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Oxidation grinding preparation method and application of carbon group element elementary substance material

A family element and simple substance technology, which is applied in the field of oxidative grinding preparation of carbon group element simple substance materials, can solve problems that affect the efficiency and quality of mass-produced products, low capacity of battery negative electrode materials, poor charge-discharge cycle performance, etc., and achieve excellent electrochemical performance. high performance, reduced ball mill energy consumption, and mild reaction

Active Publication Date: 2020-12-04
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The decomposition efficiency of this method is low, air oxidation decomposition takes several months, and the ball milling decomposition method under the protection of vacuum / inert gas is only applicable to the situation that the amount of precursor is less (less than 10g), when the amount of ternary alloy precursor When it is larger (more than 100 grams), it is difficult to complete the decomposition reaction by a single ball milling method, and a large amount of undecomposed alloy precursors remain in the product, which seriously affects the efficiency and quality of batch preparation products
[0005] Chinese patent document CN101682027A discloses a method for preparing a material comprising at least one Group 14 element by thermal decomposition of a ternary phase, also known as Zintel phase, or by reaction of the ternary phase with an organic oxidizing solvent, but The battery anode material prepared by this method has low capacity and poor charge-discharge cycle performance, and the initial capacity of the prepared silicon nanomaterial is only 1500mAh g -1 , and after 7 charge-discharge cycles, the capacity fades to 700mAh·g -1 , the decrease rate exceeds 50%, indicating that there are obvious problems in the uniformity of the silicon nanomaterials prepared by the above method, so the performance decays sharply during the charge and discharge process

Method used

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  • Oxidation grinding preparation method and application of carbon group element elementary substance material
  • Oxidation grinding preparation method and application of carbon group element elementary substance material
  • Oxidation grinding preparation method and application of carbon group element elementary substance material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A method for preparing a silicon elemental material by oxidation and grinding, comprising the following steps:

[0049] (1) Synthesis of precursors:

[0050] In the argon atmosphere glove box, according to the stoichiometric ratio of 2:1:1, the simple substances of metal lithium, zinc, and silicon were mixed to obtain a mixture; the mixture was sealed in a metal tantalum container, and the metal tantalum container was placed in a vacuum environment to Raise the temperature to 600°C at a heating rate of 200°C / h for 3 hours, then cool to room temperature with the furnace; open the metal tantalum container in an argon atmosphere glove box, and grind the powder obtained by the solid phase reaction until it has no metallic luster; grind the powder again Seal it into a metal tantalum container, place the metal tantalum in a vacuum environment, raise the temperature to 770 °C at a heating rate of 200 °C / h and keep it for 4 hours, and cool to room temperature with the furnace; ...

Embodiment 2

[0058] Performance test of nano-silicon

[0059] The nano-silicon prepared in Example 1 was used as an electrode material for a lithium battery for performance testing. Fully mix nano-silicon, acetylene black and binder (sodium alginate) in a mass ratio of 6:2:2, add a solvent to adjust the viscosity of the slurry; apply the slurry on the copper current collector with a scraper; Vacuum dry at 100°C in a drying oven for 10 hours; cut it into circular battery negative electrodes with a diameter of 12mm; assemble a button half-cell in a glove box with a lithium sheet as the counter electrode, and the electrolyte is 1.0mol LiPF6 / EC:DMC: DEC=1:1:1 Vol% with 10% FEC, 2% VC. Let the sealed battery stand for 24 hours, and use the Land (Blue Electric) battery performance test system to test the cycle performance of the battery. The test results are as follows: image 3 shown. Depend on image 3 It can be seen that the first discharge specific capacity of nano-silicon is 2870mAh·g ...

Embodiment 3

[0061] As described in Example 1, the difference is: after completing step (3), the sample is vacuumed at 10 -3 Pa, the temperature is 600 ℃ under the conditions of heating for 3 hours, can collect metal zinc.

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Abstract

The invention relates to an oxidation grinding preparation method and application of a carbon group element elementary substance material. The method comprises the following steps: mixing an intermetallic compound and an inorganic oxidant, and grinding and decomposing the intermetallic compound under vacuum or inert gas conditions to obtain the corresponding carbon group element elementary substance material. According to the method, an intermetallic compound is used as a reducing agent, and a proper inorganic solid or gas oxidizing agent is selected to be mixed and then ground, wherein the reaction is mild, pollution is avoided, and compared with direct use of active alkali metal or alkaline-earth metal, the method is obviously high in safety and higher in synthesis efficiency, and ball milling energy consumption is greatly reduced. The carbon group element elementary substance prepared by the method has excellent electrochemical performance, and shows relatively high lithium ion battery capacity and excellent charge-discharge cycle performance.

Description

technical field [0001] The invention relates to an oxidation grinding preparation method and application of a carbon group element elemental material, and relates to the technical field of inorganic materials. Background technique [0002] Nano-silicon, germanium, and tin are important semiconductor materials, which are widely used in the fields of optoelectronics, information, and energy. The corresponding nano-materials are used in aerospace, solar cells, chemical catalysts, optical fiber communications, biomedicine, and lithium-ion batteries is indispensable. In recent years, with the increasing demand for high-capacity, long-life batteries in mobile electronic devices, higher performance requirements have been placed on Li-ion batteries. [0003] At present, the preparation methods of silicon nanomaterials can be divided into two categories: physical methods and chemical methods. The physical methods are mainly high-energy ball milling, physical vapor deposition and la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/38H01M4/134H01M10/0525C01B33/02B82Y30/00
CPCB82Y30/00C01B33/02H01M4/134H01M4/386H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 夏盛清谭文杰刘超刘小村
Owner SHANDONG UNIV
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