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Preparation method for nanoscale transition metal nitride/carbon composite material

A carbon composite material and transition metal technology, applied in the field of material science, can solve problems such as product inhomogeneity, and achieve the effect of improving specific capacity and conductivity

Active Publication Date: 2011-08-03
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN100368284C discloses a method for synthesizing nitrides using metal oxides, that is, after directly mixing cyanamide, dicyandiamide or melamine with transition metal oxides in the solid phase, they are placed in a reactor to evacuate and react at high temperature, although the process Simple, but the whole process is carried out in the solid phase, which may easily lead to inhomogeneous products

Method used

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  • Preparation method for nanoscale transition metal nitride/carbon composite material
  • Preparation method for nanoscale transition metal nitride/carbon composite material

Examples

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Effect test

Embodiment 1

[0024] Add 27mL of 37% (w / w) formaldehyde solution into a 150mL three-neck flask with a stirring and temperature-controlled water bath device, adjust the pH value to 7.5-8.5 with 10% sodium hydroxide solution, add 5g of urea, and heat up in the water bath After reacting at 90°C for 2 hours, add 2.5g of P123, adjust the pH to 5.0-5.4 with 5% dilute hydrochloric acid, continue the reaction for 30 minutes, cool and adjust the pH to 7.0-7.6, and filter to obtain a mixture of urea-formaldehyde resin and P123. Under the protection of argon, the temperature of the mixture was raised to 200° C. at a rate of 5° C., heat-treated for 2 hours, and then continued to be heated at a rate of 1-10° C. to 350° C., and heat-treated for 5 hours to obtain mesoporous carbon nitride.

[0025] 228mg Ti(OC 2 h 5 ) 4 and 606mg VO(OC 2 h 5 ) 3 Dissolve in 2g of ethanol, add 0.5g of mesoporous carbon nitride to it, treat the mixture with ultrasonic vibration for 10min, then remove the air in the por...

Embodiment 2

[0027] Add 37% formaldehyde aqueous solution, 38mL to the four-neck flask equipped with stirrer, thermometer, condenser and dropping funnel, adjust pH=8-9 with 20% sodium hydroxide aqueous solution. Add 10g of melamine, stir and raise the temperature to 85°C. After the melamine is completely dissolved, keep warm until precipitation occurs. Continue the reaction for 1 hour. After adding 5g of P123, adjust the pH to 5.0-5.4 with 5% dilute hydrochloric acid, and continue the reaction for half an hour. After suction filtration, the mixture of melamine resin and P123 was obtained. Under the protection of argon, the mixture was heated to 200°C at a rate of 5°C, heat-treated for 2 hours, and then continued to heat up to 350°C at a rate of 1-10°C , heat treatment for 5 hours to obtain mesoporous carbon nitride.

[0028] 834mg of Ti(OC 2 h 5 ) 4 Dissolve in 2g of ethanol, add 0.5g of mesoporous carbon nitride to it, treat the mixture with ultrasonic vibration for 10min, then remove ...

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Abstract

The invention relates to a preparation method for nanoscale transition metal nitride / carbon composite material, the chemical formula of nanoscale transition metal nitride / carbon composite material is MeN / C (Me is one or a mixture of more of organic compounds such as titanium, vanadium, chromium, nickel, manganese, molybdenum and the like; N and C are respectively nitrogen and carbon); the anoscale transition metal nitride / carbon composite material is obtained by the following methods: a tri-block copolymer P123 of PEO-PPO-PEO is taken as a template, the tri-block copolymer P123 and the urea resin, melamine resin or carbon nitride polymer are mixed and heated so as to obtain mesoporous carbon nitride, then the mesoporous carbon nitride is added into a metal organic compound or an ethanol solution of various mixtures of the metal organic compound, the removal of air in holes by decompression after ultrasonic vibration is carried out on the mixture, and finally the nanoscale transition metal nitride / carbon composite is obtained after the mixture undergoes ethanol pumping filtration, is scrubbed, dried and processed at high temperature under the protection of inert gas; and the product is uniform and is environmental friendly.

Description

technical field [0001] The invention belongs to the field of material science, and in particular relates to a preparation method of a nanoscale transition metal nitride / carbon composite material. Background technique [0002] Transition metal nitrides are a type of intermetallic compound formed by inserting element N into the transition metal lattice, which has the properties of covalent compounds, ionic crystals and transition metal species. Due to the insertion of element N, the metal lattice expands, the metal spacing and unit cell constant become larger, and the interaction force between metal atoms weakens, resulting in a corresponding d-band shrinkage modification and a redistribution of the density of states near the Fermi energy level, and the valence electrons As the number increases, the structure changes accordingly. This modulation gives compounds such as transition metal nitrides unique physical and chemical properties, and are widely used in supercapacitor ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00C01G23/00C01B21/076
Inventor 崔光磊韩鹏献刘志宏王海波赵新生董杉木
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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