CN104466148B - A kind of H0.6moO3the preparation method and application of three-dimensional manometer superthin section - Google Patents

A kind of H0.6moO3the preparation method and application of three-dimensional manometer superthin section Download PDF

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CN104466148B
CN104466148B CN201410777190.8A CN201410777190A CN104466148B CN 104466148 B CN104466148 B CN 104466148B CN 201410777190 A CN201410777190 A CN 201410777190A CN 104466148 B CN104466148 B CN 104466148B
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moo
dimensional manometer
superthin section
lithium ion
ion battery
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CN104466148A (en
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王海
王林江
宋业萍
李字华
孙壮志
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Guilin University of Technology
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Guilin University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a kind of H0.6MoO3The preparation method and application of three-dimensional manometer superthin section.(1) 15 grams of analytical pure ammonium molybdates are dissolved in the 20 ml deionized water solution adding 0.2 0.6 grams of analytical pure ethylenediaminetetraacetic acid；(2) 0.1 0.5 grams of analytical pure cinnamic acid are added in step (1) gained mixed solvent, stir, move in 50 milliliters of reactors；(3) 180 220 DEG C of hydro-thermal reactions of products therefrom 14 24 hours, are then centrifuged for, and with absolute ethanol washing 36 times, dry, prepare H0.6MoO3Three-dimensional manometer superthin section.Gained H0.6MoO3Three-dimensional manometer superthin section is applied to assemble lithium ion battery.Preparation method of the present invention is simple, and with low cost, energy consumption is low, favorable reproducibility, and obtained lithium ion battery has high specific capacity and cyclical stability, and shows excellent multiplying power discharging property, has wide commercial application prospect.

Description

A kind of H0.6MoO3The preparation method and application of three-dimensional manometer superthin section
Technical field
The invention belongs to technical field of material chemistry, particularly to a kind of H0.6MoO3The preparation method of three-dimensional manometer superthin section.
Background technology
MoO3Big because of capacity as a kind of potential lithium ion battery electrode material, good rate capability and there is outstanding cyclical stability and by academia and the common concern of industrial quarters.The high temperature hydrogenation of material is processed particularly hydrogenation treatment to semi-conducting material and can substantially change the electronic structure of material, and and then improve the intrinsic conductivity of material.From the point of view of literature survey, to MoO3Hydrogenation treatment it has been reported that but in its method major part use containing virose raw material, and complicated process of preparation, cost is high.
The microstructure of superthin section uniqueness, because can effectively shorten the diffusion length of lithium ion battery, is very beneficial for the diffusion of lithium ion and becomes a big focus of materials synthesis in recent years.Can be in conjunction with the microstructure of this uniqueness of superthin section and be applied simultaneously to MoO3Hydrogenation treatment, is still a huge challenge at present.What it synthesized challenge is how select suitable raw material and use suitable method.From the point of view of current substantial amounts of document and patent are investigated, have not been reported.The present invention is directed to this bottleneck, invent a kind of H with three-dimensional manometer superthin section structure0.6MoO3Preparation method.
Summary of the invention
It is an object of the invention to provide a kind of technique simple, the H of low cost0.6MoO3Three-dimensional manometer superthin section and preparation method and application.The method is easy and simple to handle, low cost, power consumption are low, and the product purity obtained is high, can synthesize on a large scale.Obtained lithium ion battery has high specific capacity and cyclical stability, and shows excellent multiplying power discharging property, has wide commercial application prospect.
A kind of H0.6MoO3The preparation method of three-dimensional manometer superthin section, is to use hydro-thermal method to prepare a kind of H0.6MoO3Three-dimensional manometer superthin section.
H0.6MoO3The preparation method of three-dimensional manometer superthin section concretely comprises the following steps:
(1) 1-5 gram of analytical pure ammonium molybdate is dissolved in the 20 ml deionized water solution adding 0.2-0.6 gram of analytical pure ethylenediaminetetraacetic acid.
(2) 0.1-0.5 gram of analytical pure cinnamic acid is added in step (1) gained mixed solvent, stirs, move in 50 milliliters of reactors.
(3) 180-220 DEG C of hydro-thermal reaction 14-24 hour of step (2) products therefrom, is then centrifuged for, and with absolute ethanol washing 3-6 time, dries, prepares H0.6MoO3Three-dimensional manometer superthin section.
Described H0.6MoO3Three-dimensional manometer superthin section is applied to assemble lithium ion battery.Its assemble method is: by H0.6MoO3Three-dimensional manometer superthin section, Kynoar and acetylene black in mass ratio for 7:2:1 mixed grinding uniformly after be coated on copper mesh, to be dried as negative pole, using lithium metal as reference electrode with to electrode, by 1 mol/L LiClO4/ EC-DMC(1:1, volume ratio) solution is as electrolyte, and in glove box, described lithium ion battery is made in assembling.
The remarkable advantage of the present invention is:
(1) the invention provides a kind of H0.6MoO3The preparation method of three-dimensional manometer superthin section, the method is simple to operate, with low cost, and energy consumption is low, favorable reproducibility, has good using value.
(2) H prepared in the process of the present invention0.6MoO3Three-dimensional manometer superthin section, as the negative pole of lithium ion battery, assembles the lithium ion battery obtained and has high specific capacity and cyclical stability, and when electric current density is 100 mA/g, 100 capacity of charge and discharge cycles are stable at 387 mAh/g, show that its cyclical stability is good.
Accompanying drawing explanation
Fig. 1 is the H obtained by the embodiment of the present invention 10.6MoO3The scanning electron microscope (SEM) photograph of three-dimensional manometer superthin section.
Fig. 2 is the H obtained by the embodiment of the present invention 10.6MoO3The XRD figure of three-dimensional manometer superthin section.
Fig. 3 is that the present invention is by the H obtained by embodiment 10.6MoO3The lithium ion battery that three-dimensional manometer superthin section is assembled into is the cycle performance curve of discharge and recharge under different multiplying.
Detailed description of the invention
Embodiment 1:
A kind of H0.6MoO3The preparation method of three-dimensional manometer superthin section, comprises the following steps:
(1) 1 gram of analytical pure ammonium molybdate is dissolved in the 10 ml deionized water solution adding 0.2 gram of analytical pure ethylenediaminetetraacetic acid.
(2) 0.3 gram of analytical pure cinnamic acid is added in step (1) gained mixed solvent, stirs, move in reactor；
(3) reactor is put in 180 DEG C of baking ovens and react 14 hours, take out, naturally cool to room temperature, centrifugation product, with absolute ethanol washing 3 times, dry, prepare H0.6MoO3Three-dimensional manometer superthin section.
By gained H0.6MoO3Three-dimensional manometer superthin section is used for assembling lithium ion battery, and its assemble method includes: by H0.6MoO3Three-dimensional manometer superthin section, Kynoar and acetylene black in mass ratio for 7:2:1 mixed grinding uniformly after be coated on copper mesh, to be dried as negative pole, using lithium metal as reference electrode with to electrode, by 1 mol/L LiClO4/ EC-DMC(1:1, volume ratio) solution is as electrolyte, and in glove box, lithium ion battery is made in assembling.
Lithium ion battery charge and discharge cycles 100 times when electric current density is 100 mA/g that the present embodiment assembles, specific capacity is 387 mAh/g, shows that its cyclical stability is good.
Embodiment 2:
A kind of H0.6MoO3The preparation method of three-dimensional manometer superthin section, comprises the following steps:
(1) 5 grams of analytical pure ammonium molybdates are dissolved in the 20 ml deionized water solution adding 0.6 gram of analytical pure ethylenediaminetetraacetic acid.
(2) 0.3 gram of analytical pure cinnamic acid is added in step (1) gained mixed solvent, stirs, move in reactor.
(3) reactor is put in 200 DEG C of baking ovens and react 20 hours, take out, naturally cool to room temperature, centrifugation product, with absolute ethanol washing 6 times, dry, prepare H0.6MoO3Three-dimensional manometer superthin section.
By gained H0.6MoO3Three-dimensional manometer superthin section is used for assembling lithium ion battery, and its assemble method includes: by H0.6MoO3Three-dimensional manometer superthin section, Kynoar and acetylene black in mass ratio for 7:2:1 mixed grinding uniformly after be coated on copper mesh, to be dried as negative pole, using lithium metal as reference electrode with to electrode, by 1 mol/L LiClO4/ EC-DMC solution, as electrolyte, assembles in glove box and makes described lithium ion battery, and wherein the volume ratio of EC Yu DMC is 1:1.
Lithium ion battery charge and discharge cycles 100 times when electric current density is 100 mA/g that the present embodiment assembles, specific capacity is 387 mAh/g, shows that its cyclical stability is good.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.

