CN103715407B - A kind of preparation method of loose structure ammonium vanadate material - Google Patents

A kind of preparation method of loose structure ammonium vanadate material Download PDF

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CN103715407B
CN103715407B CN201310700620.1A CN201310700620A CN103715407B CN 103715407 B CN103715407 B CN 103715407B CN 201310700620 A CN201310700620 A CN 201310700620A CN 103715407 B CN103715407 B CN 103715407B
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loose structure
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ammonium vanadate
vanadate material
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CN103715407A (en
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黄剑锋
曹杉杉
欧阳海波
曹丽云
费杰
李翠艳
吴建鹏
卢靖
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Yancheng hi tech Pioneer Park Co.,Ltd.
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Shaanxi University of Science and 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C01G31/02—Oxides
    • 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
    • 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

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Abstract

A preparation method for loose structure ammonium vanadate material, is dissolved in ammonium metavanadate in deionized water, obtains NH 4vO 3solution, is designated as solution A; Carry out phonochemical reaction after the pH value of solution A is adjusted to 1.5 ~ 3.0, obtain B solution; B solution is poured in reactor, make microwave and uviol lamp act on B solution simultaneously, be warmed up to 60 ~ 90 DEG C and be incubated, then naturally cooling to room temperature; Suspension centrifugation in reactor is obtained powder product, dry after washing, obtain loose structure ammonium vanadate material.The NH that the inventive method is obtained 4v 3o 8crystallite chemical composition is homogeneous, and purity is higher, is special loose structure, effectively can increases the specific area of material, as having good chemical property during anode material for lithium-ion batteries.Preparation method of the present invention is simple, and reaction temperature is low, and the reaction time is short, and without the need to subsequent treatment, environmentally friendly, can large-scale production be applicable to.

