Preparation method of nitrogen-doped carbon composite transition metal carbodiimide

A carbodiimide and transition metal technology, which is applied in the field of preparation of nitrogen-doped carbon composite transition metal carbodiimide materials, can solve the problems of high synthesis cost and complex synthesis steps, and achieves reduced preparation cost and simple preparation method. , the effect of improving electrical conductivity and structural stability

Active Publication Date: 2018-08-10
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
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Problems solved by technology

[0003] The present invention aims at the problems of complex synthesis steps and high synthesis cost of transition metal carbodiimide materials in the prior art, and aims at proposing a preparation method of nitrogen-doped carbon composite transition metal carbodiimide materials, through carbon coating It can effectively solve the volume expansion of transition metal carbodiimide, study the influence of the material structure on the electrochemical sodium storage process, establish the structure-effect mechanism of the material in the sodium storage process, and provide a basis for expanding the negative electrode material system and performance of sodium ion batteries. Improve the reference

Method used

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  • Preparation method of nitrogen-doped carbon composite transition metal carbodiimide
  • Preparation method of nitrogen-doped carbon composite transition metal carbodiimide
  • Preparation method of nitrogen-doped carbon composite transition metal carbodiimide

Examples

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Embodiment 1

[0031] 1) Fully grind analytically pure ferric citrate, ferric chloride and urea in a glass mortar to form a mixture A, wherein the ferric citrate is 2.0 g, the ferric chloride is 2.0 g, and the urea is 2.0 g;

[0032] 2) Transfer the mixture A from the mortar to a quartz crucible, place the quartz crucible in a tube furnace, and raise the temperature at a rate of 30°C / min to 170°C, and keep it warm for 50min, and then continue to raise the temperature to 600°C at a rate of 4°C / min under the argon flow rate of 200mL / min, and keep it warm for 45min to obtain product B.

[0033] Adopt Japanese Rigaku D / max2000PCX-ray diffractometer to analyze product B, the XRD of the product obtained is shown in the appendix figure 1 . The sample was observed under scanning electron microscope and transmission electron microscope, from figure 2 and image 3 It can be seen from the figure that the product presents a shell-like structure, and the surface of the structure has more polyhedral s...

Embodiment 2

[0036] 1) Fully grind analytically pure cobalt oxalate, cobalt nitrate and thiocyanic acid in a glass mortar to form a mixture A, wherein 1 g of cobalt oxalate, 1 g of cobalt nitrate, and 2 g of thiocyanic acid;

[0037] 2) Transfer A from the mortar to a quartz crucible, place the quartz crucible in a tube furnace, and raise the temperature to 180 °C at a rate of 20 °C / min under an argon atmosphere at a flow rate of 750 mL / min ℃, and keep it warm for 8 minutes, and then continue to raise the temperature to 500 ℃ at a rate of 3 ℃ / min under the argon flow rate of 50mL / min, and keep it warm for 50 minutes, and the obtained product is marked as B.

[0038] Adopt Japanese Rigaku D / max2000PCX-ray diffractometer to analyze product B, the XRD of the product obtained is shown in the appendix Figure 5 . The sample was observed under scanning electron microscope and transmission electron microscope, from Image 6 and Figure 7 It can be seen that the product presents a stacked polyh...

Embodiment 3

[0040]1) Fully grind the inorganic transition metal salt and the carbon-nitrogen-containing organic compound in a glass mortar to obtain a mixture, and the mass ratio of the inorganic transition metal salt to the carbon-nitrogen-containing organic compound in the mixture is 4:1; wherein, the inorganic transition metal The salt is a mixture of ferric citrate and ferric nitrate. Carbon and nitrogen-containing organic compounds are biurets.

[0041] 2) Transfer the mixture from the mortar to a quartz crucible, place the quartz crucible in a tube furnace, and raise the temperature from room temperature at a rate of 5°C / min under an argon atmosphere with an argon flow rate of 1000mL / min To 200°C and keep it warm for 10min, then continue to raise the temperature to 700°C at a rate of 5°C / min under the argon flow rate of 100mL / min and keep it warm for 30min to obtain a nitrogen-doped carbon composite transition metal carbodiimide material.

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Abstract

Disclosed is a preparation method of a nitrogen-doped carbon composite transition metal carbodiimide material. The method comprises the steps of: grinding an inorganic transition metal salt and a carbon and nitrogen containing organic compound to obtain a mixture, the mass ratio of the inorganic transition metal salt to the carbon and nitrogen containing organic compound in the mixture being 4:1-1:7; holding the mixture in an argon atmosphere at 140-200 DEG C for 10-50 min, and then holding at 300-700 DEG C for 30 min to 4h to obtain the nitrogen-doped carbon composite transition metal carbodiimide material. By compounding the prepared transition metal material structure with a nitrogen-doped carbon material, the conductivity and structural stability of the material during charge and discharge can be significantly improved. The nitrogen-doped carbon composite transition metal carbodiimide material prepared by the method has extremely high sodium ion storage performance, high charge anddischarge capacity and excellent rate performance.

Description

technical field [0001] The invention belongs to the field of composite material synthesis, and in particular relates to a preparation method of a nitrogen-doped carbon composite transition metal carbodiimide material. Background technique [0002] Due to the advantages of high energy density, long service life, and environmental friendliness, lithium-ion batteries have become a research hotspot in recent years and have been successfully commercialized. However, the reserves of lithium resources in the earth are relatively low, and the high price has become a bottleneck for the continued development of lithium-ion batteries. Because there is an urgent need to find an element with abundant reserves and similar properties to replace lithium. Sodium and lithium are elements of the same main group, and sodium reserves are relatively high on the earth and widely distributed. Therefore, a large number of scientific researchers have invested a lot of energy in the research of sodi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/60H01M4/62H01M10/054
CPCH01M4/362H01M4/60H01M4/62H01M4/625H01M4/628H01M10/054Y02E60/10
Inventor 李嘉胤王芳敏齐慧郭鹏辉黄剑锋郭玲党欢何枢薇
Owner SHAANXI UNIV OF SCI & TECH
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