CN107845793A - A kind of lithium battery zinc oxide/lithium vanadate anode material and preparation method - Google Patents
A kind of lithium battery zinc oxide/lithium vanadate anode material and preparation method Download PDFInfo
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- CN107845793A CN107845793A CN201711007527.7A CN201711007527A CN107845793A CN 107845793 A CN107845793 A CN 107845793A CN 201711007527 A CN201711007527 A CN 201711007527A CN 107845793 A CN107845793 A CN 107845793A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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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
- 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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The present invention provides a kind of lithium battery zinc oxide/lithium vanadate anode material and preparation method.Vanadium system presoma and lithium system presoma are first prepared, the two is mixed with nanometer fibrous zinc oxide in ball mill, and using microwave heating and calcining generation zinc oxide/lithium vanadate composite.This method is modified by nanometer fibrous zinc oxide to lithium vanadate, improve structural stability, high-rate discharge ability and the electron mobility of material, suction ripple rate due to two kinds of materials in sintering process is different, internal stress increases, occur more micropore, crackle after annealing, increase Li ion deinsertion passages, while the preparation method process that this method is heated using ball mill and microwave is simple, energy consumption is low, pollution-free.
Description
Technical field
The present invention relates to lithium cell cathode material field, and in particular to by nanometer fibrous modified zinc oxide lithium vanadate,
More particularly to a kind of lithium battery zinc oxide/lithium vanadate anode material and preparation method.
Background technology
Along with a large amount of uses of economic globalization process and fossil fuel, the problem of environmental pollution and energy shortage increasingly
It is prominent.In order to reduce the pollution that fossil fuel uses process, development wind, light, the sustainable renewable sources of energy of electricity and novel power battery
With high-efficiency energy-storage system, the reasonable disposition and electric adjustment of regenerative resource are realized, for the raising level of resources utilization, solves energy
Source crisis and environmental protection all have its own strategic significance.Lithium ion battery（LIB）With self discharge more high and low than energy, circulation
Performance is good, memory-less effect and it is green the advantages that, be high efficient secondary battery most with prospects and with fastest developing speed at present
Chemical energy storage power supply.
Lithium ion battery is developed by lithium battery.Lithium battery be it is a kind of by lithium metal or lithium alloy be positive electrode,
Use the battery of non-aqueous electrolytic solution.Lithium ion battery is the one kind to grow up on the basis of studying lithium secondary battery
New chargeable battery.Its positive and negative pole material, which uses, is available for the lithium ion freely embedding de- active matter with stratiform or tunnel structure
Matter, during charging, Li+ escapes from positive pole, embedded negative pole, and during electric discharge, Li+ then deviates from from negative pole, inserts positive pole, i.e., in discharge and recharge
Cheng Zhong, Li+ are embedded in abjection in positive and negative interpolar and moved back and forth, it can be seen that, lithium ion cell positive and negative material are to determine electricity
The key factor of pond performance.
The positive electrode of lithium ion battery is the core of lithium ion battery, during battery charging and discharging, positive electrode
Not only to be used as lithium source, there is provided the reciprocal embedding de- required lithium between inside battery positive and negative polarities intercalation materials of li ions, also to bear electricity
Pond negative material surface forms the lithium that solid liquid interface film is consumed, and preferable positive electrode need to possess following characteristics：Current potential is high, ratio
Capacity is high, density is big, security is good, high rate performance is good and long-life etc..Lithium ion battery negative material should be able to accommodate greatly
The Li+ of amount, there is higher ionic conductivity and electronic conductivity, and good stability etc..In the lithium electricity applied at present
In pond positive pole and negative material, zinc oxide/lithium vanadate has the particular advantages that specific capacity is high, cheap, is conventional lithium ion
Cell positive material, it has been widely studied and applied.In addition, zinc oxide/lithium vanadate is because it has, specific capacity is big, operating voltage is low
The characteristics of, and a kind of Water-solution lithium ion battery negative pole material of great prospect, because it has excellent Li insertion extraction performance,
There are specific capacity height, low cost and other advantages as cell negative electrode material, led as lithium ion battery plus-negative plate investigation of materials
The forward position in domain and focus.