Description

A kind of preparation method of loose structure ammonium vanadate material
Technical field
The invention belongs to anode material for lithium-ion batteries preparation field, relate to a kind of preparation method of anode material for lithium-ion batteries, be specifically related to a kind of preparation method of loose structure ammonium vanadate material.
Background technology
Lithium ion battery has that voltage is high, energy density is large, have extended cycle life, fail safe is good and the advantage such as environmental protection, is with a wide range of applications, is considered to energy storage material market most with development potentiality.
NH 4v 3o 8be a kind of novel intercalation materials of li ions, it has layer structure, belongs to monoclinic system, P2 1/ m space group.At NH 4v 3o 8in structure, V 3o 8 -layer gets up along c-axis compact siro spinning technology, NH 4 +then be in its interlayer, stablize its structure.There is the NH of relatively large radius 4 +not only effectively can increase the interlamellar spacing of material, for the fast transport of lithium ion provides condition, can also intramolecular hydrogen bond be formed, the structure of stabilizing material, and then the cyclical stability that can improve material.Porous material specific area is comparatively large, when being used as lithium ion battery material, not only effectively can increasing the contact area of electrode material and electrolyte, can also promote lithium ion deintercalation, significantly can improve the chemical property of material.
Current preparation NH 4v 3o 8the method of material mainly contains the precipitation method and hydro thermal method.Heai-KuPark etc. are with V 2o 5be raw material with urea, the NH adopting the precipitation method to prepare diameter to be about 60nm 4v 3o 8nanometer rods.In the current density of 10mA/g and the voltage range of 1.8-4.0V, its initial discharge capacity can reach 210mAh/g [Heai-KuPark, GuntaeKin.Ammoniumhexavanadatenanorodspreparedbyhomogene ousprecipitationusingureaascathodesforlithiumbatteries [J] .SolidStateIonics, 2010,181:311-314.].HaiyanWang etc. take NH4VO3 as raw material, and using dodecyl sodium sulfate (SDS) as surfactant, 130 DEG C of hydrothermal treatment consists 48h, then 280 DEG C of heat treatment 4h in air atmosphere, have obtained the sheet NH that thickness is about 150nm 4v 3o 80.2H 2o, in the current density of 15mA/g and the voltage range of 1.8-4.0V, its initial discharge capacity is 225.9mAh/g, after 30 circulations, capacity remains on 209.4mAh/g [HaiyanWang, KelongHuang, SuqinLiu, etal.ElectrochemicalpropertyofNH 4v 3o 80.2H 2oflakespreparedbysurfactantassistedhydrothermalmethod [J] .JournalofPowerSource, 2011,196:788-792.].Han Yuanyuan etc. by by ammonium metavanadate acid solution at 180 DEG C of hydrothermal treatment consists 12h, obtained diameter and be about 100-150nm, reach the NH of some tens of pm 4v 3o 8nano wire [Han Yuanyuan, Zhu Weiqiong, Li Rong etc.NH 4v 3o 8the Hydrothermal Synthesis of nano wire and ultracapacitor performance [J]. application chemical industry, 2013,42 (1): 12-14.].
Above-mentioned precipitation method synthesis ammonium vanadate needs first to obtain gel, then reflux one week at 80 DEG C with the mixed liquor of urea, has that course of reaction is wayward, reaction time is grown, have the shortcomings such as side reaction generation, water heat transfer NH 4v 3o 8need surfactant, and there is the shortcoming that reaction temperature is relatively high, the reaction time is longer, so find a kind of synthesis NH that is simple, that fast, easily control 4v 3o 8method, the research and development of high performance lithium ion battery anode material is significant.
Summary of the invention
The object of the present invention is to provide the preparation method of the loose structure ammonium vanadate material that a kind of technological operation is simple, preparation temperature is low, reaction time is short, gained powder chemical composition is homogeneous, crystal morphology is regular.
In order to achieve the above object, the technical solution used in the present invention is:
1) analytically pure ammonium metavanadate is dissolved in deionized water, stirs and ammonium metavanadate is uniformly dissolved, obtain NH 4 +concentration be the NH of 0.03 ~ 0.10mol/L 4vO 3solution, is designated as solution A;
2) pH value of solution A is adjusted to after 1.5 ~ 3.0 under the ultrasonic power of 200 ~ 400W, carries out phonochemical reaction, obtain B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on B solution simultaneously, wherein the wavelength of uviol lamp is 365nm, the power of uviol lamp is 500W, microwave power is 400 ~ 600W, be incubated to 60 ~ 90 DEG C by room temperature with the heating rate of 15 DEG C/min, then naturally cool to room temperature;
4) the suspension centrifugation in reactor is obtained powder product, then powder product is used respectively deionized water and soaked in absolute ethyl alcohol, washing, then dry, obtain loose structure ammonium vanadate material.
The temperature of described deionized water is 50 ~ 60 DEG C.
Described mixing time is 0.5h ~ 1h.
Described pH value is employing 2 ~ 5molL -1watery hydrochloric acid carry out regulating.
The time of described phonochemical reaction is 0.5h ~ 1h.
Temperature in step 3) adopts platinum resistance to measure.
The time of described insulation is 20 ~ 60min.
The detailed process of described deionized water and soaked in absolute ethyl alcohol, washing is: powder product is first soaked 10min with deionized water, washs 5 times, and then use soaked in absolute ethyl alcohol 10min, wash 5 times.
Described drying is carried out in electric vacunm drying case.
The temperature of described drying is 50 ~ 60 DEG C, and the time is 6 ~ 8h.
Relative to prior art, the beneficial effect that the present invention has: the present invention adopts microwave-ultraviolet technique to prepare the NH of loose structure 4v 3o 8crystallite, i.e. loose structure anode material for lithium-ion batteries.Microwave, ultraviolet are electromagnetic wave, can provide energy for reaction, and microwave heating is even, efficiency is higher, can promote that chemical reaction evenly, rapidly carries out.The NH that the inventive method is obtained 4v 3o 8crystallite chemical composition is homogeneous, and purity is higher, is special loose structure, effectively can increases the specific area of material, as having good chemical property during anode material for lithium-ion batteries.Preparation method of the present invention is simple, reaction temperature low (lower than 100 DEG C), and the reaction time is short, and without the need to subsequent treatment, environmentally friendly, can large-scale production be applicable to.
Accompanying drawing explanation
Fig. 1 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8x-ray diffraction (XRD) collection of illustrative plates of crystallite.
Fig. 2 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8eSEM (SEM) photo of crystallite.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
Embodiment 1
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 60 DEG C, magnetic agitation 1h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.10mol/L 4vO 3solution, is designated as solution A;
2) 5molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 1.5, then the solution A after adjust ph is carried out phonochemical reaction 1h under the ultrasonic power of 400W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on B solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 90 DEG C, insulation 20min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 6h at 60 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
As can be seen from Figure 1, the NH prepared by the present embodiment 4v 3o 8good crystallinity, purity is higher.As shown in Figure 2, the NH for preparing of the present embodiment 4v 3o 8for loose structure, and comparatively loose.
Embodiment 2
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 60 DEG C, magnetic agitation 1h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.08mol/L 4vO 3solution, is designated as solution A;
2) 4molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 2.0, then it is carried out phonochemical reaction 0.5h under the ultrasonic power of 400W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 80 DEG C, insulation 30min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 6h at 60 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
Embodiment 3
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 55 DEG C, magnetic agitation 0.75h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.06mol/L 4vO 3solution, is designated as solution A;
2) 3molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 2.50, then it is carried out phonochemical reaction 0.5h under the ultrasonic power of 300W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 70 DEG C, insulation 40min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 8h at 50 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
Embodiment 4
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 53 DEG C, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.05mol/L 4vO 3solution, is designated as solution A;
2) 2molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 3.0, then it is carried out phonochemical reaction 0.75h under the ultrasonic power of 200W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 60 DEG C, insulation 60min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 7h at 50 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
Embodiment 5
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 57 DEG C, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.03mol/L 4vO 3solution, is designated as solution A;
2) 3molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 2.5, then it is carried out phonochemical reaction 0.5h under the ultrasonic power of 200W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 80 DEG C, insulation 40min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 8h at 50 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
Embodiment 6
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 57 DEG C, magnetic agitation 0.6h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.04mol/L 4vO 3solution, is designated as solution A;
2) 2molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 2, then it is carried out phonochemical reaction 0.7h under the ultrasonic power of 250W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 85 DEG C, insulation 65min, then naturally cools to room temperature;
4) reactor is opened, suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, use soaked in absolute ethyl alcohol 10min again, wash 5 times, to be then placed in electric vacunm drying case dry 7.5h at 55 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.
Embodiment 7
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 50 DEG C, magnetic agitation 0.8h makes ammonium metavanadate be uniformly dissolved, and obtains NH 4 +concentration be the NH of 0.07mol/L 4vO 3solution, is designated as solution A;
2) 5molL is adopted -1watery hydrochloric acid regulate the pH value of solution A to be 1.5, then it is carried out phonochemical reaction 0.9h under the ultrasonic power of 350W, obtains B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on solution simultaneously, wherein uviol lamp medium wavelength is 365nm, the power of uviol lamp is 500W, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 15 DEG C/min by room temperature to after 65 DEG C, insulation 50min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation in reactor is obtained powder product, powder product is first soaked 10min with deionized water, wash 5 times, then use soaked in absolute ethyl alcohol 10min, wash 5 times, then to be placed in electric vacunm drying case dry 8h at 50 DEG C, to obtain the NH of loose structure 4v 3o 8crystallite, namely obtains loose structure ammonium vanadate material.

