CN106159225A - A kind of method producing carbon complex amorphous vanadium oxide powder - Google Patents

A kind of method producing carbon complex amorphous vanadium oxide powder Download PDF

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CN106159225A
CN106159225A CN201610592630.1A CN201610592630A CN106159225A CN 106159225 A CN106159225 A CN 106159225A CN 201610592630 A CN201610592630 A CN 201610592630A CN 106159225 A CN106159225 A CN 106159225A
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vanadium oxide
oxide powder
carbon complex
source
complex amorphous
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CN106159225B (en
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秦明礼
吴昊阳
贾宝瑞
李小丽
曹知勤
曲选辉
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University of Science and Technology Beijing USTB
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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
    • H01M4/362—Composites
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
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  • Battery Electrode And Active Subsutance (AREA)
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Abstract

The present invention relates to a kind of method producing carbon complex amorphous vanadium oxide nanopowders end, belong to new energy field.Technical process is: use vanadium source, fuel, adjuvant and carbon source to be raw material, wiring solution-forming according to a certain percentage；Heating solution under certain atmosphere, after volatilization, concentrating formation gel, there is combustion synthesis reaction in solution.Combustion reaction liberated heat can make reaction from maintaining, and finally gives carbon complex amorphous vanadium oxide powder.Course of reaction produces a large amount of gas, not only can effectively prevent powder product from reuniting, also can form meso-hole structure.And owing to utilizing liquid phase to mix, can realize granularity tiny amorphous vanadium particle and carbon combine closely with dispersed.Raw material of the present invention is easy to get, and technique is simple, and low cost, it is easy to industrialization, when the carbon complex amorphous vanadium oxide powder preparing is as lithium cell negative pole material, has high power capacity and excellent cyclical stability concurrently.