It is multiple that Chinese invention patent application number 201410276159.6 discloses a kind of lithium ion battery graphene/zinc oxide
Closing negative material and preparation method thereof, the graphene/zinc oxide composite negative pole material is blend, including graphene, zinc oxide,
This method is dissolved in aqueous zinc nitrate, graphene oxide powder in the mixed liquor of 1,2-PD and absolute ethyl alcohol, ultrasonic wave
ESD precursor liquids are obtained after stirring；Metal substrate is fixed on substrate clamping plate, is heated to 100~250 DEG C；ESD is used into forerunner
Liquid is sprayed on backing material；Misting cooling obtains material requested.
Chinese invention patent application number 201610044734.9 discloses a kind of Zinc modified graphene lithium-ion electric of oxidation
Graphene powder and Zinc oxide powder are well mixed by the preparation method of pond negative material, this method, are then placed in reacting furnace
Heating, and holding is passed through protective gas and is incubated, and is then cooled to room temperature, obtains aoxidizing Zinc modified graphene lithium-ion electric
Pond negative material.
Chinese invention patent application number 201510578783.6 disclose a kind of composite cathode material of lithium ion battery and its
Preparation method, the invention first weigh lithium source and vanadium source, and addition " additive and solvent " or " complexing agent and solvent " forms molten afterwards
Liquid or slurry；Weigh lithium source and titanium source, add " additive and solvent " either " complexing agent and solvent " formed afterwards solution or
Slurry；After two kinds of solution or slurry are well mixed, dry, sintering obtains composite.
Chinese invention patent application number 201510287168.X disclose a kind of modified vanadic acid lithium material and method of modifying and
Application in lithium ion battery, it is small that 1~10 is calcined at a temperature of 300~800 DEG C by lithium vanadate sample under vacuum
When be made, this method is simple and easy, and the pattern to lithium vanadate and size do not carry out any regulation and control and cladding, avoid carbon material or
The negative effect that the introducing of other materials is brought, it is easy to accomplish industrialized production..
According to above-mentioned, when existing zinc oxide, lithium vanadate are used for lithium ion battery negative material, because vanadium has multiple oxygen
Change state, electrode multiple discharge platforms in discharge process is present, and the stability of its layer structure is not good enough, makes negative material
Capacity attenuation quickly, poor circulation.In addition, prior art zinc oxide/lithium vanadate is applied to negative electrode of lithium ion battery composite wood
The technical method of material is simultaneously immature, complex technical process and high energy consumption, in consideration of it, the present invention propose a kind of innovative lithium from
Sub- cell oxidation zinc/lithium vanadate anode material and preparation method, can effectively solve above-mentioned technical problem.
The content of the invention
When being used for lithium ion battery negative material for current lithium vanadate, because vanadium has multiple oxidation state, make lithium vanadate
Multiple discharge platforms in discharge process be present, and the stability of its layer structure is not good enough, makes the capacity attenuation of negative material very
It hurry up, the defects of poor circulation, the present invention proposes a kind of lithium ion battery zinc oxide/lithium vanadate anode material and preparation
Method, while so as to give full play to good characteristic of zinc oxide/lithium vanadate itself, realize negative material high stability will
Ask.
