Preparation method of sandwiched-layer-shaped NH4V3O8 nanocrystalline

Abstract

The invention discloses a preparation method of a sandwiched-layer-shaped NH4V3O8 nanocrystalline. The preparation method of the sandwiched-layer-shaped NH4V3O8 nanocrystalline comprises the following steps: dissolving ammonium metavanadate into deionized water, thereby obtaining a NH4VO3 solution, and labeling as a solution A; adjusting the pH value of the solution A as 4.5-6.0, thereby obtaining a solution B; pouring the solution B into a reactor so as to enable microwaves to be functioned on the solution B, and warming to 60-90 DEG C and preserving heat at the microwave power of 400-600W; carrying out centrifugal separation on suspension in the reactor so as to obtain powder body products, then washing, and drying. The preparation method disclosed by the invention is simple in process, low in reaction temperature, short in reaction cycle without subsequent treatment, protects the environment, and can be suitable for large scale production. The NH4V3O8 nanocrystalline prepared by the preparation method disclosed by the invention is homogenous in chemical constitution, is relatively high in purity, is of special sandwiched-shaped morphology, is formed by automatically assembling thin sheets with the thicknesses of 30nm and nano particles among the sheets, and has favorable electrochemical performance as the lithium ion battery cathode material.

Description

technical field

[0001] The invention belongs to the field of battery material preparation, and in particular relates to a method for synthesizing interlayer NH by using microwave radiation technology. 4 V 3 o 8 nanocrystal approach. Background technique

[0002] Lithium-ion batteries have the advantages of high voltage, high energy density, long cycle life, good safety, and environmental protection. They have broad application prospects and are considered to be the energy storage materials with the most development potential in the market.

[0003] NH 4 V 3 o 8 It is a new type of lithium intercalation material, which has a layered structure and belongs to the monoclinic crystal system, P2 1 / m space group. in NH 4 V 3 o 8 structure, V 3 o 8 - Layers are tightly connected along the c-axis, NH 4 + It is between its layers, stabilizing its structure. NH with larger radius 4 + It can not only effectively increase the layer spacing of the material, provide cond...

Examples

Embodiment 1

[0025] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 50°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration is 0.01mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0026] 2) Use 1mol L -1 dilute hydrochloric acid solution to adjust the pH value of solution A to 6.0 to obtain B solution;

[0027] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, the temperature is measured by a platinum resistance, and the temperature is raised from room temperature to 90°C at a heating rate of 10°C / min, and then kept for 60min , and then naturally cooled to room temperature;

[0028]4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol for 10 minutes, wash 5 ...

Embodiment 2

[0031] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration is 0.03mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0032] 2) Use 2mol L -1 The dilute hydrochloric acid solution adjusts the pH value of solution A to be 5.50, obtains B solution;

[0033] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, and the temperature is measured by a platinum resistance, and the temperature is raised from room temperature to 80°C at a heating rate of 10°C / min, and then kept for 90min , and then naturally cooled to room temperature;

[0034] 4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol for 10 minute...

Embodiment 3

[0036] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred magnetically for 0.75h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration of 0.05mol / L NH 4 VO 3 Solution, denoted as A solution;

[0037] 2) Use 3mol L -1 dilute hydrochloric acid solution to adjust the pH value of solution A to 5.0 to obtain B solution;

[0038] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, and the platinum resistance is used to measure the temperature. After the temperature is raised from room temperature to 70°C at a heating rate of 10°C / min, the temperature is kept for 120min. , and then naturally cooled to room temperature;

[0039] 4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol ...

technical field

[0001] The invention belongs to the field of battery material preparation, and in particular relates to a method for synthesizing interlayer NH by using microwave radiation technology. 4 V 3 o 8 nanocrystal approach. Background technique

[0002] Lithium-ion batteries have the advantages of high voltage, high energy density, long cycle life, good safety, and environmental protection. They have broad application prospects and are considered to be the energy storage materials with the most development potential in the market.

[0003] NH 4 V 3 o 8 It is a new type of lithium intercalation material, which has a layered structure and belongs to the monoclinic crystal system, P2 1 / m space group. in NH 4 V 3 o 8 structure, V 3 o 8 - Layers are tightly connected along the c-axis, NH 4 + It is between its layers, stabilizing its structure. NH with larger radius 4 + It can not only effectively increase the layer spacing of the material, provide cond...

Examples

Embodiment 1

[0025] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 50°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration is 0.01mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0026] 2) Use 1mol L -1 dilute hydrochloric acid solution to adjust the pH value of solution A to 6.0 to obtain B solution;

[0027] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, the temperature is measured by a platinum resistance, and the temperature is raised from room temperature to 90°C at a heating rate of 10°C / min, and then kept for 60min , and then naturally cooled to room temperature;

[0028]4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol for 10 minutes, wash 5 ...

Embodiment 2

[0031] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration is 0.03mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0032] 2) Use 2mol L -1 The dilute hydrochloric acid solution adjusts the pH value of solution A to be 5.50, obtains B solution;

[0033] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, and the temperature is measured by a platinum resistance, and the temperature is raised from room temperature to 80°C at a heating rate of 10°C / min, and then kept for 90min , and then naturally cooled to room temperature;

[0034] 4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol for 10 minute...

Embodiment 3

[0036] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred magnetically for 0.75h to dissolve ammonium metavanadate evenly, and prepared NH 4 + The concentration of 0.05mol / L NH 4 VO 3 Solution, denoted as A solution;

[0037] 2) Use 3mol L -1 dilute hydrochloric acid solution to adjust the pH value of solution A to 5.0 to obtain B solution;

[0038] 3) Pour the B solution into the reactor, let the microwave act on the B solution, the microwave power is controlled at 400-600W, and the platinum resistance is used to measure the temperature. After the temperature is raised from room temperature to 70°C at a heating rate of 10°C / min, the temperature is kept for 120min. , and then naturally cooled to room temperature;

[0039] 4) Open the reactor, centrifuge the suspension in the reactor to obtain a powder product, soak the powder product in deionized water for 10 minutes, wash 5 times, then soak in absolute ethanol ...

Images