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A kind of stannous oxide material and preparation method thereof

A stannous oxide and monomer technology, which is applied in the field of stannous oxide materials and their preparation, can solve the problems of high requirements for synthesis conditions, stannous oxide oxidation, and long hydrothermal method time, so as to improve the cycle performance and the required The effect of low temperature and short preparation cycle

Inactive Publication Date: 2018-01-12
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are certain deficiencies in the preparation methods of the above-mentioned stannous oxide materials: the solid-phase method requires high temperature, vacuum or inert atmosphere, and the synthesis conditions are relatively high; the liquid-phase chemical method usually requires an ultrasonic-assisted process; the hydrothermal method takes a long time and the obtained oxidation Stannous is easily oxidized to a high valence state

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  • A kind of stannous oxide material and preparation method thereof
  • A kind of stannous oxide material and preparation method thereof
  • A kind of stannous oxide material and preparation method thereof

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preparation example Construction

[0031] The invention provides a method for preparing a stannous oxide material with a bowl-shaped structure, which includes the following steps:

[0032] Step 1: Thermally inject lithium bistrimethylsilylamide dissolved in toluene into a mixture of anhydrous stannous chloride and oleylamine at 150~180℃ to form a tin-oleylamino compound;

[0033] Sn in oleylamine 2+ The concentration is 18-20mmol / L; the concentration of lithium bistrimethylsilylamide dissolved in toluene is 0.45~0.9mol / L

[0034] Step 2: Keep the composite obtained in Step 1 at 150-180°C for 5-60 minutes, then lower to room temperature, centrifuge, and wash to obtain a bowl-shaped stannous oxide material.

[0035] The washing method is as follows: uniformly transfer the reaction product to a centrifuge tube, add toluene, ultrasonic dispersion, centrifugal separation, remove the supernatant liquid, follow the same operation, wash with tetrachloroethylene and n-hexane in sequence.

[0036] In the present invention, a conta...

Embodiment 1

[0042] 0.125mol anhydrous stannous chloride (SnCl 2 ) Was mixed with 5g oleylamine to form a mixture, heated and stirred the mixture, when the temperature rose to 150°C, 0.9mmol of lithium bistrimethylsilylamide dissolved in 2mL of toluene was thermally injected into the mixture to rapidly form tin -The oleyl amino compound, keep the temperature at 150°C, continue the reaction for 5 minutes, after the reaction is over, drop to room temperature, centrifuge, and wash to obtain stannous oxide with a bowl-like structure.

[0043] The washing method is as follows: uniformly transfer the reaction product to a centrifuge tube, add toluene, ultrasonic dispersion, centrifugal separation, remove the supernatant liquid, follow the same operation, wash with tetrachloroethylene and n-hexane in sequence.

[0044] The XRD patterns and morphologies of the bowl-shaped stannous oxide of this example are as follows: figure 1 with Figure 5 Shown from figure 1 It can be seen that the product of this ex...

Embodiment 2

[0046] 0.117mol anhydrous stannous chloride (SnCl 2 ) Was mixed with 5g oleylamine to form a mixture, heated and stirred the mixture, when the temperature rose to 150°C, 0.9mmol of lithium bistrimethylsilylamide dissolved in 2mL of toluene was thermally injected into the mixture to rapidly form tin -Oleyl amino compound, keep the temperature at 150°C, continue the reaction for 30 minutes, when the reaction is over, cool to room temperature, centrifuge, and wash to obtain stannous oxide with a bowl-like structure.

[0047] The washing method is as follows: uniformly transfer the reaction product to a centrifuge tube, add toluene, ultrasonic dispersion, centrifugal separation, remove the supernatant liquid, follow the same operation, wash with tetrachloroethylene and n-hexane in sequence.

[0048] The XRD patterns and morphologies of the bowl-shaped stannous oxide of this example are as follows: figure 2 with Image 6 Shown from figure 2 It can be seen that the product of this examp...

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Abstract

The invention discloses a bowl-shaped stannous oxide material. The stannous oxide monomer has a circular cavity structure; the diameter of the stannous oxide monomer is 0.9-2.4 μm, and the circular cavity in the monomer is The diameter of the cavity is 0.5~1.1μm; mix anhydrous stannous chloride and oleylamine, heat and stir, add lithium bistrimethylsilylamide dissolved in toluene into the mixture at 150~180°C. Insulate for 5-60 minutes, then cool down to room temperature, centrifuge and wash to obtain a bowl-shaped stannous oxide material. The bowl-shaped stannous oxide material prepared by the present invention has good uniformity and can be used as a negative electrode material for lithium ion batteries; the cavity structure of the bowl-shaped stannous oxide prepared by the present invention is a good buffer between Li‑Sn alloy and The volume changes during the dealloying reaction and the structure remains stable, effectively improving the cycle performance of lithium-ion batteries.

Description

Technical field [0001] The invention belongs to the technical field of metal oxide materials, and specifically relates to a stannous oxide material and a preparation method thereof. Background technique [0002] Stannous oxide (SnO), also known as tin monoxide. Stannous oxide is an important metal oxide with a direct optical band gap of 2.5-3.4 eV. It is a natural p-type semiconductor and has attracted attention due to its large hole mobility. In recent years, due to its high theoretical specific capacity (875mAh / g), stannous oxide has been widely used in the field of lithium-ion batteries. At the same time, stannous oxide can also be used in gas-sensing materials, catalyst materials and the preparation of tin dioxide The precursors and other aspects. However, since stannous oxide is a metastable material and cannot be directly obtained in nature, the research on the preparation methods of stannous oxide with different morphologies and sizes is of great significance. In the ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02H01M4/48H01M10/0525
CPCC01G19/02C01P2002/72C01P2004/03C01P2004/61C01P2004/62H01M4/483H01M10/0525Y02E60/10
Inventor 郭昱希王英楠赵武张志勇闫军锋翟春雪贠江妮李强许曼章徐盼盼
Owner NORTHWEST UNIV
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