Concrete technical scheme of the present invention is as follows：
A kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material, is characterized in by nanometer fibrous oxidation
Zinc is modified to lithium vanadate, structural stability, high-rate discharge ability and the electron mobility of material is improved, in sintering process
In due to the suction ripple rate of two kinds of materials it is different, internal stress increase, occur more micropore, crackle after annealing, increase Li ions
Deintercalation passage；Its prepare the step of be：
（1）The preparation of vanadium system presoma：Vanadic anhydride is weighed, 4 ~ 6h is heated to reflux in organic alcohol solvent, is cooled to room temperature
After add phosphoric acid, continue to be heated to reflux 6 ~ 8h, through cooling down, filtering and wash, at 80 ~ 100 DEG C be dried in vacuo 20 ~ 24h, obtain
Vanadium system presoma；
（2）The preparation of lithium system presoma：It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, and is treated anti-
When should be 2 ~ 4 to solution ph, stop heating and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, divided after standing clarification
From, and 10 ~ 15h of drying precipitate is obtained being dehydrated phosphoric acid iron powder at 180 ~ 220 DEG C；By phosphoric acid iron powder and polyethylene
Alcohol is well mixed, and is heated to 550 ~ 650 DEG C under nitrogen protection, polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Add lithium
Source and carbon source, it is well mixed, is heated to 700 ~ 800 DEG C and continues 8 ~ 12h of calcining, lithium system presoma is made；
（3）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill；It is placed in just
In beautiful crucible, be put into micro-wave oven and carry out heating and calcining, wherein microwave power be 400 ~ 600W, microwave frequency for 2000 ~
3000MHz, reaction time are 3 ~ 5min, and zinc oxide/lithium vanadate composite is made.
Preferably, step（1）The Organic Alcohol is at least one of isopropanol, glycerine, isobutanol or phenmethylol.
Preferably, step（1）In backflow system, each material forms by weight is：It is 20 ~ 30 parts of vanadic anhydride, organic
50 ~ 68 parts of alcohol, 2 ~ 20 parts of phosphatase 11.
Preferably, step（2）The polyvinyl alcohol for analyze it is pure, number-average molecular weight be 5000 ~ 10000, alcoholysis degree be 78 ~
88%, glass transition temperature is 75 ~ 80 DEG C.
Preferably, step（2）The lithium source is lithium hydroxide or lithium carbonate.
Preferably, step（2）The carbon source is at least one of sucrose, starch, fructose or glucose.
Preferably, step（2）In preparation process, each material forms by weight is：32 ~ 53 parts of phosphoric acid iron powder, poly- second
5 ~ 10 parts of enol, 30 ~ 40 parts of lithium source, 12 ~ 18 parts of carbon source.
Preferably, step（3）The nanometer fibrous zinc oxide, length are 5-10 μm, and diameter of section is 5 ~ 50nm.
Preferably, step（3）The parts by weight of nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma form：
73 ~ 86 parts of vanadium system presoma, 10 ~ 15 parts of lithium system presoma, 4 ~ 12 parts of nanometer fibrous zinc oxide.
Preferably, step（3）The ball mill is conical ball mill, ultra-fine lamination ball mill, ceramic ball mill or grid
One kind in type ball mill.Ball mill is made up of the cylinder of level, input and output material hollow shaft and mill first class sections, and cylinder is long
Cylinder, built with abrasive body, cylinder is steel plate, is fixed by steel liner plate with cylinder, and abrasive body is generally steel ball, and by not
It is fitted into diameter and certain proportion in cylinder, abrasive body can also use steel section.Material is uniform through pan feeding quill shaft spiral by feed arrangement
Ground enters the storehouse of grinding machine first, there is ladder lining board or corrugated liner, built-in all size steel ball in the storehouse, and barrel body rotation produces centrifugation
Power is fallen after taking steel ball to certain altitude, and bang and abrasive action are produced to material.After material reaches corase grind in the first storehouse, warp
Single layer partition panel enters the second storehouse, studs with flat liner plate in the storehouse, inside there is steel ball, material is further ground.Powder is by unloading
Expect the discharge of grate plate, complete grinding operation.When material is compound, ball mill can not only play abrasive action, moreover it is possible to play very
Good immixture.Therefore, the present invention uses ball mill, to vanadium system presoma, lithium system presoma and nanometer fibrous zinc oxide
It is ground and is blended.
Preferably, the conical ball mill is body and the ball mill of frame one, and main shaft uses double-row self-aligning Roller Shaft
Hold, dry type or wet type grinding can be carried out.
Preferably, the ultra-fine lamination ball mill uses much broken and lessmill mode, by the grind grading of pulverizing-screening system+1/2
System forms, and is ground using without dust type.
Preferably, the ceramic ball mill is horizontal the lattice type of tubular rotation, two storehouses, by outer gear drive.
