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A kind of preparation method of leaf-shaped nh4v3o8 microcrystal

A leaf-shaped, microcrystalline technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of long process cycle and achieve the effects of simple preparation process, controllable morphology and short reaction cycle

Active Publication Date: 2014-10-29
杨洁如
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] These methods have a long process cycle, the general reaction time is between 24 and 96 hours, and the morphology and particle size uniformity of the prepared product need to be improved.

Method used

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  • A kind of preparation method of leaf-shaped nh4v3o8 microcrystal
  • A kind of preparation method of leaf-shaped nh4v3o8 microcrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) will analyze pure NH 4 VO 3 Dissolved in deionized water with stirring and sonication, formulated as NH 4 + Light yellow transparent NH with a concentration of 0.30mol / L 4 VO 3 Solution, denoted as A solution;

[0023] 2) Dissolve EDTA in deionized water to prepare a solution with an EDTA concentration of 0.10mol / L, which is designated as solution B;

[0024] 3) Mix solution A and solution B according to the volume ratio of 1:0.3, and stir at room temperature for 3 hours to obtain solution C;

[0025] 4) Adjust the pH of solution C to 3.0 with hydrochloric acid, and then sonicate solution C for 1 hour at an ultrasonic power of 300W;

[0026] 5) Transfer the ultrasonically treated C solution into a polytetrafluoroethylene-lined reactor, control the volume filling ratio of the reactor to 60%, and then place the reactor with C solution in a microwave hydrothermal instrument, React at 200°C for 30 minutes;

[0027] 6) After the reaction is completed and cooled to r...

Embodiment 2

[0031] 1) will analyze pure NH 4 VO 3 Dissolved in deionized water with stirring and sonication, formulated as NH 4 + Light yellow transparent NH with a concentration of 0.20mol / L 4 VO 3 Solution, denoted as A solution;

[0032] 2) Dissolve EDTA in deionized water to prepare an EDTA solution with an EDTA concentration of 0.05mol / L, solution B;

[0033] 3) Mix solution A and solution B according to the volume ratio of 1:0.5, and stir at room temperature for 4 hours to obtain solution C;

[0034] 4) Adjust the pH of solution C to 2.5 with hydrochloric acid, and then sonicate solution C for 1 hour at 400W ultrasonic power;

[0035] 5) Transfer the ultrasonically treated C solution into a polytetrafluoroethylene-lined reactor, control the volume filling ratio of the reactor to 70%, and then place the reactor with C solution in a microwave hydrothermal instrument, React at 180°C for 40 minutes;

[0036] 6) After the reaction is completed and cooled to room temperature, the ...

Embodiment 3

[0038] 1) will analyze pure NH 4 VO 3 Dissolved in deionized water with stirring and sonication, formulated as NH 4 + Light yellow transparent NH with a concentration of 0.50mol / L 4 VO 3 Solution, denoted as A solution;

[0039] 2) Dissolve EDTA in deionized water to prepare an EDTA solution with an EDTA concentration of 0.20mol / L, which is denoted as B solution;

[0040] 3) Mix solution A and solution B according to the volume ratio of 1:0.6, and stir at room temperature for 5 hours to obtain solution C;

[0041] 4) Adjust the pH of solution C to 2.0 with hydrochloric acid, and then sonicate solution C at 400W ultrasonic power for 1 hour;

[0042] 5) Transfer the ultrasonically treated C solution into a polytetrafluoroethylene-lined reactor, control the volume filling ratio of the reactor to 80%, and then place the reactor with C solution in a microwave hydrothermal instrument, React at 160°C for 60 minutes;

[0043] 6) After the reaction is completed and cooled to ro...

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Abstract

The invention provides a leaf-type NH4V3O8 microcrystalline preparation method which is easy to operate in process, short in reaction cycle, uniform in powder chemical constitution, regular and uniform in crystal morphology and even in powder particle size. The method comprises that firstly, a NH4V3O8 solution with the NH4+concentration of 0.10-0.50 mol / L, which is marked the solution A, is prepared; secondly, an ethylene diamine tetraacetic acid solution with the concentration of 0.05-0.20mol / L, which is marked the solution B is prepared; the solution A and the solution B are mixed according to the volume ratio of 1: 0.3-0.6 and are mixed at the room temperature to obtain a solution C; the pH value of the solution C is adjusted to 1.5-3.5 by using hydrochloric acid, and then ultrasonic processing is conducted; the solution C is switched to a reaction still and placed in a microwave hydrothermal device, and reaction is conducted for 30-60 min at the tempaertaure of 140-200 DEG C; the mixture is cooled to the room temperature after the reaction, and filtering is performed to obtain a solid product; and finally, the solid product is immersed and washed repeatedly by using absolute ethyl alcohol, and the solid product is dried at the temperature of 80-120 DEG C for 3-5 hours to obtain the leaf-type NH4V3O8 microcrystalline.

Description

technical field [0001] The invention relates to a preparation method that can be used as a lithium ion battery material and a sensor material powder, in particular to a leaf-shaped NH 4 V 3 o 8 Method for the preparation of microcrystals. Background technique [0002] Vanadium is a multivalent metal element (+2 to +5 valence) among transition elements and has very active chemical behavior. Vanadium has three stable oxidation states (V 3+ , V 4+ , V 5+ ), the oxygen atoms in the oxide are distributed in close-packed volumes. Vanadium can form a variety of oxides with oxygen, and can also form composite oxides with other cations and oxygen atoms. They generally have the ability to intercalate lithium and can be used as anode materials for lithium-ion batteries. NH 4 V 3 o 8 with LiV 3 o 8 Lithium-ion battery cathode materials have the same layered structure, all of which belong to the monoclinic P2 1 / m space group, in NH 4 V 3 o 8 structure, V 3 o 8 - Layer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00
CPCY02E60/10
Inventor 黄剑锋孟岩曹丽云王敦强张志清朱佳
Owner 杨洁如
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