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A magnesium secondary battery anode material and the corresponding preparation method

A technology for magnesium secondary batteries and positive electrode materials, which is applied in electrode manufacturing, battery electrodes, chemical instruments and methods, etc., can solve the problems of insufficient discharge platform stability, poor cycle performance, and no major breakthroughs, and achieves a voltage platform. High, improved integrity, large contact interface effect

Inactive Publication Date: 2008-07-09
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Other transition metal oxides such as V 6 o 13 , Mn 2.15 co 0.37 o 4 ,Co 3 o 4 , Mn 2 o 3 , RuO 2 Some people have done corresponding research, but the cycle performance is not very good
In 2001, Koji Makino et al synthesized Mg with Nasicon structure by sol-gel method 0.5 Ti 2 (PO 4 ) 3 and Mg 0.5+y (Fe y Ti 1-y ) 2 (PO 4 ) 3 (0.1≤y≤0.5), at lmol / LMg(ClO 4 ) 2 In / PC electrolyte, the intercalation reaction of magnesium can be observed, but there is no report of reversibility (Magnesium insertion intoMg 0.5+y (Fe y Ti 1-y ) 2 (PO 4 ) 3 , J. Power Sources, 2001, 97-98: 512)
Our research group has achieved certain results by using organic sulfides and organic sulfur polymers as cathode materials for magnesium secondary batteries, and the discharge platform can reach 1.35V (Nu Liyanna, Yang Jun, Li Xiaoming, Feng Zhenzhen, organic Application of cathode materials for magnesium batteries, application number: 200610027411.5), even 1.6V (Nuli Yanna, Yang Jun, Xie Fusu, Application of organosulfur polymers in cathode materials for secondary magnesium batteries, application number: 200610027413.4) , but the 1.6V discharge platform is not stable enough, and the discharge capacity reaches 110mAhg -1 left and right, with Mo 3 S 4 no big breakthrough compared to

Method used

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  • A magnesium secondary battery anode material and the corresponding preparation method
  • A magnesium secondary battery anode material and the corresponding preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Add 1.1 g of nano silicon dioxide to 190 g of water, ultrasonicate for 2 hours, then add 7.9 g of citric acid and 7.0 g of ethylene glycol, and stir vigorously to obtain a suspension;

[0028] (2) 4.1g magnesium acetate tetrahydrate (MgAc 2 4H 2 O) and 4.5g manganese acetate tetrahydrate (MnAc 2 4H 2 O) Dissolve in 50g water respectively to make two solutions, then add to the suspension obtained in step (1), continue to stir for 9 hours, then stir and dry at 60°C for 24 hours to obtain dry gel, namely silicic acid Manganese and magnesium precursors;

[0029] (3) After the xerogel is pulverized with a mortar, transfer to an agate ball mill jar equipped with an O-ring, add 10g of absolute ethanol as a dispersant, and carry out ball milling. The rotating speed of the high-energy ball mill is 450 rpm. Ball mill for 5 hours, then open the ball mill jar, transfer to a quartz boat after the ethanol volatilizes, heat treat at 750° C. for 48 hours under protective atmosp...

Embodiment 2

[0035] (1) Add 1.1 g of nano-silica to 95 g of water, ultrasonicate for 2 hours, then add 7.9 g of citric acid and 7.0 g of ethylene glycol, and stir vigorously to obtain a suspension;

[0036] (2) 4.1g magnesium acetate tetrahydrate (MgAc 2 4H 2 O) and 4.5g manganese acetate tetrahydrate (MnAc 2 4H 2 O) be dissolved in 60g water respectively to form two solutions, then add to the suspension obtained in step (1), continue to stir for 10 hours, then stir and dry at 60°C for 24 hours to obtain xerogel, i.e. silicic acid Manganese and magnesium precursors;

[0037] (3) After the xerogel is pulverized with a mortar, it is transferred to an agate ball mill jar equipped with an O-ring, 2g of sucrose is added, and 12g of absolute ethanol is added as a dispersant for ball milling. The rotating speed of the high-energy ball mill is 450 rpm, ball milling for 4 hours, then open the ball milling tank, after the ethanol volatilizes, transfer to a quartz boat, heat treatment at 800°C fo...

Embodiment 3

[0043] (1) Add 3.0 g of nano-silica to 400 g of water, ultrasonicate for 3 hours, then add 21.0 g of citric acid and 18.6 g of ethylene glycol, and stir vigorously to obtain a suspension;

[0044] (2) 7.6g magnesium oxalate dihydrate (MgC 2 o 4 2H 2 O) and 8.7g manganese oxalate dihydrate (MnC 2 o 4 2H 2 O) be dissolved in 150g water respectively to form two solutions, then add to the suspension obtained in step (1), continue to stir for 20 hours, then stir and dry at 70°C for 40 hours to obtain dry gel, i.e. silicic acid Manganese and magnesium precursors;

[0045](3) After the xerogel is pulverized with a mortar, transfer it to a ball mill jar equipped with an O-ring, add 8g of β-cyclodextrin, then add 15g of absolute ethanol as a dispersant, and carry out ball milling. The rotating speed is 500 rpm, ball milling for 5 hours, then open the ball milling tank, after the absolute ethanol volatilizes, transfer to a quartz boat, heat treatment at 750°C for 48 hours under pr...

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Abstract

The invention discloses a magnesium rechargeable battery anode material and the preparation method. The anode material is a carbon-coated magnesium manganese silicate, the chemical structural formula is MgxMnySiO4 / C, wherein, x is not less than 1 and not more than 1.03, y is not less than 0.97 and not more than 1, the content of the magnesium manganese silicate is 83.2 to 100 percent and the content of the carbon is 0 to 16.8 percent according to weight percentage, and the invention is a grey to black powder. The invention takes nano-silicon dioxide as a silicon source and adopts a modified sol-gel method for obtaining a magnesium manganese silicate precursor, and the magnesium rechargeable battery anode material is obtained by carbon coating processing and subsequent heat processing under the condition of protection atmosphere. The invention has good electrochemical charge-discharging behaviors, a discharging plateau is stabilized to achieve 1.6V (vs.Mg / Mg<2 PLUS>), the discharging capacity under the small current charge-discharging condition (C / 100) can achieve 243.9mAh.g<MINUS 1> (78 percent of theoretical capacity); compared with the ideal anode material Mo3S4 of a current magnesium rechargeable battery, the carbon-coated magnesium manganese silicate has the advantages of simple preparation, large capacity and high voltage plateau ,etc.

Description

technical field [0001] The invention relates to a battery electrode material and a preparation method thereof, in particular to a magnesium secondary battery cathode material and a preparation method thereof. Background technique [0002] With the decreasing reserves of fossil fuels represented by the three main energy sources of coal, oil and natural gas, chemical power sources have received great attention in the development and utilization of high-tech devices, green and low-energy transportation, and renewable energy. Among the existing primary and secondary batteries, lithium batteries have the highest energy density, so they are widely researched and applied. However, due to the high activity of metal lithium, the reliability and safety of lithium batteries are difficult to be guaranteed, especially in large-scale power lithium secondary batteries, there are still many safety hazards. Therefore, traditional toxic and low-capacity lead-acid or nickel-cadmium batteries ...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/48H01M4/04C01B33/20C01F5/00
CPCY02E60/10
Inventor 杨军冯真真努丽燕娜王久林
Owner SHANGHAI JIAO TONG UNIV
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