A carbon-based composite ferric cyanamide material and its preparation method and sodium-ion battery using it as negative electrode material

Abstract

The invention discloses a preparation method of a carbon-based composite iron cyanamide material. Firstly, ferric amine oxalate, urea and conductive carbon are respectively taken according to a mass ratio of 1:2:(0.1-1), fully ground and mixed to obtain a uniform mixture powder solid, the product is marked as A; add a surfactant to product A, dissolve it in water and then disperse, and the black product obtained after freeze-drying is marked as B; pyrolyze product B under a protective atmosphere to obtain product C, namely carbon Based composite ferric cyanamide material; Gained carbon-based composite ferric cyanamide material is used as the negative electrode material of sodium ion battery; The present invention adopts the method for pyrolysis nitriding of FeCN 2 Compositing with conductive carbon, the synthetic product carbon-coated iron cyanamide active material is used as the negative electrode material of the sodium ion battery. By adding conductive carbon material, a new material system is constructed, which is beneficial to enhance the conductivity of the material. The preparation method operates Simple, low cost, safe and non-toxic, it is expected to realize industrial production.

Description

technical field

[0001] The invention belongs to the technical field of electrochemical materials, in particular to a carbon-based composite iron cyanamide material and a preparation method thereof, and also relates to a sodium ion battery using the material. Background technique

[0002] In recent years, due to the increasingly urgent demand for large-scale energy storage technology due to the utilization of renewable energy, resource-cheap sodium-ion batteries have received extensive attention from the scientific and industrial circles. However, due to the large size of sodium ions (DNa+=0.106nm, DLi+=0.076nm), it is difficult to directly intercalate into the electrode materials of many sodium-ion batteries to realize the electrochemical sodium storage process, which greatly limits the application prospects of such batteries. . Therefore, how to take into account the charge-discharge rate and sodium storage capacity of electrode materials for sodium-ion batteries has becom...

Examples

Embodiment 1

[0022] Adopt the following steps to prepare carbon-based composite iron cyanamide material:

[0023] 1) Take 1 g of analytically pure feroxamine oxalate, 2 g of urea and 0.1 g of CNT according to the mass ratio of 1:2:0.1, and place them in a glass mortar to fully grind to obtain a fine and uniform pale green mixture powder. The product is recorded as A;

[0024] 2) Add 0.02 g of EDTA to product A, dissolve it in water and then ultrasonically disperse it for 10 minutes, then put it into a freeze dryer, and dry it at -50°C for 12 hours to obtain a completely dried black product, denoted as B;

[0025] 3) The product B was placed in a ceramic crucible, placed in a tube furnace, pyrolyzed in an argon atmosphere, heated from room temperature to 160°C at a rate of 30°C / min, kept for 1 h, and then continued at 5°C The heating rate of / min continued to keep the temperature up to 400°C, and the obtained product was the carbon-based composite iron cyanamide material.

[0026] The obt...

Embodiment 2

[0028] Prepare carbon-based composite iron cyanamide material according to the following steps:

[0029] 1) respectively take analytically pure feroxamine oxalate 1.5g, urea 3g and graphene 0.45g in a mass ratio of 1:2:0.3, place in a glass mortar and fully grind to obtain a fine and uniform pale green mixture powder, the product denoted as A;

[0030] 2) Add 0.045g of ethanolamine to product A, dissolve it in water and then ultrasonically disperse it for 30min, then put it into a freeze dryer, and dry it at -50°C for 16h to obtain a completely dried black product and denote it as B;

[0031] 3) The product B was placed in a ceramic crucible, placed in a tube furnace, pyrolyzed in an argon atmosphere, heated from room temperature to 160°C at a rate of 30°C / min, kept for 1 hour, and then continued at 6°C The heating rate of / min continued to keep the temperature up to 600°C, and the obtained product was the carbon-based composite iron cyanamide material.

[0032] The obtained...

