CN105261792B - The manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole - Google Patents
The manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole Download PDFInfo
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- CN105261792B CN105261792B CN201510427972.3A CN201510427972A CN105261792B CN 105261792 B CN105261792 B CN 105261792B CN 201510427972 A CN201510427972 A CN 201510427972A CN 105261792 B CN105261792 B CN 105261792B
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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
- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses the manufacture method of a kind of Si negative poles and the high-energy-density secondary lithium battery of rich lithium richness manganese positive pole, rich lithium richness manganese material molecular formula is xLi2MnO3·(1‑x)LiMO2Wherein M=Ni, Co, Mn, full GND are prepared in proportion by nano Si material and Super p carbon blacks and sodium alginate, and positive pole is mixed by rich lithium richness manganese material with PTFE and acetylene black, and rich lithium richness manganese material is then prepared by metal salt solution with NaOH solution co-precipitation, the full battery come is assembled using nano Si material and rich lithium richness manganese material has higher capacity and than energy, and average voltage is high, pollution-free.
Description
Technical field
The present invention relates to a kind of manufacture method of secondary lithium battery, more particularly to a kind of Si negative poles and rich lithium richness manganese are just
The manufacture method of the high-energy-density secondary lithium battery of pole.
Background technology
In the prior art, because lithium battery anode uses cobalt acid lithium, cost is higher, and the toxicity of cobalt is larger, to environment
Have a great influence；And existing lithium battery major part negative pole is smaller using graphite, graphite density, tap density is relatively low to cause battery
Volume is larger；It is too low that this results in lithium ion battery one side specific discharge capacity, energy density can not meet demand, on the other hand
Cobalt toxicity in lithium cobaltate cathode is larger, and environmental pollution is larger and expensive.
In order to solve the storage problem of the energy, countries in the world all generate greatly emerging to Large Copacity chemistry energy storage material
Interest, especially with the continuous development of electronic technology, various portable digital product continuing to bring out such as blowout, and to make
Electronic product small volume and less weight is easy to carry and cruising time is grown, and this requires that the electrochmical power source small volume specific capacity provisioned in it is big
And stability is good safe.At present with LiCoO2It is respectively the lithium rechargeable battery of positive pole and negative material with graphite, by
It is relatively low in its energy density and specific capacity, it is increasingly difficult to meet portable set and pure electric automobile to the energy content of battery
The demand of density.
Rich lithium richness manganese anode material xLi2MnO3·(1-x)LiMO2Relative to other LiCoO2、LiMn2O4、LiFePO4、
LiNi1/3Co1/3Mn1/3O2Deng for positive electrode because it has higher specific capacity (200~300mAh g-1) less expensive
The advantages that production cost and new charge discharge mechanism and be considered as the preferable positive pole material of lithium ion battery of future generation
Material.
For negative material, Si negative materials have 3000mAh g-1High specific capacity above, is ideal
Negative material, but Volume Changes more seriously cause the material circulation during discharge and recharge due to Si negative materials
Can be poor.Tension force et al. uses nano Si as negative pole raw material, the Si negative poles of painting film preparation using sodium alginate as binding agent
Material preferably resolves the circulation sex chromosome mosaicism of Si materials so that Si materials applications are possibly realized in lithium ion battery.Si is born
The capacity of pole material is ten times of graphite cathode or so so that will have larger ratio using with the lithium rechargeable battery of Si negative poles
Capacity.
In view of above-mentioned content, the design people, actively it is subject to research and innovation, it is rich to found a kind of Si negative poles and rich lithium
The manufacture method of the high-energy-density secondary lithium battery of manganese positive pole, make it with more the value in industry.
The content of the invention
In order to solve the above technical problems, it can be manufactured with higher capacity and than energy it is an object of the invention to provide a kind of
The manufacture method of amount, the Si negative poles for the features such as average voltage is high and the high-energy-density secondary lithium battery of rich lithium richness manganese positive pole.
