Unlock instant, AI-driven research and patent intelligence for your innovation.

Ultrafine iron-based Prussian blue and its analogue, preparation method and sodium-ion battery

A technology of Prussian blue and analogs, applied in the preparation of ultra-fine iron-based Prussian blue and its analogs, and the application field of cathode materials for sodium ion batteries, can solve the problems of unsuitability for large-scale production, low concentration of reactants, and kinetics. Poor performance and other problems, to achieve the effects of excellent cycle stability performance and rate performance, good rate performance and long cycle life

Active Publication Date: 2021-07-23
张五星
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure the crystallization quality of the product in this method, the concentration of reactants in the above method is generally low, resulting in low yield and not suitable for large-scale production
In addition, the particle size of PBAs synthesized by mild liquid phase reaction is often larger than 200nm, and the intrinsic electronic conductivity of PBAs is very low (4.08×10 -9 S cm -1 ), resulting in poor kinetic performance when used as anode material for sodium-ion batteries

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Ultrafine iron-based Prussian blue and its analogue, preparation method and sodium-ion battery
  • Ultrafine iron-based Prussian blue and its analogue, preparation method and sodium-ion battery
  • Ultrafine iron-based Prussian blue and its analogue, preparation method and sodium-ion battery

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0036] The invention provides a kind of preparation method of superfine iron-based Prussian blue and its analogues, comprising the following steps:

[0037] (1) Sodium ferrocyanide and metal salts are added to the ball mill;

[0038] (2) adding an appropriate amount of solvent in the ball milling device;

[0039] (3) placing the mixed raw materials in the ball milling device for ball milling;

[0040] (4) Wash the obtained PBAs with absolute ethanol and deionized water.

[0041] (5) drying the cleaned product.

[0042] The preparation method of the ultrafine iron-based Prussian blue and its analogues of the present invention is not limited to the size of the ball mill pot, the ball milling method and the ball milling time. Metal salts include metal chloride salts (FeCl 2 、CoCl 2 , MnCl 2 etc.), metal sulfate (FeSO 4 、CoSO 4 and MnSO 4 etc.) or perchlorate (Fe(ClO 4 ) 2 , Mn(ClO 4 ) 2 , Co(ClO 4 ) 2 ), etc., the added sodium ferrocyanide and metal salt may contai...

Embodiment 1

[0046] S1: 4 mmol of sodium ferrocyanide decahydrate and 6 mmol of ferrous chloride tetrahydrate were placed in a nylon ball mill jar, and vibrated and mixed at a rate of 1200 r / min for 1 min.

[0047] S2: In a glove box filled with Ar, the above raw materials were placed in an agate ball mill jar with a ball-to-material ratio of 1:20.

[0048] S3: The agate ball mill jar was dry-milled for 12 hours in a planetary ball mill at a speed of 300 r / min.

[0049] S4: After the ball milling, the product was washed with absolute ethanol and deionized water, and dried in a vacuum oven at 80°C for 36 hours to obtain Na x Fe[Fe(CN) 6 .

[0050] figure 1 Be the XRD diffraction pattern of unwashed product after the ball milling of present embodiment example, by and Na 4 Fe(CN) 6 Standard PDF card comparison (JCPDS-1-1026), it can be seen that the unwashed product after ball milling does not contain Na 4 Fe(CN) 6 , which shows that the ball milling reaction is complete. figure 2 Fo...

Embodiment 2

[0053] S1: Put 4mmol of anhydrous sodium ferrocyanide and 4mmol of anhydrous manganous chloride in a nylon ball mill jar, vibrate and mix at a rate of 800r / min for 1min.

[0054] S2: Add 20ml of acetonitrile into the ball mill jar.

[0055] S3: Continue vibrating ball milling on a vibrating ball mill for 30 min at a vibration rate of 1200 r / min.

[0056] S4: After ball milling, filter the product, wash with absolute ethanol, and bake in a vacuum oven at 80°C for 36 hours to obtain Na x Mn[Fe(CN) 6 .

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
particle sizeaaaaaaaaaa
sizeaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of ultrafine iron-based Prussian blue and its analogues, comprising the following steps: S1: adding sodium ferrocyanide and metal salts into a ball milling device; S2: adding sodium ferrocyanide and metal salts into the ball milling device An appropriate amount of solvent; S3: put the mixed raw materials in the ball milling device for ball milling; S4: wash the mixture obtained in step S3 with absolute ethanol and deionized water; S5: dry the cleaned product to prepare Iron-based Prussian blue and its analogues. The invention also discloses its corresponding iron-based Prussian blue and its analogs and sodium ion battery. The preparation method of ultrafine iron-based Prussian blue and its analogs of the present invention adopts a solid-to-liquid ratio greater than 50%, and promotes the reaction through ball milling. Therefore, the method has high yield and is suitable for large-scale production, and the ultrafine iron-based Prussian blue and its analogues have a particle size of less than 100nm and are used as cathode materials for sodium-ion batteries. They have the characteristics of long cycle life and good rate performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of Prussian blue and its analogues, and more specifically relates to a preparation method of ultrafine iron-based Prussian blue and its analogues and their application in anode materials for sodium ion batteries. Background technique [0002] Na-ion batteries have the characteristics of low raw material cost, abundant resources, and great electrochemical performance potential, so they are expected to be applied in the field of large-scale energy storage, and are one of the important research directions of next-generation battery technology. At present, the cathode materials of sodium-ion batteries mainly include transition metal oxides, phosphates, and Prussian blue materials. Among them, Prussian blue materials have higher voltage platform (>3V), large ion channels, and large specific capacity (~170mAh g -1 ), cheap, non-toxic and easy to prepare, and become a research hotspot of cathode ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M10/054B82Y30/00
CPCB82Y30/00H01M4/362H01M4/58H01M10/054Y02E60/10
Inventor 张五星龚文哲薛丽红黄云辉
Owner 张五星