CN103715461A - Preparation method of flexible lithium-ion battery and reticular lithium titanate electrode structure - Google Patents
Preparation method of flexible lithium-ion battery and reticular lithium titanate electrode structure Download PDFInfo
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- CN103715461A CN103715461A CN201310722472.3A CN201310722472A CN103715461A CN 103715461 A CN103715461 A CN 103715461A CN 201310722472 A CN201310722472 A CN 201310722472A CN 103715461 A CN103715461 A CN 103715461A
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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
- H01M10/058—Construction or manufacture
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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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- 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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a preparation method of a flexible lithium-ion battery and a reticular lithium titanate electrode structure. The preparation method of the flexible lithium-ion battery comprises the following steps: growing reticular lithium titanate on a titanium sheet so as to serve as a negative electrode material; and preparing a nanorod coated with lithium manganate so as to serve as a positive electrode material, superimposing the negative electrode material, a lithium battery diaphragm and the positive electrode material in a sandwiched manner, and putting between two layers of PDMS (Polydimethylsiloxane) thin films for encapsulation so as to complete the preparation of the flexible lithium-ion battery. The invention discloses the lithium titanate adopting a reticular structure in the flexible lithium-ion battery; the advantages of a one-dimensional structure and the three-dimensional reticular structure can be fully utilized so as to enlarge the contact area of an active material and electrolyte. The flexible lithium-ion battery disclosed by the invention has very high stability at a bending state, so that dozens of charge-discharge cycles are realized.
Description
Technical field
The invention belongs to energy storage of new generation field, be specifically related to the synthetic of lithium titanate network nano structure and take lithium titanate as negative material, the LiMn2O4 flexible lithium ion battery that is positive electrode and the preparation method of network-like lithium titanate electrode structure.
Background technology
Along with the development of flexible electronic, flexible electronic device has become the market focus that each major company vies each other.Samsung, the LG company crooked display screen that released one after another.In August, 2013, Technology of Flexibility Yi Bei western medium is chosen as the whole world one of ten large Progress & New Products in 2013.October 2 this year and 8 days, LG company successively announced successful volume production flexible display screen and flexible lithium ion battery, and had released curved surface smart mobile phone G Flex October 29, became the mobile phone of first use flexible battery in the world.Flexible electronic product has been come into our life as can be seen here, and is no longer fancy.Be accompanied by the rise in flexible electronic product market, its must supply-lithium ion battery, also must, towards the future development of flexibility, meandering, believe that flexible lithium ion battery will become an emerging market pet.Yet, be engaged in the businesses and institutions of the research and development of flexible lithium ion battery very few.In existing flexible lithium ion battery, do not accomplish long-life and the high magnification of battery yet, this practical application to flexible lithium ion battery has very large obstruction.Therefore, exploitation long-life, powerful flexible lithium ion battery is extremely urgent.
Summary of the invention
The object of the present invention is to provide the preparation method of the lithium ion battery of a kind of network-like lithium titanate electrode structure and flexibility.The netted lithium titanate that adopts synthesized is as negative material, synthetic LiMn2O4 nanometer rods as positive electrode, and lithium hexafluoro phosphate is electrolyte, prepares a kind of lithium ion battery of high flexibility.
The preparation method who the present invention proposes a kind of flexible lithium ion battery, the method comprises:
Step 101, the network-like lithium titanate of growing on titanium sheet are as negative material;
Step 102, making apply LiMn2O4 nanometer rods, as positive electrode;
Step 103, described negative material, lithium battery diaphragm and positive electrode are superimposed with sandwich-like, and encapsulate in the middle of being placed in two-layer polydimethylsiloxane film, complete the preparation of flexible lithium ion battery.
The preparation method who the invention allows for a kind of network-like lithium titanate electrode structure, it comprises:
Step 201: titanium sheet is successively respectively cleaned one time in deionized water, acetone, alcohol;
Step 202: prepare a certain amount of NaOH solution;
Step 203: the NaOH solution preparing is placed in to autoclave, and cleaned titanium sheet is placed in one;
Step 204: the product of gained is placed in to HCl solution, places a period of time;
Step 205: products therefrom is placed in to the solution in LiOH, reacts a period of time under uniform temperature;
Step 206: under nitrogen protection, calcining certain hour, prepares network-like lithium titanate material by above-mentioned product.
The present invention has following beneficial effect:
A., shortcoming that high rate performance poor short for current cycle life of lithium ion battery, prepared network-like lithium titanate electrode structure, cycle life can reach 5000 times, and not decay of performance; Under the high magnification of 80C, battery still keeps the high power capacity of 103mAg/g, has realized lithium battery high magnification characteristic simultaneously.
