A method for in-situ synthesis of silicate/carbon composite cathode material using rice husk powder as a silicon source

A positive electrode material and 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: 2015-12-09
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Abstract
  • Description
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Problems solved by technology

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] all use Li 2 SiO 3 As a silicon source, lithium iron silicate was synthesized by a solid-phase method; papers [Electrochemistry Communications, 2006, 9(12): A542-A544], [Electrochemical and Solid-State Letters, 2008, 11(5): A60-A63] and Chinese patents CN101764227, CN1803608A, etc. all use tetraethyl orthosilicate as a raw material, and synthesize iron manganese lithium silicate positive electrode materials by the method of sol-gel, but in the above-mentioned documents, all add glucose or sucrose as carbon source, and the resource utilization rate is not high. high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dry the rice husk in an oven at 100°C for 2 hours, then crush the dried rice husk to 100 mesh with an ordinary grinder, then take 200g and put it into a 1000ml round bottom flask with a reflux condenser, add 600ml of 10% HCl, heated to reflux for 2h, filtered, and washed rice husk powder with deionized water until neutral. The pickled and purified rice husk powder 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%, others are a small amount of CaO, MgO and Al 2 o 3 and other impurities. The silicon dioxide content in the rice husk ash was further determined by using the method for determining the silicon dioxide content in the HG / T3062-2008 standard, and the results showed that the silicon dioxide content in the rice husk ash was 15.71%. Weigh ferrous oxalate and rice husk powder with a metering ratio of Fe:Si=1:1, use ethanol as a dispersant to fully grin...

Embodiment 2

[0022] Grind the dried rice husk to 300 mesh with an ordinary grinder, then take 200g and put it 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 hulls to neutral. The pickled and purified rice husks were dried in an oven at 120 °C for 3 h. Detection of SiO in dried rice husk powder by Shimadzu XRF-1800 X-ray fluorescence spectrometer 2 The content is 15.93%. The silicon dioxide content in the rice husk ash was further determined by using the method for determining the silicon dioxide content in the HG / T3062-2008 standard, and the results showed that the silicon dioxide content in the rice husk ash was 15.71%. Weigh manganese carbonate and rice husk powder with a metering ratio of Mn:Si=1:1, use ethanol as a dispersant to fully grind and mix for 10 hours, after the ethanol volatilizes, transfer to a fixed bed, use high-purity nitrogen as a carrier gas, ...

Embodiment 3

[0026] Take by weighing ferrous manganese carbonate ferrous oxalate and purified rice husk powder in Example 1 with the metering ratio of Mn:Fe:Si=0.5:0.5:1, use ethanol as a dispersant to fully grind and mix for 10h, after the ethanol volatilizes, transfer to In the fixed bed, high-purity nitrogen is used as the carrier gas, 100ml / min, and 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 rapid pyrolysis for 1 hour.

[0027] The rice husk charcoal was crushed with a jet mill until the D50 was 1.4um (detected by Mastersize2000 laser particle size analyzer). Lithium carbonate and pulverized SiMnFeO / C mixture were weighed at a metering ratio of Li:Mn=2.07:0.5, and thoroughly ground and mixed with acetone as a dispersant for 14 hours. After the acetone is volatilized, it is transferred to a porcelain boat and placed in a tubular resistance furnace under the protection of nitrogen, heat-treated at 700°C ...

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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 synthesizing a silicate / carbon composite cathode material in situ using rice husk powder 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] all use Li 2 Si...

Claims

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Application Information

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Patent Type & Authority Patents(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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