CN106972152A - Lithium ion cell electrode preparation and the assemble method of battery - Google Patents
Lithium ion cell electrode preparation and the assemble method of battery Download PDFInfo
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- CN106972152A CN106972152A CN201710222947.0A CN201710222947A CN106972152A CN 106972152 A CN106972152 A CN 106972152A CN 201710222947 A CN201710222947 A CN 201710222947A CN 106972152 A CN106972152 A CN 106972152A
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- lithium ion
- ion cell
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- 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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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- 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
Prepared the invention provides a kind of lithium ion cell electrode and battery assemble method, including microwave synthesis, to synthesize Fe2O3Nano material is electrode activity thing, selection conductive agent and binding agent, is proportionally added into after N methyl pyrrolidone solvents, slurry is obtained by ground and mixed；Slurry is coated on copper foil of affluxion body, then at vacuum drying, solvent and moisture is removed, and is compacted, makes to contact close between electrode powder；Negative pole disk is struck out, prepares battery assembling after being dried in vacuum drying chamber.Lithium ion cell electrode preparation and the assemble method of battery that the present invention is provided, the lithium ion cell electrode capacitance characteristic prepared substantially, conduct electricity very well, the method increase the utilization rate of electrode material, so as to improve the capacity of material.
Description
Technical field
The present invention relates to a kind of preparation of lithium ion cell electrode and the assemble method of battery, belong to nano material and prepare neck
Domain.
Background technology
Iron oxide nano material due to its excellent performance be widely used in catalyst, energy storage and converting apparatus,
In terms of magnetic material, water pollution processing, gas sensitive, pigment.And ultracapacitor has power density height, charge/discharge rates
Hurry up, good cycling stability, long lifespan the advantages of, be increasingly subject to everybody concern as a kind of new energy storage device.It is herein
On the basis of iron oxide nano material present Research, main to attempt using synthesizing means such as liquid-phase precipitation methods, controllable preparation is closed
Into a variety of iron oxide nano materials, such as one-dimensional nano structure, hollow structure, polyhedral structure utilize X-ray diffraction
(XRD), SEM (SEM), field emission scanning electron microscope (FE-SEM), transmission electron microscope（TEM）, ratio
Surface Tester（BET）The microscopic appearance and structure of material are characterized Deng Modern Testing, respectively with obtained oxidation
Ferrum nano material is assembled into test device as ultracapacitor and lithium ion battery electrode material, uses cyclic voltammetric, exchange
Impedance, the constant current charge-discharge Study on Test Method chemical property of material, have obtained good test result.
As a kind of novel energy storage apparatus, ultracapacitor has that power output is high, the charging interval is short, operating temperature range
Width, service life length, it is safe and pollution-free the advantages of, be expected to turn into this century new green power supply.Conventional at present is used for
Electrode material for super capacitor includes carbon material, metal oxide materials, conducting polymer materials etc., but these materials due to
Some intrinsic problems, cause the electrode material specific capacity prepared relatively low, this certainly will have to the overall performance of capacitor
Very big influence
The content of the invention
In view of in place of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of preparation of lithium ion cell electrode
And the assemble method of battery.
The invention aims to overcome the shortcomings of the material of traditional preparation methods preparation, there is provided a kind of lithium-ion electric
Pond electrode preparation and the assemble method of battery.In order to achieve the above object, this invention takes following technical scheme：
The invention provides a kind of preparation of lithium ion cell electrode and the assemble method of battery, comprise the following steps：
Step 1: microwave is synthesized, respectively by Fe (NO3)3·9H2O and KOH dissolvings are in deionized water；By mixed solution after stirring
It is transferred in microwave reaction instrument and reacts；Gained pelleting centrifugation is come out after natural cooling, cyclic washing；Huang is obtained after vacuum drying
The product of green is alpha-feooh；By product heating and then natural cooling, red product is finally obtained for α-Fe2O3；
Step 2: to synthesize Fe2O3 nano materials as electrode activity thing, selection conductive agent and binding agent are proportionally added into N- first
After base pyrrolidinone solvent, slurry is obtained by ground and mixed；
Step 3: slurry is coated on copper foil of affluxion body, then at vacuum drying, solvent and moisture are removed, and is compacted, makes electrode
Contacted between powder close；
Step 4: striking out negative pole disk, prepare battery assembling after being dried in vacuum drying chamber.