B. the flexible lithium ion battery of made still keeps high stability under case of bending, and after circulation 70 times, battery capacity is not decay almost, can solve the problem of current flexible lithium battery capacity attenuation under bending state.
C. prepared flexible lithium ion battery has very excellent high rate performance, can circulate lower realization of large electric current (20C), and have very high stability, can realize the demand of electronic product to fast charging and discharging.
D. this flexible lithium ion battery can be realized the voltage platform of 2.5V, meets the demand of some electronic products to cell voltage.
E. this flexible lithium ion battery making is simple, cost compare is low, profit and popularization.
In addition, the present invention adopts the lithium titanate electrode of hydro thermal method network-like mechanism of direct growth on titanium sheet, compare with traditional electrode preparation method, this structure being grown directly upon in conductive substrates does not need to add binding agent, can effectively increase the electric transmission between active material and collector electrode.And this network-like structure has nano wire assembling to form, can give full play to the advantage of one-dimensional nano structure and three-dimensional net structure, increase active material and electrolytical contact area, increase the transmission of lithium ion and transporting of electronics, to improving capacity and the high rate performance of lithium ion battery, have very great help.
Accompanying drawing explanation
Fig. 1 is flexible battery preparation method flow chart in the present invention;
Fig. 2 is lithium titanate electrode material synthetic schemes in the present invention;
Fig. 3 is that the present invention that utilizes who takes is grown in the lithium titanate scanning electron microscope diagram of the network-like structure on titanium sheet;
Fig. 4 is LiMn2O4 nanometer rods synthetic schemes in the present invention;
Fig. 5 is the scanning electron microscope diagram that utilizes the LiMn2O4 nanometer rods that the present invention grows;
Fig. 6 is flexible battery encapsulation flow chart in the present invention;
Fig. 7 is the long-life test result of lithium titanate half-cell in the present invention;
Fig. 8 utilizes the circulation of the prepared flexible lithium battery of the present invention to characterize;
Fig. 9 is the graph of a relation of flexible lithium battery voltage and capacity in the present invention.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in further detail.
Fig. 1 shows preparation method's flow chart of a kind of flexible lithium ion battery of the present invention's proposition.As shown in Figure 1, the method comprises:
Step 101, the network-like lithium titanate of growing on titanium sheet are as negative material;
Step 102, making apply LiMn2O4 nanometer rods, as positive electrode;
Step 103, described negative material, lithium battery diaphragm and positive electrode are superimposed with sandwich-like, and encapsulate in the middle of being placed in two-layer polydimethylsiloxane film, complete the preparation of flexible lithium ion battery.
Fig. 2 shows preparation method's flow chart of the network-like lithium titanate of growing on titanium sheet of the present invention's proposition.As shown in Figure 2, the method comprises:
Step 201: titanium sheet is successively respectively cleaned one time in deionized water, acetone, alcohol, and described scavenging period can be 30 minutes;
Step 202: prepare a certain amount of NaOH solution, its concentration can be 1 mol/L, and its capacity can be 40 milliliters;
Step 203: the NaOH solution preparing is placed in to autoclave, and cleaned titanium sheet is placed in one, react a period of time at a certain temperature; Described uniform temperature can be 220 degrees Celsius, and the reaction time can be 16 hours;
Step 204: the product of gained is placed in to HCl solution, places a period of time, described HCl solution concentration can be 0.5 mol/L, and can be 1 hour standing time;
Step 205: products therefrom is placed in to the solution in LiOH, reacts one end time under uniform temperature, the concentration of described LiOH solution is 2 mol/L, reaction temperature can be 60 degrees Celsius, the reaction time can be 8 hours;
Step 206: above-mentioned product, under nitrogen protection, is calcined to certain hour, and described calcining heat can be 600 degrees Celsius, and calcination time can be 1.5 hours.The present invention that utilizes that Fig. 3 shows shooting is grown in the lithium titanate scanning electron microscope diagram of the network-like structure on titanium sheet.
Wherein, prepared network-like lithium titanate structure has one-dimensional nano line to assemble, and the length of nano wire, diameter etc. can be regulated and controled by the combined factors such as temperature of the time of reacting, reaction.