Description

A kind of method producing carbon complex amorphous vanadium oxide powder
Technical field
The invention belongs to new energy field, relate to the carbon complex amorphous vanadium oxide as lithium cell negative pole for a kind of one-step synthesis The method of material.
Background technology
New and renewable sources of energy technology is one of 21 century most important new high-tech industry, wherein electrochemical energy storage The developing direction of system is Large Copacity, high power and long-life.And lithium ion battery is lightweight with it, energy density big, without note Recall the advantage such as effect, life-span length, be widely used in the fields such as mobile phone, video camera, notebook computer, electric automobile.At present, business Lithium ion battery negative material be mainly carbons negative material, its theoretical capacity is only 372mAh/g, does not adapt to The miniaturization of current portable electric appts and the widespread demand of electric automobile team large-capacity high-power electrochmical power source.Cause This, for high-energy-density, long circulation life, fast charging and discharging lithium ion battery demand very urgent.At present, substantial amounts of research Having shifted towards and finding novel negative material, wherein vanadium oxide has typical layer structure, high theoretical specific capacity, valency due to it Lattice are cheap and easily obtain, and become preferable candidate material.Although the vanadium oxide capacity of crystalline state is high, it is possible to provide substantial amounts of lattice stores up Deposit lithium ion, but after storing, its lattice is easily converted to stable phase, and therefore lithium ion is pricked in lattice by solid, irreversible. Additionally, the poorly conductive of vanadium oxide, resistance is high.These two aspects all limits its application in terms of lithium electricity.
Research shows the lithium electrical property having two kinds of measures can improve vanadium oxide: one can be by the compound method of carbon enters Row improves, this is because material with carbon element has, conductance is high, specific surface area is big, pliability good and metal oxide has collaborative effect Advantage should be waited, electric conductivity and the cyclical stability of composite can be improved.Two is by vanadium oxide amorphous material, and this is due to nothing The vanadium oxide of amorphous configuration is possible not only to alleviate bulk effect, and a large amount of defects in structure are also used as lithium in charge and discharge process The storage point of ion, is conducive to improving capacity.For example, Niu etc. (Niu C, et al.Nanoresearch, 2015.) are by inclined vanadium Solution is positioned in reactor, heats at 180 DEG C by acid ammonium, citric acid and ethylene glycol wiring solution-forming, more heavy by obtain Shallow lake thing carries out washing, is dried, and finally carries out calcining in a nitrogen atmosphere and obtains amorphous vanadium/carbosphere, and this microballoon is used for During lithium ion battery, present the excellent chemical properties such as high efficiency, high stability, life-span length.Therefore, how simply, side Just, efficiently and low cost prepare carbon complex amorphous vanadium oxide material to promoting that application in lithium electricity for the vanadium oxide has weight Want meaning.
Content of the invention
The present invention provides a kind of method preparing carbon complex amorphous vanadium oxide powder.The present invention with vanadate for vanadium source, Water soluble organic substance is carbon source, and adding appropriate amine organic matter is adjuvant or fuel, utilizes synthetic method of solution burning, one Step obtains carbon and amorphous state vanadium oxide composite powder.The method is simple, efficiently, low cost, and can realize tiny amorphous Vanadium oxide particle is uniformly combined with carbon.
It is characteristic of the invention that solution combustion synthesis application in preparing carbon complex amorphous vanadium oxide powder.Solution combustion Synthesis is to betide a kind of combustion reaction between oxidant and fuel in solution, and therefore, it possesses the advantage of wet chemical method, Can ensure that the uniformity that each component mixes in the liquid phase, composition is accurate, easily-controllable, and with conventional wet chemical method such as sol-gel Method, the precipitation method etc. compare, the advantage that the method has again uniqueness: in course of reaction, liberated heat can make reaction from dimension Holding, it is not necessary to extra power, energy consumption is low；Releasing substantial amounts of gas in course of reaction and making combustion product is fluffy foam-like, permissible Effectively prevent from reuniting, form the nano-powder of high-specific surface area；Combustion velocity is fast, can complete within a few minutes, technique letter Just, fast；Furthermore, it is possible to by factor controls such as the amounts of the proportioning of adjustment fuel and oxidant, the rate of heat addition and combustible substance Combustion process processed, and then control synthetic powder composition, thing phase, pattern and performance.
After vanadium source and carbon source are dissolved in water by the present invention, in aqueous by vanadium source and carbon source at atom, lewis' acid Uniformly mix in level, by conditions such as control fuel and oxidant proportioning, combustion atmosphere, raw material proportionings, it is not necessary to external heat source, Utilize combustion reaction liberated heat to make reaction from maintenance, and make vanadium source in solution be converted into the tiny amorphous state oxidation of granularity Vanadium particle, uniform " inlaying " is distributed in the carbon base body that carbon source pyrolysis is formed, thus realizes tiny amorphous vanadium particle It is uniformly combined with carbon.Have high power capacity and excellent cyclical stability with electrode prepared by this material concurrently, close at the electric current of 0.1A/g Under degree, the capacity after 100 circulations is no less than 700mAh/g.
The invention is characterised in that and comprise the following steps:
1st, weigh the raw materials such as vanadium source, fuel, adjuvant and carbon source according to certain ratio, carry out uniformly with a certain amount of water Stirring, mixes and is made into precursor solution.Wherein the proportioning between each raw material is: the mol ratio in fuel and vanadium source is 0.5-10, The mol ratio in adjuvant and vanadium source is 2-15, and the mol ratio in carbon source and vanadium source is 0.01-1；
2nd, it is positioned over the precursor solution obtaining in step 1 on heating furnace, under certain atmosphere, this solution is added Heat, after boiling, evaporation form gel, there is combustion synthesis reaction, finally gives carbon complex amorphous vanadium oxide powder in solution End；
Vanadium source described in step 1 is selected from ammonium metavanadate, one or more in ammonium poly-vanadate；Fuel selected from urea, One or more in glycine；Adjuvant is selected from nitric acid, ammonium nitrate, one or more in citric acid；Carbon source One or more in sucrose, glucose, fructose, maltose, inosite, soluble starch, glycogen, wood sugar；One Determining atmosphere is air, argon gas, one or more in nitrogen.
The invention have the advantage that
1st, combustion reaction one step between each raw material in liquid phase is utilized to prepare carbon complex amorphous vanadium oxide powder, technique Easy, quick, efficiency is high, low cost.
2nd, combustion reaction liberated heat can make reaction from maintaining, and energy consumption is low；
3rd, a large amount of gases released in course of reaction not only can effectively prevent powder product from reuniting, and can form a large amount of Jie Pore structure, the beneficially raising of lithium electrical property.
4th, can realize granularity tiny amorphous vanadium particle and carbon combine closely with dispersed；
5th, can by adjust the factor controlling products such as proportioning between raw material, the atmosphere of reaction and heating parameters phase, Pattern and carbon content, and then the performance of control synthetic powder.
6th, when the carbon complex amorphous vanadium oxide powder preparing is as lithium cell negative pole material, high power capacity and excellent is had concurrently Cyclical stability.
Brief description
Fig. 1 is the X-ray diffractogram of example 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of example 1.
Fig. 3 is the nitrogen adsorption desorption curve map of example 1.
Fig. 4 is lithium electricity cycle performance figure under 0.1A/g current density for the example 1.
Detailed description of the invention
Embodiment 1
Weigh ammonium metavanadate 0.1 mole, 0.8 mole of ammonium nitrate, citric acid 0.3 mole, glycine 0.08 mole, glucose 0.02 mole is configured to solution, uniformly mixes vanadic acid radical ion and carbon source molecule in the solution.Solution is placed on heating furnace, Heat under air.After boiling, evaporation form gel, there is combustion synthesis reaction in solution, finally obtains carbon and be combined Amorphous vanadium powder.
Embodiment 2
Weigh ammonium metavanadate 0.1 mole, 0.8 mole of ammonium nitrate, citric acid 0.3 mole, glycine 0.08 mole, glucose 0.03 mole is configured to solution, is placed in solution on heating furnace, heats under air.Solution is formed through boiling, evaporation After gel, there is combustion synthesis reaction, obtain carbon complex amorphous vanadium oxide powder.
Embodiment 3
Weigh ammonium metavanadate 0.06 mole, 0.8 mole of ammonium nitrate, citric acid 0.3 mole, glycine 0.08 mole, grape Sugar 0.01 mole is configured to solution, is placed in solution on heating furnace, heats under air.Solution is through boiling, evaporation shape After becoming gel, there is combustion synthesis reaction, obtain carbon complex amorphous vanadium oxide powder.
Result of the test
Use the carbon complex amorphous vanadium oxide material preparing in above-mentioned 3 embodiments as active material, with conduction charcoal Black (Super P), polyvinylidene fluoride (PVDF) makes the negative material of lithium electricity according to mass ratio 60:30:10.Mixture is divided It is scattered in nmp solution make slurry, then equably slurry is coated onto on Copper Foil with blade, 120 DEG C of dryings in vacuum drying chamber After 12h, at 200kg m-2Pressure under be pressed into disk.It is CR2023 type button cell by electrode assembling in vacuum glove box Carrying out electro-chemical test, the EC/DMC (1:1wt%) containing 1M LiPF6 is as electrolyte.Metal lithium sheet is as to electrode.Envelope After the button cell installing stands 12h, LAND test system carries out the constant current charge-discharge test of button cell, voltage model Enclose for 0.01-3V (vs Li+/ Li), current density is 0.1A/g, and test environment temperature is maintained at about 25 DEG C.Result is added up such as Table 1:
Comparative example 1:
Weighing ammonium metavanadate 0.1 mole, 0.8 mole of ammonium nitrate, citric acid 0.32 mole, glycine 0.08 mole, by respectively Plant raw material soluble in water, be configured to solution.Solution is placed on heating furnace, heats under a nitrogen.Solution through boiling, After evaporation forms gel, there is combustion synthesis reaction, finally give the V of crystalline state2O3Powder.Use and embodiment is the 1st, the 2nd, 3 identical Method is prepared as lithium ion battery with this material for negative material and carries out electro-chemical test.Under the current density of 0.1A/g, 100 Capacity after secondary circulation is 320mAh/g.
In sum, the present invention uses solution combustion synthetic method one step to prepare carbon complex amorphous vanadium oxide powder, its The vanadium oxide particle of middle amorphous state uniform " inlaying " is distributed in the carbon base body that carbon source pyrolysis is formed.The oxygen of this impalpable structure Changing vanadium to be possible not only to alleviate the bulk effect in charge and discharge process, a large amount of defects in structure are also used as in charge and discharge process The storage point of lithium ion；And carbon base body has, and conductance is high, specific surface area is big, pliability is good has collaborative with metal oxide The advantages such as effect, can improve electric conductivity and the cyclical stability of whole composite.Therefore, the carbon complex amorphous of the present invention The vanadium oxide that vanadium oxide powder compares crystalline state as the negative material of lithium ion battery has higher capacity, and outstanding following Ring stability.