It is preferred that, above-mentioned steps one are specifically included：
Step 1.1, respectively by Fe (NO3)3·9H2O and KOH dissolvings are in deionized water；
Step 1.2, by KOH solution be added dropwise to stirring in Fe (NO3)3·9H2In O solution；
After stirring, mixed solution is transferred in three-necked flask into mixed solution for step 1.3 plus deionized water；
Step 1.4, the three-necked flask for filling solution react in microwave reaction instrument；
Step 1.5, reaction treat that flask naturally cools to room temperature after terminating, and gained pelleting centrifugation are come out, with absolute ethyl alcohol and steaming
Distilled water cyclic washing, to remove the reagent that unreacted is complete；
Step 1.6, washed precipitation is dried in vacuo, the product for obtaining yellow green is alpha-feooh；
Step 1.7, product is then placed in Muffle furnace, is warming up to 350 °C of holdings, then naturally cools to room temperature, finally obtain
It is α-Fe to dry loose red product2O3。
It is preferred that, respectively by 0.02mol Fe (NO in above-mentioned steps 1.13)3·9H2O and 0.02mol KOH are dissolved in
In 20ml deionized waters.
It is preferred that, add 30ml deionized waters into mixed solution in above-mentioned steps 1.3, after stirring 10 minutes, will mix molten
Liquid is transferred in three-necked flask.
It is preferred that, in the three-necked flask for filling solution 1 is reacted in 90 °C of microwave reaction instrument in above-mentioned steps 1.4 small
When.
It is preferred that, conductive agent is carbon black in above-mentioned steps two, and binding agent is Kynoar, is 75 according to mass ratio:20:
5 proportioning electrode activity things, conductive agent and binding agent.
It is preferred that, above-mentioned steps three are specially that slurry is coated on copper foil of affluxion body, and 8 are dried in vacuo at 120 DEG C
~ 10 hours, solvent and moisture are removed, and in being compacted under 8 ~ 12MPa pressure, make to contact close between electrode powder.
It is preferred that, above-mentioned steps four are specially the negative pole disk for striking out a diameter of 10 mm sizes, in vacuum drying chamber
Prepare battery assembling after drying 8-10 hours.
It is preferred that, above-mentioned battery is assembled in the dry glove box full of argon gas.
Lithium ion cell electrode preparation and the assemble method of battery that the present invention is provided, the lithium ion cell electrode prepared
Capacitance characteristic substantially, conducts electricity very well, the method increase the utilization rate of electrode material, so as to improve the capacity of material.
Brief description of the drawings
Cyclic voltammetry curve under the alpha-feooh different scanning rates that Fig. 1 is prepared for the present invention is without PVP schematic diagrames.
Cyclic voltammetry curve under the alpha-feooh different scanning rates that Fig. 2 is prepared for the present invention adds PVP schematic diagrames.
Embodiment
The present invention provides the assemble method of a kind of lithium ion cell electrode preparation and battery, to make the purpose of the present invention, skill
Art scheme and effect are clearer, clear and definite, and the present invention is described in more detail for the embodiment that develops simultaneously referring to the drawings.It should manage
Solution, specific embodiment described herein only to explain the present invention, is not intended to limit the present invention.
Lithium ion cell electrode preparation and the assemble method of battery that the present embodiment is provided, specifically include following steps：
Microwave is synthesized, first respectively by 0.02mol Fe (NO3)3·9H2O and 0.02mol KOH are dissolved in 20ml deionized waters
In.Then KOH solution is added dropwise to the Fe (NO in stirring3)3·9H2In O solution.Plus 30ml deionized waters are into mixed solution,
After stirring 10 minutes, mixed solution is transferred in three-necked flask.Fill microwave reaction instrument of the three-necked flask of solution at 90 °C
Middle reaction 1 hour.Reaction treats that flask naturally cools to room temperature after terminating, and gained pelleting centrifugation is come out, with absolute ethyl alcohol and steaming
Distilled water cyclic washing, to remove the reagent that unreacted is complete.Washed being deposited under 60 °C is dried in vacuo 8h, yellow green is obtained
Product is alpha-feooh.Product is then placed in Muffle furnace, 350 °C is warming up to and is kept for 3 hours, then naturally cool to room temperature, most
Obtain drying loose red product afterwards for α-Fe2O3。
To synthesize Fe2O3 nano materials as electrode activity thing, carbon black is conductive agent, Kynoar（PVDF）For bonding
Agent, in proportion（Mass ratio is 75:20:5）Add 1-METHYLPYRROLIDONE（NMP）After solvent, slurry is obtained by ground and mixed.