Fig. 4 shows preparation method's flow chart of LiMn2O4 nanometer rods in the present invention.As shown in Figure 4, the method comprises:
Step 401: manganese sulfate and potassium chlorate are dissolved in deionized water, stir a period of time, the ratio of wherein said manganese sulfate, potassium chlorate and deionized water is: manganese sulfate is 0.338g, and potassium chlorate is 0.246g, deionized water is 25mL, and mixing time is chosen as 30 minutes;
Step 402: above-mentioned solution is placed in to autoclave and reacts, obtain manganese dioxide nano-rod, reaction temperature is chosen as 200 degrees Celsius, and the reaction time is chosen as 12 hours;
Step 403: prepared manganese dioxide nano-rod is fully mixed with certain proportion with lithium hydroxide in alcoholic solution and be dried, described ratio can be that mol ratio is the relation of 2: 1;
Step 404: the product after dry is reacted to certain hour in air, obtain LiMn2O4 nanometer rods, described reaction temperature can be 750 degrees Celsius, and the reaction time can be 10 hours.Fig. 5 shows the scanning electron microscope diagram that utilizes the LiMn2O4 nanometer rods that the present invention grows.
Fig. 6 shows the method for packing flow chart of the flexible lithium battery of the present invention's proposition.As shown in Figure 6, it comprises:
Step 601: after silicon rubber is mixed with certain proportion with curing agent, in refrigerator, place an a period of time, it is 10: 1 that described certain proportion can be mass ratio, standing time can 2 hours, remove afterwards bubble wherein, then baking oven in dry, described baking temperature can be 50 degrees Celsius, drying time can 3 hours;
Step 602: by the method for filming, LiMn2O4 is coated on flexible stainless (steel) wire, is dried, described baking temperature can be 80 degrees Celsius, can be 12 hours drying time;
Step 603: lithium titanate, barrier film and LiMn2O4 are stacked with sandwich-like, be placed on ready PDMS film, drip after electrolyte, with another PDMS thin film thereon;
Step 604: with uncured PDMS, surrounding's encapsulation of above-mentioned assembled battery is tight, and dry in vacuum drying chamber, baking temperature can be 50 degrees Celsius and is dried.
The present invention is long-life and high magnification research and the application on flexible lithium ion battery thereof of the lithium titanate electrode of network-like structure.Mainly comprise the preparation of network-like lithium titanate electrode, the making of the synthetic and flexible lithium ion battery of manganate cathode material for lithium etc.
Fig. 7 is the long-life test result of lithium titanate half-cell in the present invention.As shown in Figure 7, utilize the prepared network-like lithium titanate electrode structure of the present invention, cycle life can reach 5000 times, and not decay of performance.
Fig. 8 utilizes the circulation of the prepared flexible lithium battery of the present invention to characterize.As shown in Figure 8, utilize the flexible lithium ion battery of made of the present invention under case of bending, still to keep high stability, after circulation 70 times, battery capacity is not decay almost.And prepared flexible lithium ion battery has very excellent high rate performance, can realize circulation large electric current (20C) is lower, and there is very high stability.
Fig. 9 is the graph of a relation of flexible lithium battery voltage and capacity in the present invention.As shown in Figure 9, utilize flexible lithium ion battery that the present invention makes can realize the voltage platform of 2.5V, meet the demand of some electronic products to cell voltage.
Netted lithium titanate chemical property and flexible lithium ion battery high rate capability about synthesized, be specially: netted lithium titanate electrode structure discharges and recharges under 2C and 20C multiplying power, after circulation 5000 times, battery capacity still keeps good stability, has showed excellent long circulation life.While discharging and recharging, still keep the high power capacity of 103mAh/g under the current density of 80C, showed outstanding high rate capability.When the flexible lithium ion battery of assembling is tested simultaneously under the current density of 20C, circulate 70 times, capacity is decay not, remains on 120mAh/g, compares with the flexible lithium ion battery of having researched and developed at present, has higher high rate performance.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a preparation method for flexible lithium ion battery, the method comprises:
Step 101, the network-like lithium titanate of growing on titanium sheet are as negative material;
Step 102, making apply LiMn2O4 nanometer rods, as positive electrode;
Step 103, described negative material, lithium battery diaphragm and positive electrode are superimposed with sandwich-like, and encapsulate in the middle of being placed in two-layer polydimethylsiloxane film, complete the preparation of flexible lithium ion battery.
2. the method for claim 1, wherein step 101 comprises:
Step 201: titanium sheet is successively respectively cleaned one time in deionized water, acetone, alcohol;
Step 202: prepare a certain amount of NaOH solution;
Step 203: the NaOH solution preparing is placed in to autoclave, and cleaned titanium sheet is placed in one, react a period of time under uniform temperature;
Step 204: the product of gained is placed in to HCl solution, places a period of time;
Step 205: products therefrom is placed in to the solution in LiOH, reacts a period of time under uniform temperature;
Step 206: under nitrogen protection, calcining certain hour, prepares network-like lithium titanate material by above-mentioned product.