Embodiment 3

[0034] Prepare carbon-based composite iron cyanamide material according to the following steps:

[0035] 1) Take 2 g of analytically pure feroxamine oxalate, 4 g of urea and 0.12 g of super-p respectively in a mass ratio of 1:2:0.6, and place them in a glass mortar to fully grind and mix to obtain a fine and uniform pale green mixture powder, The product is denoted as A;

[0036] 2) Add 0.08 g of oleic acid to product A, dissolve it in water, and then ultrasonically disperse it for 60 minutes, then put it into a freeze dryer, and dry it at -50°C for 18 hours to obtain a completely dried black product, denoted as B;

[0037] 3) The product B was placed in a ceramic crucible, and put into a tube furnace together, pyrolyzed in an argon atmosphere, heated from room temperature to 160 °C at a rate of 30 °C / min, and kept for 1 h, and then continued to heat for 8 The temperature rising rate of ℃ / min continued to keep heating up to 600 ℃, and the obtained product was the carbon-based...

technical field

[0001] The invention belongs to the technical field of electrochemical materials, in particular to a carbon-based composite iron cyanamide material and a preparation method thereof, and also relates to a sodium ion battery using the material. Background technique

[0002] In recent years, due to the increasingly urgent demand for large-scale energy storage technology due to the utilization of renewable energy, resource-cheap sodium-ion batteries have received extensive attention from the scientific and industrial circles. However, due to the large size of sodium ions (DNa+=0.106nm, DLi+=0.076nm), it is difficult to directly intercalate into the electrode materials of many sodium-ion batteries to realize the electrochemical sodium storage process, which greatly limits the application prospects of such batteries. . Therefore, how to take into account the charge-discharge rate and sodium storage capacity of electrode materials for sodium-ion batteries has becom...

Examples

Embodiment 1

[0022] Adopt the following steps to prepare carbon-based composite iron cyanamide material:

[0023] 1) Take 1 g of analytically pure feroxamine oxalate, 2 g of urea and 0.1 g of CNT according to the mass ratio of 1:2:0.1, and place them in a glass mortar to fully grind to obtain a fine and uniform pale green mixture powder. The product is recorded as A;

[0024] 2) Add 0.02 g of EDTA to product A, dissolve it in water and then ultrasonically disperse it for 10 minutes, then put it into a freeze dryer, and dry it at -50°C for 12 hours to obtain a completely dried black product, denoted as B;

[0025] 3) The product B was placed in a ceramic crucible, placed in a tube furnace, pyrolyzed in an argon atmosphere, heated from room temperature to 160°C at a rate of 30°C / min, kept for 1 h, and then continued at 5°C The heating rate of / min continued to keep the temperature up to 400°C, and the obtained product was the carbon-based composite iron cyanamide material.

[0026] The obt...

Embodiment 2

[0028] Prepare carbon-based composite iron cyanamide material according to the following steps:

[0029] 1) respectively take analytically pure feroxamine oxalate 1.5g, urea 3g and graphene 0.45g in a mass ratio of 1:2:0.3, place in a glass mortar and fully grind to obtain a fine and uniform pale green mixture powder, the product denoted as A;

[0030] 2) Add 0.045g of ethanolamine to product A, dissolve it in water and then ultrasonically disperse it for 30min, then put it into a freeze dryer, and dry it at -50°C for 16h to obtain a completely dried black product and denote it as B;

[0031] 3) The product B was placed in a ceramic crucible, placed in a tube furnace, pyrolyzed in an argon atmosphere, heated from room temperature to 160°C at a rate of 30°C / min, kept for 1 hour, and then continued at 6°C The heating rate of / min continued to keep the temperature up to 600°C, and the obtained product was the carbon-based composite iron cyanamide material.

[0032] The obtained...

Embodiment 3

[0034] Prepare carbon-based composite iron cyanamide material according to the following steps:

[0035] 1) Take 2 g of analytically pure feroxamine oxalate, 4 g of urea and 0.12 g of super-p respectively in a mass ratio of 1:2:0.6, and place them in a glass mortar to fully grind and mix to obtain a fine and uniform pale green mixture powder, The product is denoted as A;

[0036] 2) Add 0.08 g of oleic acid to product A, dissolve it in water, and then ultrasonically disperse it for 60 minutes, then put it into a freeze dryer, and dry it at -50°C for 18 hours to obtain a completely dried black product, denoted as B;

[0037] 3) The product B was placed in a ceramic crucible, and put into a tube furnace together, pyrolyzed in an argon atmosphere, heated from room temperature to 160 °C at a rate of 30 °C / min, and kept for 1 h, and then continued to heat for 8 The temperature rising rate of ℃ / min continued to keep heating up to 600 ℃, and the obtained product was the carbon-based...

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