Preferably, the grate ball mill using segmental orifice plate composition grate carry out discharge, grate hole width be 1 ~
3mm。
The microwave heating and calcining should be carried out under excess oxygen, real by being passed through the oxygen-enriched air that oxygen content is 26 ~ 30%
It is existing.
A kind of lithium battery zinc oxide/lithium vanadate anode material, is prepared by the above method.Pass through nanofiber
Shape zinc oxide is modified to lithium vanadate, improves the stability and high-rate discharge ability, electron mobility of material structure.
The present invention is using nanometer fibrous zinc oxide to generated in-situ LiV3O8It is modified, the structure for improving material is steady
Qualitative, high-rate discharge ability, electron mobility and cyclical stability, due to the suction of two kinds of materials especially in sintering process
Ripple rate is different, internal stress increase, occurs more micropore, crackle after annealing, increases Li ion deinsertion passages.Thus, can obtain
To the zinc oxide/lithium vanadate composite for being more suitable as lithium cell cathode material.
The present invention a kind of lithium battery zinc oxide/lithium vanadate anode material and preparation method, compared with prior art,
The characteristics of it is protruded and excellent effect are：
1st, the method that zinc oxide/lithium vanadate anode material is prepared using ball mill and microwave heating is proposed.
2nd, lithium vanadate is modified by nanometer fibrous zinc oxide, improves the structural stability of material, high magnification is put
Electrical property, electron mobility and cycle performance.
3rd, the suction ripple rate due to two kinds of materials in sintering process is different, internal stress increase, occurs after annealing more
Micropore, crackle, increase Li ion deinsertion passages.
4th, the inventive method prepares zinc oxide/lithium vanadate anode material, raw material, equipment, energy consumption and cost of labor compared with
It is low, it is pollution-free, it can promote.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 6h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
6h, through cooling down, filtering and wash, 20h is dried in vacuo at 100 DEG C, obtains vanadium system precursor powder.Organic Alcohol be isopropanol with
The mixture of glycerine.Match and be：20 parts of vanadic anhydride, 60 parts of Organic Alcohol, 20 parts of phosphoric acid.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 4, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 220 DEG C
10h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 650 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 700 DEG C and continues to calcine
12h, lithium system presoma is made.Polyvinyl alcohol is to analyze pure, number-average molecular weight 10000, alcoholysis degree 78%, glass transition temperature
For 80 DEG C；Lithium source is lithium hydroxide；Carbon source is sucrose.Match and be：40 parts of ferric phosphate, 10 parts of polyvinyl alcohol, 32 parts of lithium source, carbon source
18 parts.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 78 parts of body, 10 parts of lithium system presoma, 12 parts of nanometer fibrous zinc oxide.Ball mill is conical ball mill, and its power of motor is
50kW, rotating cylinder rotating speed are 15r/min, Ball-milling Time 30min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 600W,
Microwave frequency is 2000MHz, reaction time 5min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 30%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Embodiment 2
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 4h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
8h, through cooling down, filtering and wash, 20h is dried in vacuo at 80 DEG C, obtains vanadium system precursor powder.Organic Alcohol be glycerine with
The mixture of isobutanol.Match and be：30 parts of vanadic anhydride, 58 parts of Organic Alcohol, 2 parts of phosphatase 11.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 4, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 180 DEG C
10h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 550 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 700 DEG C and continues to calcine
12h, lithium system presoma is made.To analyze pure, number-average molecular weight 5000, alcoholysis degree 88%, glass transition temperature is polyvinyl alcohol
80℃；Lithium source is lithium hydroxide；Carbon source is starch.Match and be：32 parts of ferric phosphate, 10 parts of polyvinyl alcohol, 40 parts of lithium source, carbon source 18
Part.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 81 parts of body, 15 parts of lithium system presoma, 4 parts of nanometer fibrous zinc oxide.Ball mill is ultra-fine lamination ball mill, its power of motor
For 50kW, rotating cylinder rotating speed is 35r/min, Ball-milling Time 30min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 600W,
Microwave frequency is 3000MHz, reaction time 3min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 30%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Embodiment 3
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 5h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
7h, through cooling down, filtering and wash, 22h is dried in vacuo at 90 DEG C, obtains vanadium system precursor powder.Organic Alcohol be isobutanol with