The manufacturer of the high-energy-density secondary lithium battery of a kind of Si negative poles proposed by the present invention and rich lithium richness manganese positive pole
Method, it is characterised in that：Comprise the following steps：
(1) mixed salt solution is prepared with the metal salt of nickel, cobalt and manganese；
(2) mixed salt solution obtained in step (1) is instilled under the conditions of 60 DEG C and filled in the reactor of ammoniacal liquor
Reaction a period of time, and sodium hydroxide control ph is used, obtain coprecipitated product after the completion of reaction；
(3) coprecipitated product obtained in step (2) is washed and filtered and be then well mixed with lithium carbonate, mixed
Thing；
(4) mixture obtained in step (3) is put into Muffle furnace, be calcined in air atmosphere to 750 DEG C~850 DEG C
Continue 10~12 hours, target product richness lithium richness manganese material is obtained after natural cooling；
(5) by the rich lithium richness manganese material obtained in step (4) and acetylene black and polytetrafluoroethylene (PTFE) (PTFE) with 85:10：5
Ratio is well mixed to be prepared into anode；
(6) by nano Si powder and sodium alginate and Super p carbon blacks with 60：20：20 ratio is well mixed to be prepared into
GND；
(7) anode obtained in step (5) is assembled into the GND obtained in step (6) in glove box
Full battery.
As the further improvement of the inventive method, the reaction time described in step (2) is 10~50 hours.
As the further improvement of the inventive method, pH value range described in step (2) is controlled between 9~11.
As the further improvement of the inventive method, the coprecipitated product described in step (3), molecular formula is M (OH)2,
Wherein M=Ni, Co, Mn.
As the further improvement of the inventive method, the target product richness lithium richness manganese material described in step (4) is
xLi2MnO3·(1-x)LiMO2Wherein M=Ni, Co, Mn；X ＜ 1.
As the further improvement of the inventive method, the just extremely rich lithium richness manganese material of the full battery described in step (7),
Molecular formula is xLi2MnO3·(1-x)LiMO2, wherein M=Ni, Co, Mn, negative pole is Si materials.
By such scheme, the present invention at least has advantages below：The present invention uses spherical rich lithium richness manganese material as electricity
Pond positive pole, negative pole of the nano Si material as battery, its Heterosis exist：On the one hand, rich lithium richness manganese material has tap density
Height ratio capacity is big and the features such as first circle efficiency high and good reversibility.On the other hand, nano Si material is relative to other negative pole materials
There is larger advantage in specific capacity, therefore assemble the lithium ion battery come using both materials there is specific volume for material
Amount is high, and average voltage is high, it is bigger than energy the advantages that.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 is the manufacture method flow of the high-energy-density secondary lithium battery of Si negative poles of the present invention and rich lithium richness manganese positive pole
Figure.
Fig. 2 is rich lithium richness manganese material electron microscope；
Fig. 3 is rich lithium richness manganese material XRD spectra；
Fig. 4 is rich lithium richness manganese material and Si material charge-discharge performance figures；
Fig. 5 is full battery charging and discharging performance map and 0.2C cycle performance figures.
Embodiment
With reference to the accompanying drawings and examples, the embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment one：A kind of manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole,
The step of this method, is as follows：
(1) mixed salt solution, concentration 2mol/L are prepared with the sulfate of nickel, cobalt and manganese；
(2) mixed salt solution obtained in step (1) is instilled under the conditions of 60 DEG C and fills the anti-of 1mol/L ammoniacal liquor
Answer in kettle and react 50 hours, and the use of sodium hydroxide control ph is 10, coprecipitated product is obtained after the completion of reaction；
(3) coprecipitated product obtained in step (2) is washed and filtered, be then well mixed, mixed with lithium carbonate
Compound；
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnaces, be calcined in air atmosphere to
750 DEG C~850 DEG C, continue 10~12 hours, target product richness lithium richness manganese material is obtained after natural cooling；
(5) by the rich lithium richness manganese material obtained in step (4) and acetylene black and PTFE with 85:10：5 ratio is well mixed
It is prepared into anode；
(6) by nano Si powder and sodium alginate and Super p carbon blacks with 60：20：20 ratio is well mixed to be prepared into
GND；
(7) anode obtained in step (5) is assembled into the GND obtained in step (6) in glove box
Full battery.
