CN103700824B - A kind of sandwich-like NH 4v 3o 8nanocrystalline preparation method - Google Patents

A kind of sandwich-like NH 4v 3o 8nanocrystalline preparation method Download PDF

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CN103700824B
CN103700824B CN201310697856.4A CN201310697856A CN103700824B CN 103700824 B CN103700824 B CN 103700824B CN 201310697856 A CN201310697856 A CN 201310697856A CN 103700824 B CN103700824 B CN 103700824B
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solution
sandwich
nanocrystalline
deionized water
reactor
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CN103700824A (en
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黄剑锋
曹杉杉
欧阳海波
曹丽云
李翠艳
费杰
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
    • 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

A kind of sandwich-like NH 4v 3o 8nanocrystalline preparation method, dissolves ammonium metavanadate in deionized water, obtains NH 4vO 3solution, is designated as solution A; The pH value of solution A is adjusted to 4.5 ~ 6.0, obtains B solution; B solution is poured in reactor, make microwave action in B solution, under microwave power is 400 ~ 600W, is warmed up to 60 ~ 90 DEG C and is incubated; Suspension centrifugation in reactor is obtained powder product, then washing, drying.Preparation technology of the present invention is simple, and reaction temperature is low, and reaction time is short, and without the need to subsequent treatment, environmentally friendly, can large-scale production be applicable to.The NH that the inventive method is obtained 4v 3o 8nanocrystalline chemical composition is homogeneous, and purity is higher, is special sandwich-like pattern, and the nano-particles self assemble be about between the thin slice of 30nm and sheet by thickness forms, and it will have good chemical property as during anode material for lithium-ion batteries.

Description

A kind of sandwich-like NH 4v 3o 8nanocrystalline preparation method
Technical field
The invention belongs to battery material preparation field, be specifically related to a kind of microwave irradiation technology that adopts and synthesize sandwich-like NH 4v 3o 8nanocrystalline method.
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.In addition, NH 4v 3o 8material also can be used as ammonia sensitive sensor, ultracapacitor and catalysis material, has purposes widely and Research Prospects.
Current preparation NH 4v 3o 8the method of material mainly contains two kinds: the precipitation method and hydro thermal method.NianWang etc. are with NH 4vO 3be raw material with hydrochloric acid, 180 DEG C of hydro-thermal reactions 4 days, obtain the ammonium vanadate nano wire [NianWang that diameter is about 20-50nm, length reaches some tens of pm, WenChen, LiqiangMai, etal.Selected-controlhydrothermalsynthesisandformationme chanismof1Dammoniumvanadate [J] .JournalofSolidStateChemistry, 2008,181:652-657.] Heai-KuPark etc. is with V 2o 5be raw material with urea, adopt sluggish precipitation to prepare NH 4v 3o 8.First obtained barium oxide gel, then refluxes the mixed liquor of itself and urea one week at 80 DEG C, has obtained the NH that diameter is 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.].S.G.Leonardi etc. are with V 2o 5, NaOH and (NH 4) 2sO 4for raw material, first pass through V 2o 5na is obtained with NaOH 3vO 4, and then with (NH 4) 2sO 4at 100 DEG C of reaction 20-40min, obtained thickness is about the sheet NH of 150-200nm 4v 3o 80.5H 2o [S.G.Leonardi, P.Primerano, N.Donato, etal.Behaviorofsheet-likecrystallineammoniumtrivanadateh emihydrate (NH 4v 3o 80.5H 2o) asanovelammoniasensingmaterial [J] .JournalofSolidStateChemistry, 2013,202:105-110.].
Above-mentioned precipitation method synthesis NH 4v 3o 8have that course of reaction is wayward, shortcoming, the water heat transfer NH such as have side reaction generation, product purity low and reaction time long 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 simple, easy control, Fast back-projection algorithm NH 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 sandwich-like NH 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 4v 3o 8nanocrystalline preparation method.
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, stir and ammonium metavanadate is uniformly dissolved, obtain NH 4 +concentration be the NH of 0.01 ~ 0.10mol/L 4vO 3solution, is designated as solution A;
2) pH value of solution A is adjusted to 4.5 ~ 6.0, obtains B solution;
3) B solution is poured in reactor, make microwave action in B solution, under microwave power is 400 ~ 600W, is incubated to 60 ~ 90 DEG C by room temperature with the heating rate of 10 DEG C/min, then naturally cools to room temperature;
4) the suspension centrifugation in reactor is obtained powder product, then powder product is washed with deionized water and soaked in absolute ethyl alcohol respectively, then dry, obtain the NH of sandwich-like 4v 3o 8nanocrystalline.
The temperature of described deionized water is 50 ~ 60 DEG C.
Described mixing time is 0.5 ~ 1h.
Described pH value is employing 1 ~ 4molL -1dilute hydrochloric acid solution carry out regulating.
Temperature in step 3) adopts platinum resistance to measure.
The time of described insulation is 60 ~ 150min.
The detailed process that described deionized water and soaked in absolute ethyl alcohol are also washed 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 technique to prepare NH 4v 3o 8nanocrystalline, microwave heating is even and efficiency is higher, can promote that chemical reaction evenly, rapidly carries out.Preparation technology of the present invention is simple, reaction temperature low (lower than 100 DEG C), and reaction time is short, and without the need to subsequent treatment, environmentally friendly, can large-scale production be applicable to.The NH that the inventive method is obtained 4v 3o 8nanocrystalline chemical composition is homogeneous, and purity is higher, is special sandwich-like pattern, and the nano-particles self assemble be about between the thin slice of 30nm and sheet by thickness forms, and it will have good chemical property as during anode material for lithium-ion batteries.
Accompanying drawing explanation
Fig. 1 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8nanocrystalline X-ray diffraction (XRD) collection of illustrative plates.
Fig. 2 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8nanocrystalline ESEM (SEM) photo.
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 50 DEG C, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.01mol/L 4vO 3solution, is designated as solution A;
2) 1molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 6.0, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 90 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 6h at 60 DEG C, to obtain the NH of sandwich-like 4v 3o 8nanocrystalline.
As can be seen from Figure 1, the NH prepared by the present embodiment 4v 3o 8nanocrystalline good crystallinity, purity is higher.As shown in Figure 2, the NH for preparing of the present embodiment 4v 3o 8nanocrystalline growth is better, is special sandwich-like pattern, and the nano-particles self assemble be about between the thin slice of 30nm and sheet by thickness forms.
Embodiment 2
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 60 DEG C, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.03mol/L 4vO 3solution, is designated as solution A;
2) 2molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 5.50, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 80 DEG C, insulation 90min, 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 60 DEG C, to obtain the NH of sandwich-like 4v 3o 8nanocrystalline.
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 is mixed with NH 4 +concentration be the NH of 0.05mol/L 4vO 3solution, is designated as solution A;
2) 3molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 5.0, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 70 DEG C, insulation 120min, then naturally cools to room temperature;
4) open reactor, the suspension centrifugation obtained 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 sandwich-like 4v 3o 8nanocrystalline.
Embodiment 4
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 53 DEG C, magnetic agitation 0.75h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.07mol/L 4vO 3solution, is designated as solution A;
2) 4molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 4.5, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 60 DEG C, insulation 150min, 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 50 DEG C, to obtain the NH of sandwich-like 4v 3o 8nanocrystalline.
Embodiment 5
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 57 DEG C, magnetic agitation 1h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.10mol/L 4vO 3solution, is designated as solution A;
2) 2molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 5.0, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 70 DEG C, insulation 100min, 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 sandwich-like 4v 3o 8nanocrystalline.
Embodiment 6
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in the deionized water of 50 DEG C, magnetic agitation 0.6h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.06mol/L 4vO 3solution, is designated as solution A;
2) 2.5molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to be 6.0, obtain B solution;
3) pour in reactor by B solution, make microwave action in B solution, microwave power controls at 400 ~ 600W, adopts platinum resistor temperature measuring, with the heating rate of 10 DEG C/min by room temperature to after 65 DEG C, insulation 135min, 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 7.5h at 55 DEG C, to obtain the NH of sandwich-like 4v 3o 8nanocrystalline.

