Oxidative grinding preparation method and application of carbon group element simple material

A group element and elemental technology, applied in the field of oxidative grinding and preparation of carbon group element materials, can solve the problems affecting the efficiency and quality of batch preparation products, low capacity of battery anode materials, poor charge-discharge cycle performance, etc., and achieve excellent electrochemical performance. performance, excellent charge-discharge cycle performance, and the effect of reducing the energy consumption of ball milling

Active Publication Date: 2021-09-21
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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  • Oxidative grinding preparation method and application of carbon group element simple material
  • Oxidative grinding preparation method and application of carbon group element simple material
  • Oxidative grinding preparation method and application of carbon group element simple material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Single elemental silicon oxide material preparation method of grinding, comprising the steps of:

[0049] (1) Synthesis of precursors:

[0050] In an argon atmosphere glove box, in a 2: 1: Chemical Formula metered 1 obtained ratio of mixing metallic lithium, zinc, silicon simple substance mixture; mixture was sealed into the tantalum container, the tantalum container is placed in a vacuum environment to heating rate 200 ℃ / h heating to 600 ℃ incubated 3h, cooled to room temperature with the furnace; tantalum container is opened in an argon atmosphere glove box, the milled powder obtained by a solid phase reaction to the non-metallic luster; the powder after regrinding sealing the tantalum container, the tantalum metal is placed in a vacuum environment to / heating rate h, 200 ℃ heated to 770 deg.] C incubation for 4h, and the furnace was cooled to room temperature; under an inert gas atmosphere the tantalum container is opened, the solid phase reaction milled to obtain pow...

Embodiment 2

[0058] Nanometer silicon performance test

[0059] Preparation Example 1 nanometer silicon embodiment of the performance tests as an electrode material of a lithium battery. Nano-silicon, acetylene black, and a binder (sodium alginate) mass ratio of 6: 2: 2 ratio thoroughly mixed, the slurry viscosity adjusting solvent is added; the slurry with a doctor blade coated on a copper current collector; in vacuo an oven dried 100 ℃ vacuum 10H; 12mm in diameter was cut into a circular sheet battery anode; in a glove box for the lithium electrode sheet assembled coin half-cell electrolyte is 1.0mol LiPF6 / EC: DMC: DEC = 1: 1: 1Vol% with 10% FEC, 2% VC. The sealed battery was allowed to stand 24h, using Land (electric blue) Battery performance test battery system cycle performance test results as image 3 Indicated. Depend on image 3 Seen, the first ring nanometer silicon discharge capacity was 2870mAh · g -1 , The first lap coulombic efficiency was 82%, preferably the first charge-discharg...

Embodiment 3

[0061] As described in Example 1, except that: after completion of step (3), the samples in a vacuum of 10 -3 PA was heated at 3h, at 600 ℃ conditions, can be collected zinc metal.

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Abstract

The present invention relates to an oxidation grinding preparation method and application of carbon group element simple material. The method is to mix an intermetallic compound with an inorganic oxidizing agent, grind and decompose the above intermetallic compound under vacuum or inert gas conditions, and obtain the corresponding carbon group element simple substance Material. The method of the present invention uses intermetallic compounds as reducing agents, selects appropriate inorganic solids or gas oxidants and grinds them after mixing. The reaction is mild and pollution-free. Compared with the direct use of active alkali metals or alkaline earth metals, it is obviously safer and more efficient. High synthesis efficiency greatly reduces the energy consumption of ball milling. The simple substance of the carbon group element prepared by the invention has excellent electrochemical properties, and exhibits higher lithium ion battery capacity and excellent charge-discharge cycle performance.

Description

Technical field [0001] The present invention relates to an oxidative abrasive preparation method of a carbon element element and its application, inorganic material technology. Background technique [0002] Nano-silicon, germanium, tin is an important semiconductor material, with a wide range of applications in photoelectric, information, and energy, the corresponding nanomaterials in aerospace, solar cells, chemical catalysts, fiber communications, biomedicine, lithium-ion batteries, etc. It is indispensable. In recent years, with the growing demand for high capacity and long life battery, people have put forward higher requirements for the performance of lithium-ion batteries. [0003] At present, the preparation method of silicon nanomaterials can be divided into two categories of physical law and chemistry. Physical law is mainly high energy ball mill, physical vapor deposition and laser treatment block silicon. The high energy ball mill is to ground silicon fine particles in...

Claims

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Application Information

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Patent Type & Authority Patents(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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