteries have achieved rapid development in portable electronic products (notebook computers, smart mobile equipment, tablet computers, etc.) and electric vehicles, and have shown good development prospects . Graphite has been commercially used as the anode of lithium-ion batteries due to its cheapness and good stability, but its capacity is still low. [0003] Recently, transition metal oxides have attracted attention in the field of lithium-ion batteries because of their relatively high theoretical specific capacity. Among these oxides, molybdenum d...

Claims

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Application Information

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IPC IPC(8): H01M4/48H01M10/0525C01G39/02
CPCC01G39/02H01M4/483H01M10/0525Y02E60/10
Inventor 张治安宋俊肖吕晓军赖延清张凯李劼
Owner CENT SOUTH UNIV
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