Method for in-situ synthesizing silicate/carbon composite cathode material by taking rice husk carbon as silicon source

A cathode material, in-situ synthesis technology, applied in battery electrodes, electrical components, circuits, etc., can solve the problem of low resource utilization and achieve the effect of resource utilization

Active Publication Date: 2013-10-09
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Chinese invention patent CN101499527A uses Na2SiO4 as a silicon source to synthesize lithium iron silicate positive electrode material by co-precipitation method; paper [Electrochemistry Communications, 2005, 7(2) :156-160] and [Journal of Power Sources,2006,160:1381-1386] both used Li2SiO3 as silicon source and synthesized by solid phase method Lithium iron silicate; papers [Electrochemistry Communications, 2006, 9 (12): A542-A544], [Electrochemical and Solid-State Letters, 2008, 11 (5): A60-A63] and Chinese patents CN101764227, CN1803608A, etc. Ethyl orthosilicate is used as a raw material, and iron manganese lithium silicate cathode material is synthesized by a sol-gel method. However, in the above-mentioned documents, glucose or sucrose is added as a carbon source, and the resource utilization rate is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Bake the rice husk in an oven at 100℃ for 2 hours, then crush the dried rice husk to 100 mesh with an ordinary crusher, then take 200g into a 1000ml round bottom flask with a reflux condenser, and add 600ml of 10% concentration HCl, heat to reflux for 2h, filter, and wash rice husk powder with deionized water to neutrality. The rice husk powder purified by pickling was dried in an oven at 120°C for 3 hours. Detection of SiO in dried rice husk powder by Shimadzu XRF-1800 X-ray fluorescence spectrometer 2 The content is 15.93%, the others are a small amount of CaO, MgO and Al 2 O 3 And other impurities. The silica content in the rice husk ash was further determined by the method for determining the silica content in the HG / T3062-2008 standard. The results showed that the silica content in the rice husk ash was 15.71%. Weigh ferrous oxalate and rice husk powder at a ratio of Fe:Si=1:1, grind and mix them thoroughly with ethanol as a dispersant for 10 hours, after the ethan...

Embodiment 2

[0022] Crush the dried rice husk to 300 mesh with a common grinder, then take 200g into a 1000ml round bottom flask with a reflux condenser, add 600ml of HCl with a concentration of 10%, heat to reflux for 2h, filter, and use deionized water Wash the rice husk to neutral. The purified rice husks were dried in an oven at 120°C for 3 hours. Detection of SiO in dried rice husk powder by Shimadzu XRF-1800 X-ray fluorescence spectrometer 2 The content is 15.93%. The silica content in the rice husk ash was further determined by the method for determining the silica content in the HG / T3062-2008 standard. The results showed that the silica content in the rice husk ash was 15.71%. Weigh out manganese carbonate and rice husk powder at a ratio of Mn:Si=1:1, grind and mix them thoroughly with ethanol as a dispersant for 10 hours, after the ethanol evaporates, transfer to a fixed bed, use high-purity nitrogen as carrier gas, 100ml / min, the temperature is increased to 475°C at a heating r...

Embodiment 3

[0026] Weigh out manganese carbonate ferrous oxalate and the purified rice husk powder in Example 1 with a measurement ratio of Mn:Fe:Si=0.5:0.5:1. Use ethanol as a dispersant to thoroughly grind and mix for 10 hours. After the ethanol evaporates, transfer to In the fixed bed, high-purity nitrogen is used as the carrier gas, 100ml / min, the temperature is raised to 750°C at a heating rate of 100°C / min in the fixed bed, and the SiMnFeO / C mixture is obtained after 1h rapid pyrolysis.

[0027] Pulverize rice husk charcoal with a jet mill to a D50 of 1.4um (detected by Mastersize2000 laser particle size analyzer). The lithium carbonate and the crushed SiMnFeO / C mixture were weighed with the measurement ratio of Li:Mn=2.07:0.5, and acetone was used as a dispersant to fully grind and mix for 14 hours. After the acetone is volatilized, it is transferred to a porcelain boat in a tubular resistance furnace under nitrogen protection, heat-treated at 700°C for 10 hours, and naturally cooled ...

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Abstract

A disclosed method for in-situ synthesizing a silicate/carbon composite cathode material by taking rice husk carbon as a silicon source comprises the following preparation steps: (1) primary smashing of rice husks; (2) purification of the rice husks; (3) pyrolyzing the rice husks under catalysis of metal elements to obtain a SiMO/C mixture; (4) smashing the SiMO/C mixture to D50=1-2 [mu]m by an jet mill; (5) adding a lithium source, ball milling and mixing; and (6) sintering under gas protection to obtain Li2MSiO4/C. According to the method, cheap biological silica is used to prepare the silicate cathode material, resource utilization of agriculture wastes is realized, and high added-value products are produced; at the same time, the rice husk carbon is obtained by the middle-temperature pyrolysis method, the residual carbon of the rice husk carbon is taken as a carbon source, and the synthesis process of the silicate cathode material does not need extra carbon, and the in-situ synthesis of the Li2MSiO4 material is realized synchronously.

Description

technical field [0001] The invention mainly relates to a method for synthesizing a silicate / carbon composite cathode material, in particular to a method for in-situ synthesis of a silicate / carbon composite cathode material using rice husk charcoal as a silicon source. Background technique [0002] In the synthesis literature of silicate cathode materials, the choice of silicon source varies. The paper published in [Chinese Journal of Nonferrous Metals, 2009, 19(8): 1449-1454] and the Chinese patent CN101807690A all disclose that lithium source, iron source and silicon dioxide are used as raw materials, and synthesized by microwave synthesis after solid phase ball milling Lithium iron silicate. Chinese invention patent CN101499527A with Na 2 SiO 4 As a silicon source, lithium iron silicate cathode materials were synthesized by co-precipitation; papers [Electrochemistry Communications, 2005, 7(2): 156-160] and [Journal of Power Sources, 2006, 160: 1381-1386] both used Li ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36
CPCY02E60/10
Inventor 杨续来宋金保
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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