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Method for preparing tritin tetraphosphide rivets for sodium ion negative electrode materials in carbon skeleton composite materials

A negative electrode material and composite material technology, applied in the field of inorganic nanomaterial synthesis, can solve the problems of difficult product morphology, volume change, and difficult phase, and achieve the effects of improving cycle stability, buffering volume expansion, and good conductivity

Active Publication Date: 2021-11-23
TIANJIN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The main problem is that the phase is difficult to synthesize. The current synthesis methods include high-speed ball milling, hydrothermal reaction, low-temperature phosphating, etc. The high-speed ball milling method is simple and easy, but it is difficult to control the morphology of the product; hydrothermal reaction can synthesize many Sn 3 P 4 , but in the phosphating process, hydrazine hydrate is generally used as the reaction solvent, and a long-term solvothermal reaction at a higher temperature has certain risks; low-temperature phosphating generally uses sodium hydrogen hypophosphite as the phosphorus source. The precursor is phosphated, and this phosphating method has certain selectivity for the precursor
In addition, since the radius of the sodium ion is A larger ionic radius causes serious volume changes in the material during the energy storage process, resulting in structural damage to the material after multiple cycles, and the greater the current density, the more serious the damage to the material
Jun Liu (JunLiu, bc Peter Kopold, b Chao Wu, b Peter A. van Aken, b Joachim Maierb and Yan Yu) and others synthesized the Sn core-shell structure 3 P 4 / C, although the hollow core-shell structure alleviates the volume change of the material during the cycle, and the coating of the carbon layer enhances the conductivity of the material, but hydrazine hydrate is generally used as the reaction solvent, and the hydrothermal reaction is carried out at 200 °C for a long time. Many potential safety hazards, so looking for a safe and reliable method to prepare high-capacity Sn 3 P 4 Materials are of great significance for the application of large-scale anode materials

Method used

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  • Method for preparing tritin tetraphosphide rivets for sodium ion negative electrode materials in carbon skeleton composite materials
  • Method for preparing tritin tetraphosphide rivets for sodium ion negative electrode materials in carbon skeleton composite materials
  • Method for preparing tritin tetraphosphide rivets for sodium ion negative electrode materials in carbon skeleton composite materials

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Experimental program
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Effect test

Embodiment 1

[0026] 1). SnCl 4 ·5H 2 O was dispersed into deionized water, and stirred at a speed of 200r / min for 30min to form a uniformly dispersed solution with a molar concentration of 0.5mol / L;

[0027] 2). Add sodium citrate to step 1), stir at 200r / min for 30min, the molar concentration of sodium citrate is 0.5mol / L to form a mixed white suspension; Freeze-dried for 24 hours to obtain a white solid;

[0028] 3). The product obtained in step 2) is carbonized in a tube furnace with Ar gas as the protective gas, and the temperature is raised to 700°C at a heating rate of 2°C / min, kept for 3h, and cooled with the furnace;

[0029] 4). The product obtained in step 3) and sodium hydrogen hypophosphite are respectively placed on both sides of the same quartz boat, wherein the amount of sodium hydrogen hypophosphite added is 5 times the quality of the product obtained in step 3), and then covered Quartz slices were phosphated under the condition of argon as a protective gas, raised to 300°...

Embodiment 2

[0032] 1). SnCl 4 ·5H 2 O was dispersed into deionized water, and stirred at a speed of 300r / min for 40min to form a uniformly dispersed solution with a molar concentration of 1.0mol / L;

[0033] 2). Add sodium citrate to step 1), stir at 300r / min for 40min, the molar concentration of sodium citrate is 1.0mol / L to form a mixed white suspension; Freeze-dried for 36 hours to obtain a white solid;

[0034] 3). The product obtained in step 2) is carbonized in a tube furnace with Ar gas as the protective gas, raised to 750°C at a heating rate of 5°C / min, kept for 4 hours, and cooled with the furnace;

[0035] 4). Place the product obtained in step 3) and sodium hydrogen hypophosphite on both sides of the same quartz boat, wherein the amount of sodium hydrogen hypophosphite added is 10 times the quality of the product obtained in step 3), and then cover Put the quartz plate on, carry out phosphating under the condition of argon as the protective gas, raise the temperature to 300°C...

Embodiment 3

[0038] 1). SnCl 4 ·5H 2 O was dispersed in deionized water, stirred at a speed of 400r / min for 50min to form a uniformly dispersed solution with a molar concentration of 1.5mol / L;

[0039] 2). Add sodium citrate to step 1), stir at 400r / min for 50min, the molar concentration of sodium citrate is 3.0mol / L to form a mixed white suspension; Freeze-dried for 48 hours to obtain a white solid;

[0040] 3). The product obtained in step 2) is carbonized in a tube furnace with Ar gas as the protective gas, raised to 800°C at a heating rate of 10°C / min, kept for 5 hours, and cooled with the furnace;

[0041] 4). Place the product obtained in step 3) and sodium hydrogen hypophosphite on both sides of the same quartz boat respectively, wherein the amount of sodium hydrogen hypophosphite added is 15 times the quality of the product obtained in step 3), and then cover Quartz slices were phosphated under the condition of argon as a protective gas, raised to 350°C at a heating rate of 5°C / ...

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Abstract

The invention provides a method for preparing a tritin tetraphosphide rivet used in a sodium ion negative electrode material in a carbon skeleton composite material, and the SnCl 4 ·5H 2 O was dispersed in deionized water and stirred, sodium citrate was added to the aqueous solution and stirred to form a mixed white suspension; the mixed white suspension was freeze-dried to obtain a white solid; Carry out carbonization treatment in a type furnace, and cool with the furnace; place the product and sodium hydrogen hypophosphite on both sides of the same quartz boat, and then cover with a quartz plate, and carry out phosphating under the condition of argon as a protective gas, using copper sulfate The solution is used to treat the waste gas, and the reactants are taken out, washed by centrifugation with absolute ethanol and deionized water, and dried in vacuum to obtain Sn 3 P 4 / C composite material. sn 4 P 3 The rivets are on the carbon skeleton, which improves the conductivity and prevents pulverization and falling off during the cycle, and is used as the negative electrode material of the sodium-ion battery.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanometer materials. Specifically, low-temperature phosphating of Sn / C is used to synthesize Sn 3 P 4 / C Composite. In particular, the invention relates to a method for preparing tritin tetraphosphide rivets on carbon skeleton composite materials for sodium ion negative electrode materials. Background technique [0002] In the industrial age, humans have carried out large-scale exploitation of fossil energy. Due to the low energy utilization rate, it has caused great waste of energy and environmental damage. Moreover, fossil energy is a one-time energy source. Unreasonable exploitation and use have caused energy pollution. Therefore, the development and use of green and renewable energy has become the development direction of the times, and energy storage materials have emerged as the times require. Since the end of the last century, lithium-ion batteries have been applied on a large scal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/054B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00H01M4/362H01M4/5805H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 孙晓红郭金泽郑春明
Owner TIANJIN UNIV