Claims (9)

1. a preparation method for loose structure ammonium vanadate material, is characterized in that, comprises the following steps:
1) analytically pure ammonium metavanadate is dissolved in deionized water, stirs and ammonium metavanadate is uniformly dissolved, obtain NH 4 +concentration be the NH of 0.03 ~ 0.10mol/L 4vO 3solution, is designated as solution A;
2) pH value of solution A is adjusted to after 1.5 ~ 3.0 under the ultrasonic power of 200 ~ 400W, carries out phonochemical reaction, obtain B solution;
3) B solution is poured in reactor, make microwave and uviol lamp act on B solution simultaneously, wherein the wavelength of uviol lamp is 365nm, the power of uviol lamp is 500W, microwave power is 400 ~ 600W, be incubated to 60 ~ 90 DEG C by room temperature with the heating rate of 15 DEG C/min, the time of insulation is 20 ~ 60min, then naturally cool to room temperature;
4) the suspension centrifugation in reactor is obtained powder product, then powder product is used respectively deionized water and soaked in absolute ethyl alcohol, washing, then dry, obtain loose structure ammonium vanadate material.
2. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, is characterized in that, the temperature of described deionized water is 50 ~ 60 DEG C.
3. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, it is characterized in that, described mixing time is 0.5h ~ 1h.
4. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, it is characterized in that, described pH value is employing 2 ~ 5molL -1watery hydrochloric acid carry out regulating.
5. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, is characterized in that, the time of described phonochemical reaction is 0.5h ~ 1h.
6. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, is characterized in that, step 3) in temperature adopt platinum resistance measure.
7. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, it is characterized in that, the detailed process of described deionized water and soaked in absolute ethyl alcohol, washing is: powder product is first soaked 10min with deionized water, wash 5 times, and then use soaked in absolute ethyl alcohol 10min, wash 5 times.
8. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1, it is characterized in that, described drying is carried out in electric vacunm drying case.
9. the preparation method of a kind of loose structure ammonium vanadate material according to claim 1 or 8, is characterized in that, the temperature of described drying is 50 ~ 60 DEG C, and the time is 6 ~ 8h.
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CN105932278B (en) * 2016-04-29 2019-03-22 陕西科技大学 A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method
CN106129349A (en) * 2016-06-27 2016-11-16 陕西科技大学 A kind of anode material for lithium-ion batteries ammonium vanadate/Graphene and preparation method thereof
CN107162054B (en) * 2017-05-16 2019-04-02 陕西科技大学 A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal
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