Claims (6)

1. the method producing carbon complex amorphous vanadium oxide powder, it is characterised in that comprise the steps:
A, weigh vanadium source, fuel, adjuvant and carbon source raw material according to certain ratio, carry out uniform stirring with a certain amount of water, Mix and be made into precursor solution；Wherein the proportioning between each raw material is: the mol ratio in fuel and vanadium source is 0.5-10, adjuvant Mol ratio with vanadium source is 2-15, and the mol ratio in carbon source and vanadium source is 0.01-1；
It b, is positioned over the precursor solution obtaining in step a on heating furnace, under certain atmosphere, this solution is heated, molten After boiling, evaporation form gel, there is combustion synthesis reaction, finally give carbon complex amorphous vanadium oxide powder in liquid.
2. the method for production carbon complex amorphous vanadium oxide powder according to claim 1, it is characterised in that institute in a step The vanadium source stated is ammonium metavanadate, one or more in ammonium poly-vanadate.
3. the method for production carbon complex amorphous vanadium oxide powder according to claim 1, it is characterised in that institute in a step The fuel stated is urea, one or more in glycine.
4. the method for production carbon complex amorphous vanadium oxide powder according to claim 1, it is characterised in that institute in a step The adjuvant stated is nitric acid, ammonium nitrate, one or more in citric acid.
5. the method for production carbon complex amorphous vanadium oxide powder according to claim 1, it is characterised in that institute in a step The carbon source stated be sucrose, glucose, fructose, maltose, inosite, soluble starch, glycogen, in wood sugar one or both with On.
6. the method for production carbon complex amorphous vanadium oxide powder according to claim 1, it is characterised in that institute in a step The certain atmosphere stated is air, argon gas, one or more in nitrogen.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106829923A (en) * 2017-03-16 2017-06-13 石河子大学 A kind of biomass carbon material and preparation method
CN107892329A (en) * 2017-11-23 2018-04-10 北京科技大学 A kind of high flux conbustion synthesis powder body material preparation facilities and preparation method
CN113161522A (en) * 2021-03-12 2021-07-23 广东工业大学 Amorphous vanadium oxide/carbon composite material and preparation method and application thereof
CN113782726A (en) * 2021-09-13 2021-12-10 厦门理工学院 Preparation method of zinc ion battery positive electrode material, zinc ion battery positive electrode material and zinc ion battery

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CN103035882A (en) * 2011-10-10 2013-04-10 成都理工大学 Method for synthesizing Li3V2(PO4)3/C by using glycine-nitrate combustion method
CN103996826A (en) * 2013-02-15 2014-08-20 三星Sdi株式会社 Negative active material, and negative electrode and lithium battery each including the negative active material
CN103553131A (en) * 2013-10-29 2014-02-05 黑龙江大学 Preparation method of lithium ion battery negative electrode spherical V2O3/C composite material with multilevel structure

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106829923A (en) * 2017-03-16 2017-06-13 石河子大学 A kind of biomass carbon material and preparation method
CN107892329A (en) * 2017-11-23 2018-04-10 北京科技大学 A kind of high flux conbustion synthesis powder body material preparation facilities and preparation method
CN113161522A (en) * 2021-03-12 2021-07-23 广东工业大学 Amorphous vanadium oxide/carbon composite material and preparation method and application thereof
CN113161522B (en) * 2021-03-12 2022-07-19 广东工业大学 Amorphous vanadium oxide/carbon composite material and preparation method and application thereof
CN113782726A (en) * 2021-09-13 2021-12-10 厦门理工学院 Preparation method of zinc ion battery positive electrode material, zinc ion battery positive electrode material and zinc ion battery

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