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Nitrogen and phosphorus co-doped carbon coated MoO3-x and preparation method thereof

A co-doping, carbon-coated technology, applied in active material electrodes, electrical components, electrochemical generators, etc., can solve the problem that electrospinning cannot be mass-produced, the preparation of spinning slurry is complicated, and the electrochemical stability is insufficient. problems, to achieve the effect of loose experimental conditions, improved purity, and low cost

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

Chinese patent CN 102623687A discloses a method for preparing a high-capacity molybdenum dioxide negative electrode material and its application. The method uses a combination of electrospinning and heat treatment to prepare molybdenum dioxide. The product has a high specific capacity, but electrospinning It cannot be mass-produced, the preparation of spinning slurry is relatively complicated, and there are certain shortcomings in electrochemical stability

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  • Nitrogen and phosphorus co-doped carbon coated MoO3-x and preparation method thereof
  • Nitrogen and phosphorus co-doped carbon coated MoO3-x and preparation method thereof
  • Nitrogen and phosphorus co-doped carbon coated MoO3-x and preparation method thereof

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preparation example Construction

[0025] The invention relates to a nitrogen-phosphorus co-doped carbon-coated MoO 3-x The preparation method comprises the following steps:

[0026] (1) Add phosphomolybdic acid to deionized water, and stir evenly to obtain a phosphomolybdic acid solution with a concentration of 1 to 2.5 mg / ml;

[0027] (2) Add N-methylimidazole to the phosphomolybdic acid solution, the molar ratio of the added N-methylimidazole to step (1) phosphomolybdic acid is 3:1, stir for 7-12h, and obtain a yellow precipitate;

[0028] (3) After the yellow precipitate of step (2) is centrifuged to obtain the separated product, the separated product is washed 3-5 times to remove impurities with a mixed solution of hexanaphthene and ethanol, and the reaction product is obtained, wherein the mixture of hexanaphthene and ethanol is The volume ratio is (2-5):1.

[0029] (4) Vacuum drying the reaction product obtained in step (3) for 7-10 hours at a drying temperature of 40-70° C. to obtain a dry product.

...

Embodiment 1

[0033] 1) Add 100 mg of phosphomolybdic acid to 40 mL of deionized water, and stir evenly to obtain a phosphomolybdic acid solution with a concentration of 2.5 mg / mL;

[0034] 2) Add 12.4 mg of N-methylimidazole to the phosphomolybdic acid solution, stir for 7 hours, and obtain a yellow precipitate;

[0035] 3) centrifuging the yellow precipitate to obtain a centrifuged product, washing the centrifuged product 3 times with a mixed solution of cyclohexane and ethanol to remove impurities, and obtaining a reaction product; wherein the volume ratio of cyclohexane and ethanol is 3:1;

[0036] 4) vacuum drying the reaction product obtained in step 3) at 50° C. for 7 hours to obtain a dried product;

[0037] 5) Calcining the dried product of step 4) in an argon atmosphere for 2 hours at a calcination temperature of 400°C to obtain nitrogen and phosphorus co-doped carbon-coated MoO 3-x nanomaterials.

[0038] Nitrogen and phosphorus co-doped carbon-coated MoO prepared by the data o...

Embodiment 2

[0040] 1) Add 100 mg of phosphomolybdic acid to 50 mL of deionized water, and stir evenly to obtain a phosphomolybdic acid solution with a concentration of 2 mg / mL;

[0041] 2) Add 12.4 mg of N-methylimidazole to the phosphomolybdic acid solution, stir for 12 hours, and obtain a yellow precipitate;

[0042] 3) centrifuging the yellow precipitate to obtain a centrifuged product, washing the centrifuged product 5 times with a mixed solution of cyclohexane and ethanol to remove impurities, and obtaining a reaction product; wherein the volume ratio of cyclohexane and ethanol is 3:1;

[0043] 4) vacuum drying the reaction product obtained in step 3) at 50° C. for 8 hours to obtain a dry product;

[0044] 5) Calcining the dried product of step 4) in an argon atmosphere for 2 hours at a calcination temperature of 400°C to obtain nitrogen and phosphorus co-doped carbon-coated MoO 3-x nanomaterials.

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Abstract

The invention discloses nitrogen and phosphorus co-doped carbon coated MoO3-x and a preparation method thereof. Phosphomolybdic acid and N-methyl imidazole serve as raw materials, a yellow precipitateis prepared through precipitation in the preparation process, and impurities in the process products are washed with a mixed solution of cyclohexane and ethanol, so the purity of the reaction products is improved; a nitrogen and phosphorus co-doped carbon coated MoO3-x composite material is prepared by a calcining method; and the whole preparation process is simple in technology, loose in experimental condition, low in cost and suitable for large-scale production. The nitrogen and phosphorus co-doped carbon coated MoO3-x composite material is molybdenum trioxide containing oxygen vacancy, theoxygen vacancy serves as a shallow donor and the density of current carriers can be increased, so that the electrical conductivity of the material can be improved. According to discovery from that the nitrogen and phosphorus co-doped carbon coated MoO3-x composite material is subjected to charge and discharge capacity test under 100 mA / g, the specific discharge capacity and the specific charge capacity are 1077 mAh g<-1> and 787 mAh g<-1>, and the prepared composite material has excellent electrochemical activity.

Description

【Technical field】 [0001] The invention belongs to the field of preparation of inorganic nanomaterials, in particular to a nitrogen-phosphorus co-doped carbon-coated MoO 3-x and its preparation method. 【Background technique】 [0002] In recent years, the excessive use of fossil energy has brought many environmental problems, and the development and use of new sustainable clean energy is an inevitable trend of my country's development. However, there are certain technical obstacles in the storage and output of these clean energy sources. Therefore, the development of energy storage devices with excellent performance is the focus of many researchers. Among them, lithium-ion batteries are currently the most widely studied energy storage devices. Anode materials are an important part of lithium-ion batteries. The anode materials for commercial lithium-ion batteries are mainly graphite, but the theoretical specific capacity of graphite is low (372mAh / g), which restricts the real...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/48H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/48H01M4/625H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 张利锋神克超贺文杰刘毅郭守武
Owner SHAANXI UNIV OF SCI & TECH
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