The mixture of phenmethylol.Match and be：25 parts of vanadic anhydride, 60 parts of Organic Alcohol, 5 parts of phosphatase 11.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 3, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 200 DEG C
13h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 650 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, 750 DEG C is heated to and continues to calcine 9h,
Lithium system presoma is made.Polyvinyl alcohol is to analyze pure, number-average molecular weight 8000, alcoholysis degree 80%, glass transition temperature 78
℃；Lithium source is lithium carbonate；Carbon source is fructose.Match and be：40 parts of ferric phosphate, 5 parts of polyvinyl alcohol, 40 parts of lithium source, 15 parts of carbon source.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 80 parts of body, 12 parts of lithium system presoma, 8 parts of nanometer fibrous zinc oxide.Ball mill is ceramic ball mill, and its power of motor is
40kW, rotating cylinder rotating speed are 25r/min, Ball-milling Time 25min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 500W,
Microwave frequency is 2500MHz, reaction time 4min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 28%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Embodiment 4
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 6h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
6h, through cooling down, filtering and wash, 20h is dried in vacuo at 100 DEG C, obtains vanadium system precursor powder.Organic Alcohol be isopropanol with
The mixture of phenmethylol.Match and be：24 parts of vanadic anhydride, 58 parts of Organic Alcohol, 8 parts of phosphatase 11.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 4, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 190 DEG C
12h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 600 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 720 DEG C and continues to calcine
10h, lithium system presoma is made.To analyze pure, number-average molecular weight 7000, alcoholysis degree 85%, glass transition temperature is polyvinyl alcohol
80℃；Lithium source is lithium hydroxide；Carbon source is glucose.Match and be：40 parts of ferric phosphate, 10 parts of polyvinyl alcohol, 32 parts of lithium source, carbon source
18 parts.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 81 parts of body, 15 parts of lithium system presoma, 4 parts of nanometer fibrous zinc oxide.Ball mill is grate ball mill, and its power of motor is
20kW, rotating cylinder rotating speed are 35r/min, Ball-milling Time 30min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 600W,
Microwave frequency is 3000MHz, reaction time 3min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 26%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Embodiment 5
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 5h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
8h, through cooling down, filtering and wash, 22h is dried in vacuo at 80 DEG C, obtains vanadium system precursor powder.Organic Alcohol is glycerine, different
The mixture of butanol and phenmethylol.Match and be：25 parts of vanadic anhydride, 55 parts of Organic Alcohol, 20 parts of phosphoric acid.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 2, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 220 DEG C
12h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 550 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 740 DEG C and continues to calcine
11h, lithium system presoma is made.To analyze pure, number-average molecular weight 6000, alcoholysis degree 78%, glass transition temperature is polyvinyl alcohol
80℃；Lithium source is lithium carbonate；Carbon source is sucrose.Match and be：45 parts of ferric phosphate, 5 parts of polyvinyl alcohol, 38 parts of lithium source, 12 parts of carbon source.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 80 parts of body, 10 parts of lithium system presoma, 10 parts of nanometer fibrous zinc oxide.Ball mill is grate ball mill, its power of motor
For 40kW, rotating cylinder rotating speed is 30r/min, Ball-milling Time 25min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 500W,
Microwave frequency is 2800MHz, reaction time 4min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 30%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Embodiment 6
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 5h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
6h, through cooling down, filtering and wash, 24h is dried in vacuo at 80 DEG C, obtains vanadium system precursor powder.Organic Alcohol be isopropanol with
The mixture of glycerine.Match and be：20 parts of vanadic anhydride, 68 parts of Organic Alcohol, 2 parts of phosphatase 11.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 3, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 220 DEG C
12h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 600 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 750 DEG C and continues to calcine
10h, lithium system presoma is made.Polyvinyl alcohol is to analyze pure, number-average molecular weight 10000, alcoholysis degree 88%, glass transition temperature
For 80 DEG C；Lithium source is lithium hydroxide；Carbon source is sucrose.Match and be：42 parts of ferric phosphate, 8 parts of polyvinyl alcohol, 35 parts of lithium source, carbon source
15 parts.
