Preparation method of high-load Mn-N active site doped carbon material catalyst and application of high-load Mn-N active site doped carbon material catalyst in lithium-sulfur battery

A technology of active sites and catalysts, applied in the field of electrochemistry, can solve problems such as the difficulty of preparing catalysts, and achieve the effects of improving specific capacity and cycle stability, excellent conductivity, and improving utilization

Active Publication Date: 2021-11-16
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the low loading of M-N active sites on carbon materials has always been the biggest problem faced by this type of catalysts.
Especially the preparation of high-loaded manganese-nitrogen (Mn-N) active site doped carbon catalysts, because manganese has more valence states (0~+7) and is easy to form compounds; at the same time, it is very easy to agglomerate during pyrolysis Clustering or granular structure makes it more difficult to prepare the catalyst

Method used

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  • Preparation method of high-load Mn-N active site doped carbon material catalyst and application of high-load Mn-N active site doped carbon material catalyst in lithium-sulfur battery
  • Preparation method of high-load Mn-N active site doped carbon material catalyst and application of high-load Mn-N active site doped carbon material catalyst in lithium-sulfur battery
  • Preparation method of high-load Mn-N active site doped carbon material catalyst and application of high-load Mn-N active site doped carbon material catalyst in lithium-sulfur battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0038] Embodiment 1 Case (prepared as schematic flow diagram Figure 5 Disted):

[0039] The first step, synthesis of Mn-ZIF-8 precursor

[0040] Take 30mL2- methylimidazole methanol concentration A 1.2mmol / ml; and zinc nitrate hexahydrate takes manganese acetate and 30mL methanol was added two concentrations of 0.2mmol / ml and 0.05mmol / ml, was stirred for 30min to give solution B. At room temperature, the solution B was added to solution A slowly stirred 50min, the resulting precipitate was allowed to stand 24h washed several times with ethanol, and dried in vacuo at 70 deg.] C 14h to give Mn-ZIF-8 precursor.

[0041] The second step, low-load synthetic Mn-N site catalysts

[0042] The pyrolysis of precursor Mn-ZIF-8, the first control heating rate in an argon atmosphere were 5 ℃ / min, heated to 750 deg.] C held IH; then ammonia gas temperature after 1.5h, continued argon atmosphere replaced after the temperature was raised to 950 deg.] C 2.5h, cooled to room temperature; th...

Embodiment example 2

[0055] The first step, synthesis of Mn-ZIF-8 precursor

[0056] Take 30mL2- methylimidazole methanol concentration A 1.0mmol / ml; and take zinc nitrate hexahydrate was added manganese acetate and 30mL methanol was both concentration 0.18mmol / ml and 0.04mmol / ml, was stirred for 30min to give solution B. At room temperature, the solution B was added to solution A, stirring slowly after 30min, allowed to stand 20h obtained was washed precipitated with ethanol several times, and dried in vacuo at 60 ℃ 12h to give Mn-ZIF-8 precursor.

[0057] The second step, low-load synthetic Mn-N site catalysts

[0058] The pyrolysis of precursor Mn-ZIF-8, the first controlled argon atmosphere were a temperature rise rate 3 ℃ / min, heated to 750 deg.] C held 0.5H; then ammonia gas temperature after 1.5h, replaced with argon gas atmosphere after the temperature was raised to 900 deg.] C thermostat continues 2.5h, cooled to room temperature; the product was obtained at 70 ℃ for using 0.5mol / LH...

Embodiment example 3

[0069] The first step, synthesis of Mn-ZIF-8 precursor

[0070] Take 30mL2- methylimidazole methanol concentration A 1.4mmol / ml; and take zinc nitrate hexahydrate was added manganese acetate and 30mL methanol was both concentration 0.22mmol / ml and 0.06mmol / ml, was stirred for 30min to give solution B. At room temperature, the solution B was added to solution A, stirring slowly after 60min, allowed to stand 26h obtained was washed precipitated with ethanol several times, and dried in vacuo at 80 ℃ 16h to give Mn-ZIF-8 precursor.

[0071] The second step, low-load synthetic Mn-N site catalysts

[0072] The pyrolysis of precursor Mn-ZIF-8, the first control heating rate in an argon atmosphere were 5 ℃ / min, holding temperature was raised to 750 deg.] C for 1.5 h; then ammonia gas temperature after 2h, continued argon atmosphere replaced after the temperature was raised to 950 deg.] C 2.5h, cooled to room temperature; the product was obtained at 80 ℃ for using 0.5mol / LH 2 SO ...

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Abstract

The invention provides a preparation method of a high-load Mn-N active site doped carbon material catalyst and the application of the high-load Mn-N active site doped carbon material catalyst in a lithium-sulfur battery, and belongs to the field of energy storage batteries. According to the catalyst, a manganese-doped zinc-based metal organic framework Mn-ZIF-8 is adopted as a precursor, the number of air sites and nitrogen atom anchoring sites on a substrate material is increased through high-temperature pyrolysis evaporation of Zn atoms and ammonia NH3 treatment, and then manganese ions are secondarily adsorbed to increase the doping amount of Mn-N sites. According to the synthesis method, in-situ loading of Mn-N sites is adopted in the two steps. Meanwhile, the aperture structure of the catalyst is optimized, and the nitrogen atom doping amount is increased. When the prepared catalyst is applied to the lithium-sulfur battery, high-load Mn-N active sites and nitrogen atoms not only increase the catalysis and adsorption effects of the catalyst on polysulfide, but also ensure the high utilization rate of elemental sulfur and Li2S/Li2S2 through the high-conductivity carbon material substrate.

Description

Technical field [0001] The present invention belongs to the field of electrochemistry, relates to a Mn-N-doped active site of the carbon material catalyst and preparation method and application, in particular, it relates to a method for preparing a high-carbon material catalyst load Mn-N-doped and the active site as the finishing materials used in lithium-sulfur battery separator material modification, to effect catalysis and adsorption polysulfide. Background technique [0002] Lithium-sulfur secondary battery is a new energy storage battery, which has a high theoretical specific capacity (1675mAh g -1 ) And energy density (2600Wh kg -1 ); The same time, elemental sulfur as a cathode material having a wide variety of sources, low cost, low pollution and other advantages. Therefore, the second is a promising energy storage system. However, many problems of its own, but greatly limits its development: (1) the insulating properties of elemental sulfur results in a lower utilization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/58H01M4/62H01M10/052H01M10/42
CPCB01J27/24B01J35/0033H01M4/58H01M4/625H01M10/4235H01M10/052Y02E60/10
Inventor 张凤祥乔少明王倩
Owner DALIAN UNIV OF TECH
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