Claims (8)

1. a sandwich-like NH 4v 3o 8nanocrystalline preparation method, is characterized in that, comprises the following steps:
1) analytically pure ammonium metavanadate is dissolved in deionized water, stir and ammonium metavanadate is uniformly dissolved, obtain NH 4 +concentration be the NH of 0.01 ~ 0.10mol/L 4vO 3solution, is designated as solution A;
2) pH value of solution A is adjusted to 4.5 ~ 6.0, obtains B solution;
3) B solution is poured in reactor, make microwave action in B solution, under microwave power is 400 ~ 600W, is incubated to 60 ~ 90 DEG C by room temperature with the heating rate of 10 DEG C/min, then naturally cools to room temperature;
4) the suspension centrifugation in reactor is obtained powder product, then powder product is washed with deionized water and soaked in absolute ethyl alcohol respectively, then dry, obtain the NH of sandwich-like 4v 3o 8nanocrystalline;
The time of described insulation is 60 ~ 150min.
2. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, the temperature of described deionized water is 50 ~ 60 DEG C.
3. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, described mixing time is 0.5 ~ 1h.
4. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, described pH value is employing 1 ~ 4molL -1dilute hydrochloric acid solution carry out regulating.
5. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, step 3) in temperature adopt platinum resistance measure.
6. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, the detailed process that described deionized water and soaked in absolute ethyl alcohol are also washed 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.
7. a kind of sandwich-like NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, described drying is carried out in electric vacunm drying case.
8. a kind of sandwich-like NH according to claim 1 or 7 4v 3o 8nanocrystalline preparation method, is characterized in that, the temperature of described drying is 50 ~ 60 DEG C, and the time is 6 ~ 8h.
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CN104485442B (en) * 2014-12-05 2017-01-11 陕西科技大学 Preparation method of self-assembled ball-flower type cathode material for lithium ion battery
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
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
CN113353981B (en) * 2021-07-01 2023-01-31 陕西理工大学 Cu 3 (VO 4 ) 2 Preparation method of irregular nanorod

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