It is prepared by zinc oxide/vanadic acid lithium titanate cathode material：
（1）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.Before vanadium system
Drive 82 parts of body, 12 parts of lithium system presoma, 6 parts of nanometer fibrous zinc oxide.Ball mill is ultra-fine lamination ball mill, its power of motor
For 50kW, rotating cylinder rotating speed is 15r/min, Ball-milling Time 30min.
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 600W,
Microwave frequency is 2000MHz, reaction time 5min, and zinc oxide/lithium vanadate composite is made.Oxygen is passed through in calcination process to contain
Measure the oxygen-enriched air for 30%.
Zinc oxide/lithium vanadate composite is assembled with other electrode materials, obtains cathode of lithium battery.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Comparative example 1
It is prepared by vanadium system presoma：
Vanadic anhydride is weighed, 5h is heated to reflux in organic alcohol solvent, phosphoric acid is added after being cooled to room temperature, continues to be heated to reflux
6h, through cooling down, filtering and wash, 24h is dried in vacuo at 80 DEG C, obtains vanadium system precursor powder.Organic Alcohol be isopropanol with
The mixture of glycerine.Match and be：20 parts of vanadic anhydride, 68 parts of Organic Alcohol, 2 parts of phosphatase 11.
It is prepared by lithium system presoma：
It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, when question response to solution pH value is 3, stops
Only heat and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, separated after standing clarification, and to sediment at 220 DEG C
12h is dried, obtains being dehydrated phosphoric acid iron powder；Powder is uniform with polyvinyl alcohol, 600 DEG C are heated under nitrogen protection,
Polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Lithium source and carbon source are added, is well mixed, is heated to 750 DEG C and continues to calcine
10h, lithium system presoma is made.Polyvinyl alcohol is to analyze pure, number-average molecular weight 10000, alcoholysis degree 88%, glass transition temperature
For 80 DEG C；Lithium source is lithium hydroxide；Carbon source is sucrose.Match and be：42 parts of ferric phosphate, 8 parts of polyvinyl alcohol, 35 parts of lithium source, carbon source
15 parts.
It is prepared by vanadic acid lithium titanate cathode material：
（1）Vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill.82 parts of vanadium system presoma, lithium system forerunner
18 parts of body.Ball mill is ultra-fine lamination ball mill, and its power of motor is 50kW, and rotating cylinder rotating speed is 15r/min, and Ball-milling Time is
30min。
（2）Mixture is placed in corundum crucible, micro-wave oven is put into and carries out heating and calcining, wherein microwave power is 600W,
Microwave frequency is 2000MHz, reaction time 5min, and vanadic acid lithium titanate cathode material is made.Oxygen content is passed through in calcination process as 30%
Oxygen-enriched air.
（3）Vanadic acid lithium titanate cathode material and other electrode materials are assembled, obtain cathode of lithium battery.
It is not modified in comparative example 1 using nano zine oxide, other preparation conditions are consistent with embodiment 6.Its battery holds
Amount, voltage platform, cycle life, temperature tolerance, security and manufacturing cost, as shown in table 1.