Embodiment two：A kind of manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole,
The step of this method, is as follows：
(1) mixed salt solution, concentration 1mol/L are prepared with the sulfate of nickel, cobalt and manganese；
(2) mixed salt solution obtained in step (1) is instilled under the conditions of 60 DEG C and fills the anti-of 1mol/L ammoniacal liquor
Answer in kettle and react 50 hours, and the use of sodium hydroxide control ph is 11, coprecipitated product is obtained after the completion of reaction；
(3) coprecipitated product obtained in step (2) is washed and filtered, be then well mixed, mixed with lithium carbonate
Compound；
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnaces, be calcined in air atmosphere to
750 DEG C~850 DEG C continue 10~12 hours, and target product richness lithium richness manganese material is obtained after natural cooling.
(5) by the rich lithium richness manganese material obtained in step (4) and acetylene black and PTFE with 85:10：5 ratio is well mixed
It is prepared into anode；
(6) by nano Si powder and sodium alginate and Super p carbon blacks with 60：20：20 ratio is well mixed to be prepared into
GND；
(7) anode obtained in step (5) is assembled into the GND obtained in step (6) in glove box
Full battery.
Embodiment three：A kind of manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole,
The step of this method, is as follows：
(1) mixed salt solution, concentration 2mol/L are prepared with the sulfate of nickel, cobalt and manganese；
(2) mixed salt solution obtained in step (1) is instilled under the conditions of 60 DEG C and fills the anti-of 1mol/L ammoniacal liquor
Answer in kettle and react 10 hours, and the use of sodium hydroxide control ph is 10, coprecipitated product is obtained after the completion of reaction；
(3) coprecipitated product obtained in step (2) is washed and filtered, be then well mixed, mixed with lithium carbonate
Compound；
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnaces, be calcined in air atmosphere to
750 DEG C~850 DEG C continue 10~12 hours, and target product richness lithium richness manganese material is obtained after natural cooling.
(5) by the rich lithium richness manganese material obtained in step (4) and acetylene black and PTFE with 85:10：5 ratio is well mixed
It is prepared into anode；
(6) by nano Si powder and sodium alginate and Super p carbon blacks with 60：20：20 ratio is well mixed to be prepared into
GND；
(7) anode obtained in step (5) is assembled into the GND obtained in step (6) in glove box
Full battery.
A kind of lithium ion battery can be produced by above three embodiment, the electrode reaction when lithium ion battery charges
It is as follows:
(1) negative reaction:x Li++Si+x e-→LixSi；
Positive electrode is with lithium ion (Li+) form be dissolved in organic electrolyte, electronics is supplied to wire.
(2) positive pole reacts:xLi2MnO3·(1-x)LiMO2→xMnO2·(1-x)MO2+(1+x)Li++x/2O2+(1+x)
e-；
Rich lithium richness manganese material is used in the present invention as positive pole, because cobalt content is less in rich lithium richness manganese material thus cost
It is relatively low, and rich lithium richness manganese material specific capacity is more than cobalt acid lithium, on the other hand, the specific capacity of Si negative materials is graphite cathode
Ten times or so of material, and density is more than graphite, so the lithium ion battery specific capacity produced using both materials is big, puts down
Equal operating voltage can reach 590Wh/Kg in 3V or so, energy density, will not cause environmental pollution, can substitute existing cause
The gasoline equal energy source of environmental pollution, no pollution realize pure electric automobile.
From Fig. 2 rich lithium richness manganese material SEM it can be seen from the figure thats, the material morphology of preparation is spheric granules, particle size
At 8~10 μm.
It can be seen that the material belongs to (R-3m) symmetrical structure from Fig. 3 rich lithium richness manganese material XRD spectra, there is stratiform
LiCoO2Architectural feature.
From Fig. 4 rich lithium richness manganese material with Si material charge-discharge performance figures can, the discharge capacity of Si materials is
0.94mAh, rich lithium richness manganese material discharge capacity are 0.89mAh.
