CN105261792A - Preparation method for high-specific-energy secondary lithium ion battery with Si negative electrode and lithium- and manganese-rich positive electrode - Google Patents
Preparation method for high-specific-energy secondary lithium ion battery with Si negative electrode and lithium- and manganese-rich positive electrode Download PDFInfo
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- CN105261792A CN105261792A CN201510427972.3A CN201510427972A CN105261792A CN 105261792 A CN105261792 A CN 105261792A CN 201510427972 A CN201510427972 A CN 201510427972A CN 105261792 A CN105261792 A CN 105261792A
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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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- 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
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- 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
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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
- H01M2004/028—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
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- 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
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- 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 for high-specific-energy secondary lithium ion battery with Si negative electrode and lithium- and manganese-rich positive electrode. The molecular formula of a lithium- and manganese-rich material is (x)Li<2>MnO<3>.(1-x)LiMO<2>, M is Ni, Co and Mn, the total battery negative electrode is prepared from a nanometer Si material, Super p carbon black and sodium alginate according to a proportion, the positive electrode is prepared by mixing the lithium- and manganese-rich material, polytetrafluoroethylene and acetylene black, and the lithium- and manganese-rich material is prepared by co-precipitation of a metal salt solution and a NaOH solution. The total battery assembled from the Si material and the lithium- and manganese-rich material has the advantages of relatively high capacity and specific energy, high average voltage and no pollution.
Description
Technical field
The present invention relates to a kind of manufacture method of secondary lithium battery, particularly relate to the manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole and the rich manganese positive pole of rich lithium.
Background technology
In prior art, because lithium battery anode adopts cobalt acid lithium, cost is higher, and the toxicity of cobalt is comparatively large, larger on the impact of environment; And the employing of existing lithium battery major part negative pole is graphite, graphite density is less, and the lower battery volume that causes of tap density is larger; This just causes lithium ion battery, and specific discharge capacity is too low on the one hand, and energy density cannot satisfy the demands, and the cobalt toxicity on the other hand in lithium cobaltate cathode is comparatively large, and environmental pollution is larger and expensive.
In order to solve the storage problem of the energy, countries in the world all create great interest to Large Copacity chemistry energy storage material, especially along with the development of electronic technology, various portable digital products continuing to bring out as blowout, and electronic product small volume and less weight will be made to be easy to carry and cruising time long, the little specific capacity of chemical power source volume that this just requires it to be equipped with is large and good stability fail safe is high.At present with LiCoO
2be respectively the lithium rechargeable battery of positive pole and negative material with graphite, due to its energy density and specific capacity relatively low, be more and more difficult to meet portable set and pure electric automobile to the demand of battery energy density.
The rich manganese anode material xLi of rich lithium
2mnO
3(1-x) LiMO
2relative to other LiCoO
2, LiMn2O
4, LiFePO
4, LiNi
1/3co
1/3mn
1/3o
2deng positive electrode because it has higher specific capacity (200 ~ 300mAhg
-1) be considered to the desirable positive electrode of lithium ion battery of future generation compared with advantages such as low production cost and new charge discharge mechanism.
With regard to negative material, Si negative material has 3000mAhg
-1above comparatively height ratio capacity is ideal negative material, but causes this material circulation poor-performing because Si negative material change in volume in the process of discharge and recharge is comparatively serious.The people such as tension force adopt nano Si as negative pole raw material, use sodium alginate to be coated with as binding agent the cyclicity problem that the Si negative material of film preparation preferably resolves Si material, make Si materials application become possibility in lithium ion battery.The capacity of Si negative material is about ten times of graphite cathode, makes the lithium rechargeable battery of employing Si negative pole will have larger specific capacity.
Because above-mentioned content, the design people, actively in addition research and innovation, to founding the manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole and the rich manganese positive pole of rich lithium, make it have more value in industry.
Summary of the invention
For solving the problems of the technologies described above, the object of this invention is to provide a kind of can manufacture and there is higher capacity and specific energy, the manufacture method of the high-energy-density secondary lithium battery of the Si negative pole of average voltage high and the rich manganese positive pole of rich lithium.
The manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole that the present invention proposes and the rich manganese positive pole of rich lithium, is characterized in that: comprise the steps:
(1) with the slaine preparation mixed salt solution of nickel, cobalt and manganese;
(2) mixed salt solution obtained in step (1) is instilled under 60 DEG C of conditions the reaction kettle for reaction a period of time filling ammoniacal liquor, and use NaOH control ph, after having reacted, obtain coprecipitated product;
(3) coprecipitated product obtained in step (2) is washed and filtered then mix with lithium carbonate, obtain mixture;
(4) mixture obtained in step (3) is put into Muffle furnace, roasting to 750 DEG C in air atmosphere ~ 850 DEG C continues 10 ~ 12 hours, naturally obtains target product rich lithium richness manganese material after cooling;
(5) rich for the rich lithium obtained in step (4) manganese material and acetylene black and polytetrafluoroethylene (PTFE) are mixed with the ratio of 85:10:5 be prepared into anode;
(6) nano Si powder and sodium alginate and Superp carbon black are mixed with the ratio of 60:20:20 be prepared into battery cathode;
(7) battery cathode obtained in the anode obtained in step (5) and step (6) is assembled in glove box help 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, described in step (2), pH value range controls 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 rich manganese material of the rich lithium of the target product described in step (4) is xLi
2mnO
3(1-x) LiMO
2wherein M=Ni, Co, Mn; X < 1.
As the further improvement of the inventive method, the rich manganese material of just very rich lithium of the full battery described in step (7), molecular formula is xLi
2mnO
3(1-x) LiMO
2, wherein M=Ni, Co, Mn, negative pole is Si material.
By such scheme, the present invention at least has the following advantages: the present invention uses the rich manganese material of spherical rich lithium as anode, nano Si material is as the negative pole of battery, its Heterosis exists: on the one hand, and the rich manganese material of rich lithium has that tap density height ratio capacity is large and first circle efficiency is high and the feature such as good reversibility.On the other hand, the advantages such as nano Si material has larger advantage for other negative materials in specific capacity, and it is high that the lithium ion battery therefore using this bi-material to assemble out has specific capacity, and average voltage is high, and specific energy is large.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to better understand technological means of the present invention, and can be implemented according to the content of specification, coordinates accompanying drawing to be described in detail as follows below with preferred embodiment of the present invention.
Accompanying drawing explanation
Fig. 1 is the manufacture method flow chart of the high-energy-density secondary lithium battery of the rich manganese positive pole of Si negative pole of the present invention and rich lithium.
Fig. 2 is the rich manganese material Electronic Speculum figure of rich lithium;
Fig. 3 is the rich manganese material XRD spectra of rich lithium;
Fig. 4 is the rich manganese material of rich lithium and Si material charge-discharge performance figure;
Fig. 5 is full battery charging and discharging performance map and 0.2C cycle performance figure.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment one: the manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole and the rich manganese positive pole of rich lithium, the step of the method is as follows:
(1) with the sulfate preparation mixed salt solution of nickel, cobalt and manganese, concentration is 2mol/L;
(2) mixed salt solution obtained in step (1) is instilled under 60 DEG C of conditions the reaction kettle for reaction 50 hours filling 1mol/L ammoniacal liquor, and use NaOH control ph to be 10, after having reacted, obtain coprecipitated product;
(3) coprecipitated product obtained in step (2) washed and filtered, then mixing with lithium carbonate, obtain mixture;
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnace, roasting to 750 DEG C in air atmosphere ~ 850 DEG C, continue 10 ~ 12 hours, naturally after cooling, obtain target product rich lithium richness manganese material;
(5) rich for the rich lithium obtained in step (4) manganese material and acetylene black and PTFE are mixed with the ratio of 85:10:5 be prepared into anode;
(6) nano Si powder and sodium alginate and Superp carbon black are mixed with the ratio of 60:20:20 be prepared into battery cathode;
(7) battery cathode obtained in the anode obtained in step (5) and step (6) is assembled in glove box help battery.
Embodiment two: the manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole and the rich manganese positive pole of rich lithium, the step of the method is as follows:
(1) with the sulfate preparation mixed salt solution of nickel, cobalt and manganese, concentration is 1mol/L;
(2) mixed salt solution obtained in step (1) is instilled under 60 DEG C of conditions the reaction kettle for reaction 50 hours filling 1mol/L ammoniacal liquor, and use NaOH control ph to be 11, after having reacted, obtain coprecipitated product;
(3) coprecipitated product obtained in step (2) washed and filtered, then mixing with lithium carbonate, obtain mixture;
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnace, roasting to 750 DEG C in air atmosphere ~ 850 DEG C continues 10 ~ 12 hours, naturally obtains target product rich lithium richness manganese material after cooling.
(5) rich for the rich lithium obtained in step (4) manganese material and acetylene black and PTFE are mixed with the ratio of 85:10:5 be prepared into anode;
(6) nano Si powder and sodium alginate and Superp carbon black are mixed with the ratio of 60:20:20 be prepared into battery cathode;
(7) battery cathode obtained in the anode obtained in step (5) and step (6) is assembled in glove box help battery.