3. method as claimed in claim 2, wherein, described network-like lithium titanate material is assembled by one-dimensional nano line, and the attribute of nano wire regulates and controls by growth parameter(s).
4. the method for claim 1, wherein described step 102 specifically comprises:
Step 301: manganese sulfate and potassium chlorate are dissolved in deionized water, stir a period of time;
Step 302: above-mentioned solution is placed in to autoclave and reacts, obtain manganese dioxide nano-rod;
Step 303: prepared manganese dioxide nano-rod is fully mixed with certain proportion with lithium hydroxide in alcoholic solution and be dried;
Step 304: the product after dry is calcined to certain hour in air, obtain LiMn2O4 nanometer rods.
5. the method for claim 1, wherein described step 103 specifically comprises:
Step 401: silicon rubber and curing agent are mixed rear cooling with certain proportion, then solidify at 50 ℃, form PDMS film;
Step 402: by the method for filming, LiMn2O4 is coated on flexible stainless (steel) wire, is dried;
Step 403: described network-like lithium titanate, lithium battery diaphragm and the LiMn2O4 that is coated on flexible stainless (steel) wire are stacked with sandwich-like, be placed on PDMS film, drip after electrolyte,, form battery assembling structure with another PDMS thin film thereon;
Step 404: with uncured PDMS, surrounding's encapsulation of above-mentioned battery assembling structure is tight, and dry in vacuum drying chamber, complete the preparation of flexible lithium battery.
6. method as claimed in claim 2, wherein in step 201, the scavenging period of titanium sheet is respectively 30 minutes, in step 202, the concentration of NaOH solution is 1 mol/L; Reaction temperature in step 203 is 220 degrees Celsius, 16 hours time; In step 204, HCl concentration is 0.5 mol/L; In step 205, LiOH concentration is 2 mol/L.
7. method as claimed in claim 4, the reaction temperature of step 302 is 200 degrees Celsius, the reaction time is 12 hours; In step 303, the mol ratio of manganese dioxide and lithium hydroxide is 2: 1; Reaction temperature in step 304 is 750 degrees Celsius, and the reaction time is 10 hours.
8. a preparation method for network-like lithium titanate electrode structure, it comprises:
Step 101: titanium sheet is successively respectively cleaned one time in deionized water, acetone, alcohol;
Step 102: prepare a certain amount of NaOH solution;
Step 103: the NaOH solution preparing is placed in to autoclave, and cleaned titanium sheet is placed in one, react a period of time at a certain temperature;
Step 104: the product of gained is placed in to HCl solution, places a period of time;
Step 105: products therefrom is placed in to the solution in LiOH, reacts a period of time under uniform temperature;
Step 106: under nitrogen protection, calcining certain hour, prepares network-like lithium titanate material by above-mentioned product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826558A (en) * | 2016-05-09 | 2016-08-03 | 复旦大学 | Flexible wearable water system lithium ion battery |
| CN106684114A (en) * | 2017-01-04 | 2017-05-17 | 武汉华星光电技术有限公司 | Flexible display device and method of manufacturing same |
| CN110335982A (en) * | 2019-07-28 | 2019-10-15 | 电子科技大学 | A kind of micro-nano integrated Solid State film lithium cell and preparation method thereof |
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| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
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Patent Citations (1)
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| CN102544574A (en) * | 2011-12-30 | 2012-07-04 | 华中科技大学 | Flexible lithium ion battery and packaging method thereof |
Non-Patent Citations (2)
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| LAIFA SHEN，ET AL: "Hydrogenated Li 4 Ti 5 O 12 Nanowire Arrays for High Rate Lithium Ion Batteries", 《ADVANCED MATERIALS》, vol. 24, 5 October 2012 (2012-10-05), pages 6502 - 6506 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105826558A (en) * | 2016-05-09 | 2016-08-03 | 复旦大学 | Flexible wearable water system lithium ion battery |
| CN106684114A (en) * | 2017-01-04 | 2017-05-17 | 武汉华星光电技术有限公司 | Flexible display device and method of manufacturing same |
| CN106684114B (en) * | 2017-01-04 | 2019-10-18 | 武汉华星光电技术有限公司 | Flexible display device and preparation method thereof |
| CN110335982A (en) * | 2019-07-28 | 2019-10-15 | 电子科技大学 | A kind of micro-nano integrated Solid State film lithium cell and preparation method thereof |
| CN110335982B (en) * | 2019-07-28 | 2021-04-27 | 电子科技大学 | Micro-nano integrated solid film lithium battery and preparation method thereof |
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