Can be seen that full battery average voltage with 0.2C cycle performance figures from Fig. 5 full battery charging and discharging performance map is 3V,
Specific capacity is 259mAh g-1。
By the manufacture method of above-mentioned Si negative poles and the high-energy-density secondary lithium battery of rich lithium richness manganese positive pole, produce
The species of lithium ion battery include：Square, button, cylinder, flexible packaging type battery etc..
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and
Modification, these improvement and modification also should be regarded as protection scope of the present invention.
Claims (4)
- A kind of 1. manufacture method of the high-energy-density secondary lithium battery of Si negative poles and rich lithium richness manganese positive pole, it is characterised in that： Comprise the following steps：(1) mixed salt solution is prepared with the metal salt of nickel, cobalt and manganese；(2) mixed salt solution obtained in step (1) is instilled in the reactor for filling ammoniacal liquor under the conditions of 60 DEG C and reacted For a period of time, and sodium hydroxide control ph is used, coprecipitated product is obtained after the completion of reaction；(3) coprecipitated product obtained in step (2) is washed and filtered and be then well mixed with lithium carbonate, obtain mixture；(4) mixture obtained in step (3) is put into Muffle furnace, is calcined to 750 DEG C~850 DEG C and continues in air atmosphere 10~12 hours, target product richness lithium richness manganese material is obtained after natural cooling；(5) by the rich lithium richness manganese material obtained in step (4) and acetylene black and polytetrafluoroethylene (PTFE) (PTFE) with 85:10：5 ratio It is well mixed to be prepared into anode；(6) by nano Si powder and sodium alginate and Super p carbon blacks with 60：20：20 ratio is well mixed to be prepared into battery Negative pole；(7) GND obtained in the anode obtained in step (5) and step (6) is assembled in glove box and helps electricity Pond；Reaction time described in step (2) is 10~50 hours；PH value range described in step (2) is controlled between 9~11.
- 2. the manufacturer of the high-energy-density secondary lithium battery of Si negative poles according to claim 1 and rich lithium richness manganese positive pole Method, it is characterised in that：Coprecipitated product described in step (3), molecular formula are M (OH)2, wherein M=Ni, Co, Mn.
- 3. the manufacturer of the high-energy-density secondary lithium battery of Si negative poles according to claim 2 and rich lithium richness manganese positive pole Method, it is characterised in that：Target product richness lithium richness manganese material described in step (4) is xLi2MnO3·(1-x)LiMO2Wherein M= Ni,Co,Mn；X ＜ 1.
- 4. the manufacturer of the high-energy-density secondary lithium battery of Si negative poles according to claim 3 and rich lithium richness manganese positive pole Method, it is characterised in that：The just extremely rich lithium richness manganese material of full battery described in step (7), molecular formula xLi2MnO3·(1- x)LiMO2, wherein M=Ni, Co, Mn, negative pole is Si materials.
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| CN103633305A (en) * | 2013-12-10 | 2014-03-12 | 苏州宇豪纳米材料有限公司 | Silicon composite anode material of lithium ion battery and preparation method of silicon composite anode material |
| CN103956479A (en) * | 2014-05-20 | 2014-07-30 | 天津理工大学 | Preparation method of spherical high-capacity lithium-rich positive electrode material |
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| CN103633305A (en) * | 2013-12-10 | 2014-03-12 | 苏州宇豪纳米材料有限公司 | Silicon composite anode material of lithium ion battery and preparation method of silicon composite anode material |
| CN103956479A (en) * | 2014-05-20 | 2014-07-30 | 天津理工大学 | Preparation method of spherical high-capacity lithium-rich positive electrode material |
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Effective date of registration: 20160303 Address after: 309, room 215021, building D, 99 Yan Ai Road, Suzhou Industrial Park, Jiangsu, China Applicant after: SUZHOU DISIFU NEW ENERGY TECHNOLOGY CO., LTD. Applicant after: Nanjing University Address before: 309, room 215021, building D, 99 Yan Ai Road, Suzhou Industrial Park, Jiangsu, China Applicant before: SUZHOU DISIFU NEW ENERGY TECHNOLOGY CO., LTD. |
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Inventor after: He Ping Inventor after: Ye Jing Inventor after: Zhou Haoshen Inventor before: He Ping Inventor before: Xu Feng Inventor before: Zhou Haoshen |