Table 1：
| Performance indications | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 |
| Battery capacity（mAh/g） | 180~200 | 180~200 | 180~200 | 180~200 | 180~200 | 180~200 | 150~180 |
| Voltage platform（V） | 2~2.5 | 2~2.5 | 2~2.5 | 2~2.5 | 2~2.5 | 2~2.5 | 3~3.5 |
| Cycle life（It is secondary） | 800~1200 | 800~1200 | 800~1200 | 800~1200 | 800~1200 | 800~1200 | 300~500 |
| High-temperature behavior | Preferably | Preferably | Preferably | Preferably | Preferably | Preferably | Typically |
| Cryogenic property | Preferably | Preferably | Preferably | Preferably | Preferably | Preferably | Preferably |
| Security performance | Preferably | Preferably | Preferably | Preferably | Preferably | Preferably | Typically |
| Cost | It is relatively low | It is relatively low | It is relatively low | It is relatively low | It is relatively low | It is relatively low | It is relatively low |
Claims (9)
1. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material, is characterized in by nanometer fibrous oxygen
Change zinc to be modified lithium vanadate, structural stability, high-rate discharge ability and the electron mobility of material are improved, sintered
Suction ripple rate in journey due to two kinds of materials is different, internal stress increase, occurs more micropore, crackle after annealing, increase Li from
Sub- deintercalation passage；Its prepare the step of be：
（1）The preparation of vanadium system presoma：Vanadic anhydride is weighed, 4 ~ 6h is heated to reflux in organic alcohol solvent, is cooled to room temperature
After add phosphoric acid, continue to be heated to reflux 6 ~ 8h, through cooling down, filtering and wash, at 80 ~ 100 DEG C be dried in vacuo 20 ~ 24h, obtain
Vanadium system presoma；
（2）The preparation of lithium system presoma：It is 10% or so that excess phosphoric acid is diluted into mass concentration, adds iron plate and simultaneously heats up, and is treated anti-
When should be 2 ~ 4 to solution ph, stop heating and add hydrogen peroxide, produce a large amount of ferric phosphate precipitations, divided after standing clarification
From, and 10 ~ 15h of drying precipitate is obtained being dehydrated phosphoric acid iron powder at 180 ~ 220 DEG C；By phosphoric acid iron powder and polyethylene
Alcohol is well mixed, and is heated to 550 ~ 650 DEG C under nitrogen protection, polyvinyl alcohol obtains amorphous ferric phosphate after decomposing；Add lithium
Source and carbon source, it is well mixed, is heated to 700 ~ 800 DEG C and continues 8 ~ 12h of calcining, lithium system presoma is made；
（3）Nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma are sufficiently mixed uniformly in ball mill；It is placed in just
In beautiful crucible, be put into micro-wave oven and carry out heating and calcining, wherein microwave power be 400 ~ 600W, microwave frequency for 2000 ~
3000MHz, reaction time are 3 ~ 5min, and zinc oxide/lithium vanadate composite is made.
2. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（1）The Organic Alcohol is at least one of isopropanol, glycerine, isobutanol or phenmethylol.
3. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（1）In backflow system, each material forms by weight is：20 ~ 30 parts of vanadic anhydride, 50 ~ 68 parts of Organic Alcohol,
2 ~ 20 parts of phosphatase 11.
4. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（2）The polyvinyl alcohol is pure to analyze, and number-average molecular weight is 5000 ~ 10000, and alcoholysis degree is 78 ~ 88%, vitrifying
Temperature is 75 ~ 80 DEG C；The lithium source is lithium hydroxide or lithium carbonate；The carbon source is in sucrose, starch, fructose or glucose
It is at least one；In preparation process, each material forms by weight is：32 ~ 53 parts of phosphoric acid iron powder, 5 ~ 10 parts of polyvinyl alcohol, lithium
30 ~ 40 parts of source, 12 ~ 18 parts of carbon source.
5. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（3）The nanometer fibrous zinc oxide, length are 5-10 μm, and diameter of section is 5 ~ 50nm.
6. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（3）The parts by weight of nanometer fibrous zinc oxide, vanadium system presoma and lithium system presoma form：Vanadium system presoma
73 ~ 86 parts, 10 ~ 15 parts of lithium system presoma, 4 ~ 12 parts of nanometer fibrous zinc oxide.
7. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：Step（3）The ball mill is in conical ball mill, ultra-fine lamination ball mill, ceramic ball mill or grate ball mill
One kind.
8. a kind of lithium battery preparation method of zinc oxide/lithium vanadate anode material according to claim 1, its feature
It is：The microwave heating and calcining is carried out under excess oxygen, is passed through the oxygen-enriched air that oxygen content is 26 ~ 30%.
9. a kind of lithium battery zinc oxide/lithium vanadate anode material, is prepared into by any one of claim 1-8 methods described
Arrive.
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