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Preparation method and application of ultrafine phosphorous-doped porous silicon nanomaterial

A technology of nanomaterials and phosphorus doping, applied in the field of preparation of porous silicon nanomaterials, can solve the problems of particle size limitation, small volume effect, high cost, etc., and achieve controllable production process, simple preparation method and low cost Effect

Active Publication Date: 2022-05-06
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the smaller the particle size of silicon nanomaterials, the smaller the volume effect and the better the capacity expression efficiency. The industry generally adopts the method of high-energy ball milling to pulverize metal silicon powder to prepare nano-silicon materials. The disadvantage is high energy consumption and high cost. , particle size is limited (about 100nm)

Method used

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  • Preparation method and application of ultrafine phosphorous-doped porous silicon nanomaterial
  • Preparation method and application of ultrafine phosphorous-doped porous silicon nanomaterial
  • Preparation method and application of ultrafine phosphorous-doped porous silicon nanomaterial

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Effect test

Embodiment 1

[0032] 1) Ball mill n-type silicon wafers to powder particles of 5-10 μm, grind and mix with 400-mesh metal magnesium powder, heat treatment at 700 °C for 6 hours at a heating rate of 5 °C / min in a vacuum state;

[0033] 2) After the reaction product in step 1) is cooled to room temperature, continue to pass in an oxygen / argon mixed gas containing 10% oxygen by volume, heat treatment at 700°C for 5 hours at a heating rate of 5°C / min;

[0034] 3) Rinse the product obtained in step 2) with hydrochloric acid with a concentration of 1mol / L for 3 hours, completely remove the reaction impurities, take it out, wash it in deionized water for 20 minutes, centrifuge, and then rinse it with hydrofluoric acid with a concentration of 1% by mass for 30 minutes. After the reaction product was centrifuged and washed three times with deionized water, it was vacuum-dried at 65° C. into powder.

[0035] figure 1 X-ray diffraction pattern (bottom curve) of the silicon / silicon-magnesium alloy com...

Embodiment 2

[0038] 1) Ball mill n-type silicon wafers to powder particles of 5-10 μm, grind and mix with 400 mesh metal magnesium powder, heat treatment at 650 °C for 4 hours at a heating rate of 5 °C / min in a vacuum state;

[0039] 2) After the reaction product in step 1) is cooled to room temperature, continue to pass in an oxygen / argon mixed gas containing 10% oxygen by volume, heat treatment at 700°C for 5 hours at a heating rate of 5°C / min;

[0040] 3) Rinse the product obtained in step 2) with hydrochloric acid with a concentration of 1mol / L for 3 hours, completely remove the reaction impurities, take it out, wash it in deionized water for 20 minutes, centrifuge, and then rinse it with hydrofluoric acid with a concentration of 1% by mass for 30 minutes. After the reaction product was centrifuged and washed three times with deionized water, it was vacuum-dried at 65° C. into powder.

[0041] figure 1 The X-ray diffraction pattern (middle curve) of the silicon / silicon-magnesium alloy...

Embodiment 3

[0044] 1) Ball mill n-type silicon wafers to powder particles of 5-10 μm, grind and mix with 400-mesh metal magnesium powder, and heat-treat at 600 °C for 5 hours at a heating rate of 5 °C / min in a vacuum state;

[0045] 2) After the reaction product in step 1) is cooled to room temperature, continue to pass in an oxygen / argon mixed gas containing 10% oxygen by volume, heat treatment at 700°C for 5 hours at a heating rate of 5°C / min;

[0046] 3) Rinse the product obtained in step 2) with hydrochloric acid with a concentration of 1mol / L for 3 hours, completely remove the reaction impurities, take it out, wash it in deionized water for 20 minutes, centrifuge, and then rinse it with hydrofluoric acid with a concentration of 1% by mass for 30 minutes. After the reaction product was centrifuged and washed three times with deionized water, it was vacuum-dried at 65° C. into powder.

[0047] figure 1 and figure 2 d is the X-ray diffraction pattern (top curve) of the silicon / silico...

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Abstract

The invention discloses a method for preparing ultrafine phosphorus-doped porous silicon nanomaterials, which comprises the following steps: carrying out incomplete alloying reaction between n-type phosphorus-doped silicon powder and metal silicon powder at different temperatures, and then using the synthesized The silicon / silicon-magnesium alloy mixture is placed in an oxygen / argon mixed atmosphere at a certain temperature for heat treatment for re-decomposition, and finally pickled to obtain phosphorus-doped porous silicon nanomaterials with a porous structure and ultrafine primary particle size. The present invention effectively overcomes the The traditional high-energy ball milling method for nano-silicon is overcome, and phosphorus-doped porous silicon materials with a primary particle size of less than 100nm are prepared, which is beneficial to solve key problems such as volume expansion and poor conductivity during the charge-discharge process of silicon electrodes. It is used as a negative electrode material for lithium In lithium-ion batteries, the cycle stability of lithium-ion batteries is significantly improved.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a preparation method and application of a phosphorus-doped porous silicon nanomaterial with primary particle size. Background technique [0002] Lithium-ion batteries are widely used in consumer electronics, aerospace, biomedical and large-scale energy storage due to their remarkable advantages such as stable working voltage, high charging efficiency and energy density, low self-discharge rate, no memory effect and long service life. Especially in the environment where the country vigorously advocates the development of new energy vehicles, lithium-ion batteries, as an ideal power source for a new generation of electric vehicles, have broad development prospects. However, with the development of the power battery market towards high energy density, long cycle life and high safety, there is an urgent need for the development and application of new lithium-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M10/0525B82Y30/00B82Y40/00
CPCH01M4/362H01M4/386H01M4/38H01M10/0525B82Y30/00B82Y40/00H01M2004/027Y02E60/10
Inventor 陈逸凡徐聪徐斐然戴尚义徐思源鲍亮元勇军
Owner HANGZHOU DIANZI UNIV