Large-scale preparation of high-crystallinity prussian blue analogue for sodium ion battery based on'water-in-salt 'microreactor principle

A sodium-ion battery and ion battery technology, which is applied in the preparation and application of manganese-based Prussian blue analogues, can solve problems such as poor cycle stability, increased production costs, and cumbersome process flow, and achieve good rate performance, less defects, and The effect of simple process

Active Publication Date: 2022-03-29
温州大学碳中和技术创新研究院
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prussian blue materials are mostly synthesized by the traditional co-precipitation method, which reacts quickly and produces considerable [Fe(CN) 6 ] 4- defects and a large amount of interstitial water, which makes the product have a very large irreversible structure and low sodium content, resulting in low capacity and poor cycle stability
In order to solve the problems of rapid co-precipitation, researchers have adopted many strategies in recent years, including controlling the synthesis temperature and adding chelating agents to slow down the growth of crystal nuclei. The process is cumbersome

Method used

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  • Large-scale preparation of high-crystallinity prussian blue analogue for sodium ion battery based on'water-in-salt 'microreactor principle
  • Large-scale preparation of high-crystallinity prussian blue analogue for sodium ion battery based on'water-in-salt 'microreactor principle
  • Large-scale preparation of high-crystallinity prussian blue analogue for sodium ion battery based on'water-in-salt 'microreactor principle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Manganese sulfate monohydrate (4mmol) and sodium ferrocyanide decahydrate (6mmol) were thoroughly mixed and ground according to the molar ratio of 1:1.5, the mixture was transferred to a stainless steel ball mill jar (50mL), and zirconia ball mill beads were added (Ball to material ratio is about 10:1), at 300rmp speed, mechanical ball milling in air atmosphere for 24h, the product was washed 3 times with deionized water, washed 1 time with ethanol, to remove impurities and unreacted raw materials, in a vacuum oven at 120 After drying at ℃ for 12h, the product MnHCF-S was obtained.

[0030] (2) Heat treatment: the product MnHCF-S obtained in (1) is heated at 1°C·min in an argon atmosphere -1 The heating rate was raised to 170 °C, and the temperature was kept for 12 hours to obtain the target product, namely MnHCF-S-170 material. figure 1 Shown is the scanning electron microscope image of the MnHCF-S-170 material, and it can be seen that it presents an elliptical sh...

Embodiment 2

[0035] The difference between this embodiment and Example 1 is that there is no step (2) in Example 1, and other conditions are exactly the same as Example 1 to obtain the MnHCF-S material.

[0036] The scanning electron microscope picture of the MnHCF-S material that embodiment 2 obtains is as figure 2 As shown, it presents an oval shape similar to that of MnHCF-S-170.

Embodiment 3

[0038] (1) MnHCF-L was prepared using the same materials as in Example 1. Manganese sulfate monohydrate (4mmol) was dispersed in 40mL deionized water, and magnetically stirred at room temperature for 3h to form solution A, and sodium ferrocyanide decahydrate (6mmol) was dissolved in 40mL deionized water to form solution B.

[0039] (2) Pour A into solution B under continuous stirring, and then age the resulting mixed solution at room temperature for 24 h. The product was washed three times with deionized water and once with ethanol to remove impurities and unreacted raw materials, and the collected product was dried in a vacuum oven at 120°C for 12 hours. The resulting sample was labeled MnHCF-L.

[0040] The scanning electron micrograph of the MnHCF-L material that embodiment 3 obtains is as image 3 As shown, it presents an oval shape of 10-100 nm.

[0041] Figure 4 It is the XRD comparison diagram of the three products of Examples 1-3, which can prove that the products...

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Abstract

The Prussian blue analogue (PBA) has the advantages of low cost, rich redox active sites, open channel structure and the like, and is considered to be an excellent positive electrode material of a rechargeable sodium ion battery. However, commercialization of PBA-based sodium-ion batteries still faces a series of problems, such as poor cycling stability, which may be attributed to the generation of large amounts of [Fe (CN) 6] defects and interstitial water during rapid growth of crystals. The invention provides a'water-in-salt 'microreactor for synthesizing high-quality PBA, namely PBA with low defect, low crystal water content and high crystallinity, which is used as a positive electrode of a sodium-ion battery and shows high specific capacity and excellent rate capability. From the practical perspective, compared with PBA synthesized by a traditional coprecipitation method, the PBA shows better performance in the aspects of air stability, high and low temperature and total battery. The work can promote the application and development of the PBA in a power grid scale sodium ion energy storage system.

Description

technical field [0001] The invention relates to the field of sodium ion battery materials, in particular to the preparation and application of a manganese-based Prussian blue analog (MnHCF-S-170) with low defects, low crystal water content and high crystallinity. [0002] technical background [0003] In recent years, due to serious environmental pollution and water shortage, there is an urgent need to develop clean energy, and lithium-ion batteries have emerged as the times require. With the gradual development and application of lithium-ion batteries from portable electronic devices to high-power electric vehicles, large-scale energy storage power stations and smart grids, the demand for lithium-ion batteries is increasing, but limited lithium resources limit the availability of lithium-ion batteries. Continuous development. And sodium reserves are abundant, and sodium and lithium belong to the same main group, and their chemical properties are similar. Therefore, sodium-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/1397H01M10/054C01C3/12B82Y40/00
CPCH01M4/58H01M4/1397H01M10/054C01C3/12B82Y40/00C01P2004/03C01P2002/72C01P2006/40C01P2004/64C01P2004/30H01M2004/028Y02E60/10
Inventor 侴术雷高云彭建张旺
Owner 温州大学碳中和技术创新研究院
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