Claims (2)

1. a H0.6MoO3The preparation method of three-dimensional manometer superthin section, it is characterised in that concretely comprise the following steps:
(1) 1-5 gram of analytical pure ammonium molybdate is dissolved in the 20 ml deionized water solution adding 0.2-0.6 gram of analytical pure ethylenediaminetetraacetic acid；
(2) 0.1-0.5 gram of analytical pure cinnamic acid is added in step (1) gained mixed solution, stirs, move in 50 milliliters of reactors；
(3) 180-220 DEG C of hydro-thermal reaction 14-24 hour of step (2) products therefrom, is then centrifuged for, and with absolute ethanol washing 3-6 time, dries, prepares H0.6MoO3Three-dimensional manometer superthin section.
H the most according to claim 10.6MoO3The H that the preparation method of three-dimensional manometer superthin section prepares0.6MoO3The application of three-dimensional manometer superthin section, it is characterised in that: H0.6MoO3Three-dimensional manometer superthin section is applied to assemble lithium ion battery；
The assemble method of described lithium ion battery is: by H0.6MoO3Three-dimensional manometer superthin section, Kynoar and acetylene black in mass ratio for 7:2:1 mixed grinding uniformly after be coated on copper mesh, to be dried as negative pole, using lithium metal as reference electrode with to electrode, by 1 mol/L LiClO4/ EC-DMC solution, as electrolyte, assembles in glove box and makes described lithium ion battery, and wherein the volume ratio of EC Yu DMC is 1:1.
CN201410777190.8A 2014-12-17 2014-12-17 A kind of H0.6moO3the preparation method and application of three-dimensional manometer superthin section Active CN104466148B (en)

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CN105152212B (en) * 2015-07-31 2016-09-28 桂林理工大学 A kind of H4.5mo5.25o18(H2o)1.36the preparation method and application of hexagonal columnar micron bar
CN105140478B (en) * 2015-07-31 2017-07-28 桂林理工大学 A kind of MoO3‑H0.4MoO3The preparation method of core-shell structure nanoribbon
CN107516737A (en) * 2017-08-08 2017-12-26 南陵县生产力促进中心 A kind of preparation method containing hydrionic molybdenum trioxide nano material for anode of lithium ion battery

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CN101723462A (en) * 2009-10-30 2010-06-09 陕西科技大学 Method for preparing fibrous MoO3 nanobelt
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