Slurry is coated on copper foil of affluxion body, is dried in vacuo 8 ~ 10 hours at 120 DEG C, solvent and moisture is removed, and in 8 ~
It is compacted under 12MPa pressure, makes to contact close between electrode powder.The negative pole disk of a diameter of 10 mm sizes is struck out again, true
Prepare battery assembling after being dried 8-10 hours in empty drying box.Battery is assembled in the dry glove box full of argon gas.Survey
Try battery and use CR2025 button cells, positive pole uses metal lithium sheet, and barrier film uses the films of Celgard 2325, and electrolyte is 1 M
LiPF6 EC：DMC= 1:1 （Volume ratio）Electrolyte.
Cyclic voltammetry is a kind of common method of Electrode electrochemical behavior in electrolyte system.Utilize circulation volt
Peace method can test electrode material for super capacitor in charge and discharge process electric current with charging/discharging voltage situation of change.It is tested
Principle is：The periodic scan electric potential signal of one linear change of electrode is applied to, by detecting the current-responsive value in circuit,
The information for the electrode case that experiment needs is obtained from gained collection of illustrative plates.As the invertibity of electrode, charge-discharge performance, analysis oxygen characteristic,
Characteristic of electrode material and electrolyte ion exchange charge etc..
Fig. 1 and 2 is the cyclic voltammetry curve figure for the alpha-feooh material for being not added with PVP and adding PVP respectively, and it scans speed
Rate is from 5 mVs-1Increase to 100 mVs-1, scanning voltage scope is -0.01-0.8V.It can be seen that two kinds
The cyclic voltammetry curve figure difference of material is simultaneously little, and respective CV curves have a pair of obvious redox peaks, rather than present
Go out the shape of class rectangle, illustrate that this is obvious Faraday pseudo-capacitance, rather than electric double layer capacitance.With the increasing of sweep speed
Plus, voltage difference is increasing between oxidation peak and reduction peak, and this explanation is with the increase of sweep speed, and reaction difficulty is increasingly
Greatly, mainly due to caused by polarization of electrode.
Lithium ion cell electrode preparation and the assemble method of battery that the present invention is provided, the lithium ion cell electrode electric capacity prepared
Characteristic substantially, conducts electricity very well, the method increase the utilization rate of electrode material, so as to improve the capacity of material.
It is understood that for those of ordinary skills, can be with technique according to the invention scheme and its invention structure
Think of is subject to equivalent substitution or change, and all these changes or replacement should all belong to the protection model of appended claims of the invention
Enclose.
Claims (9)
1. a kind of lithium ion cell electrode preparation and the assemble method of battery, it is characterised in that：It the described method comprises the following steps：
Step 1: microwave is synthesized, respectively by Fe (NO3)3·9H2O and KOH dissolvings are in deionized water；By mixed solution after stirring
It is transferred in microwave reaction instrument and reacts；Gained pelleting centrifugation is come out after natural cooling, cyclic washing；Huang is obtained after vacuum drying
The product of green is alpha-feooh；By product heating and then natural cooling, red product is finally obtained for α-Fe2O3；
Step 2: to synthesize Fe2O3 nano materials as electrode activity thing, selection conductive agent and binding agent are proportionally added into N- first
After base pyrrolidinone solvent, slurry is obtained by ground and mixed；
Step 3: slurry is coated on copper foil of affluxion body, then at vacuum drying, solvent and moisture are removed, and is compacted, makes electrode
Contacted between powder close；
Step 4: striking out negative pole disk, prepare battery assembling after being dried in vacuum drying chamber.
2. lithium ion cell electrode preparation as claimed in claim 1 and the assemble method of battery, it is characterised in that：The step
One specifically includes：
Step 1.1, respectively by Fe (NO3)3·9H2O and KOH dissolvings are in deionized water；
Step 1.2, by KOH solution be added dropwise to stirring in Fe (NO3)3·9H2In O solution；
After stirring, mixed solution is transferred in three-necked flask into mixed solution for step 1.3 plus deionized water；
Step 1.4, the three-necked flask for filling solution react in microwave reaction instrument；
Step 1.5, reaction treat that flask naturally cools to room temperature after terminating, and gained pelleting centrifugation are come out, with absolute ethyl alcohol and steaming
Distilled water cyclic washing, to remove the reagent that unreacted is complete；
Step 1.6, washed precipitation is dried in vacuo, the product for obtaining yellow green is alpha-feooh；
Step 1.7, product is then placed in Muffle furnace, is warming up to 350 °C of holdings, then naturally cools to room temperature, finally obtain
It is α-Fe to dry loose red product2O3。
3. lithium ion cell electrode preparation as claimed in claim 2 and the assemble method of battery, it is characterised in that：The step
Respectively by 0.02mol Fe (NO in 1.13)3·9H2O and 0.02mol KOH are dissolved in 20ml deionized waters.
4. lithium ion cell electrode preparation as claimed in claim 2 and the assemble method of battery, it is characterised in that：The step
Add 30ml deionized waters into mixed solution in 1.3, after stirring 10 minutes, mixed solution is transferred in three-necked flask.
5. lithium ion cell electrode preparation as claimed in claim 2 and the assemble method of battery, it is characterised in that：The step
Reacted 1 hour in 90 °C of microwave reaction instrument in the three-necked flask for filling solution in 1.4.
6. lithium ion cell electrode preparation as claimed in claim 1 and the assemble method of battery, it is characterised in that：The step
Conductive agent is carbon black in two, and binding agent is Kynoar, is 75 according to mass ratio:20:5 proportioning electrode activity things, conductive agent
And binding agent.
7. lithium ion cell electrode preparation as claimed in claim 1 and the assemble method of battery, it is characterised in that：The step
Three be specially that slurry is coated on copper foil of affluxion body, is dried in vacuo 8 ~ 10 hours at 120 DEG C, removes solvent and moisture,
And in being compacted under 8 ~ 12MPa pressure, make to contact close between electrode powder.
8. lithium ion cell electrode preparation as claimed in claim 1 and the assemble method of battery, it is characterised in that：The step
Four be specially the negative pole disk for striking out a diameter of 10 mm sizes, and battery is prepared after being dried 8-10 hours in vacuum drying chamber
Assembling.
9. lithium ion cell electrode preparation as claimed in claim 8 and the assemble method of battery, it is characterised in that：The battery
Assembled in the dry glove box full of argon gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710222947.0A CN106972152A (en) | 2017-04-07 | 2017-04-07 | Lithium ion cell electrode preparation and the assemble method of battery |
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| CN201710222947.0A CN106972152A (en) | 2017-04-07 | 2017-04-07 | Lithium ion cell electrode preparation and the assemble method of battery |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950457A (en) * | 2017-12-21 | 2019-06-28 | 北京金羽新能科技有限公司 | A kind of water system ion energy storage device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475222A (en) * | 2009-01-22 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Iron oxide hollow microsphere and preparation thereof |
| CN103606672A (en) * | 2013-10-12 | 2014-02-26 | 安泰科技股份有限公司 | Rod-shaped nano iron oxide electrode material, and preparation method and application thereof |
-
2017
- 2017-04-07 CN CN201710222947.0A patent/CN106972152A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475222A (en) * | 2009-01-22 | 2009-07-08 | 中国科学院上海硅酸盐研究所 | Iron oxide hollow microsphere and preparation thereof |
| CN103606672A (en) * | 2013-10-12 | 2014-02-26 | 安泰科技股份有限公司 | Rod-shaped nano iron oxide electrode material, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郝迷花: ""α-Fe2O3 电极的制备"", 《新乡学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109950457A (en) * | 2017-12-21 | 2019-06-28 | 北京金羽新能科技有限公司 | A kind of water system ion energy storage device |
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Application publication date: 20170721 |