Embodiment three: the manufacture method of the high-energy-density secondary lithium battery of a kind of Si negative pole and the rich manganese positive pole of rich lithium, the step of the method is as follows:
(1) with the sulfate preparation mixed salt solution of nickel, cobalt and manganese, concentration is 2mol/L;
(2) mixed salt solution obtained in step (1) is instilled under 60 DEG C of conditions the reaction kettle for reaction 10 hours filling 1mol/L ammoniacal liquor, and use NaOH control ph to be 10, after having reacted, obtain coprecipitated product;
(3) coprecipitated product obtained in step (2) washed and filtered, then mixing with lithium carbonate, obtain mixture;
(4) mixture obtained in step (3) is put into KSL-1100X type Muffle furnace, roasting to 750 DEG C in air atmosphere ~ 850 DEG C continues 10 ~ 12 hours, naturally obtains target product rich lithium richness manganese material after cooling.
(5) rich for the rich lithium obtained in step (4) manganese material and acetylene black and PTFE are mixed with the ratio of 85:10:5 be prepared into anode;
(6) nano Si powder and sodium alginate and Superp carbon black are mixed with the ratio of 60:20:20 be prepared into battery cathode;
(7) battery cathode obtained in the anode obtained in step (5) and step (6) is assembled in glove box help battery.
All can produce a kind of lithium ion battery by above-mentioned three embodiments, during this lithium ion cell charging, electrode reaction is as follows:
(1) negative reaction: xLi
++ Si+xe
-→ Li
xsi;
Positive electrode is with lithium ion (Li
+) form be dissolved in organic electrolyte, electronics is supplied to wire.
(2) positive pole reaction: xLi
2mnO
3(1-x) LiMO
2→ xMnO
2(1-x) MO
2+ (1+x) Li
++ x/2O
2+ (1+x) e
-;
Use the rich manganese material of rich lithium as positive pole in the present invention, due to the less thus advantage of lower cost of cobalt content in the rich manganese material of rich lithium, and the rich manganese material specific capacity of rich lithium is greater than cobalt acid lithium, on the other hand, the specific capacity of Si negative material is about ten times of graphite cathode material, and density is greater than graphite, so the lithium ion battery specific capacity using this bi-material to produce is large, average working voltage is at about 3V, energy density can reach 590Wh/Kg, environmental pollution can not be caused, can substitute existing cause environmental pollution gasoline equal energy source, no pollution realize pure electric automobile.
As can be seen from the rich lithium rich manganese material SEM figure of Fig. 2, the material morphology of preparation is spheric granules, and particle size is at 8 ~ 10 μm.
Can find out that this material belongs to (R-3m) symmetrical structure from the rich manganese material XRD spectra of the rich lithium of Fig. 3, there is stratiform LiCoO
2architectural feature.
From the rich manganese material of the rich lithium of Fig. 4 and Si material charge-discharge performance figure can, the discharge capacity of Si material is 0.94mAh, and rich lithium richness manganese material discharge capacity is 0.89mAh.
As can be seen from full battery charging and discharging performance map and the 0.2C cycle performance figure of Fig. 5, full battery average voltage is 3V, and specific capacity is 259mAhg
-1.
By the manufacture method of the high-energy-density secondary lithium battery of the rich manganese positive pole of above-mentioned Si negative pole and rich lithium, the kind of the lithium ion battery produced comprises: square, button, cylindrical, flexible packaging type battery etc.
The above is only the preferred embodiment of the present invention; be not limited to the present invention; should be understood that; for those skilled in the art; under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (6)
1. a manufacture method for the high-energy-density secondary lithium battery of Si negative pole and the rich manganese positive pole of rich lithium, is characterized in that: comprise the steps:
(1) with the slaine preparation mixed salt solution of nickel, cobalt and manganese;
(2) mixed salt solution obtained in step (1) is instilled under 60 DEG C of conditions the reaction kettle for reaction a period of time filling ammoniacal liquor, and use NaOH control ph, after having reacted, obtain coprecipitated product;
(3) coprecipitated product obtained in step (2) is washed and filtered then mix with lithium carbonate, obtain mixture;
(4) mixture obtained in step (3) is put into Muffle furnace, roasting to 750 DEG C in air atmosphere ~ 850 DEG C continues 10 ~ 12 hours, naturally obtains target product rich lithium richness manganese material after cooling;
(5) rich for the rich lithium obtained in step (4) manganese material and acetylene black and polytetrafluoroethylene (PTFE) are mixed with the ratio of 85:10:5 be prepared into anode;
(6) nano Si powder and sodium alginate and Superp carbon black are mixed with the ratio of 60:20:20 be prepared into battery cathode;
(7) battery cathode obtained in the anode obtained in step (5) and step (6) is assembled in glove box help battery.
2. the manufacture method of the high-energy-density secondary lithium battery of Si negative pole according to claim 1 and the rich manganese positive pole of rich lithium, is characterized in that: the reaction time described in step (2) is 10 ~ 50 hours.
3. the manufacture method of the high-energy-density secondary lithium battery of Si negative pole according to claim 2 and the rich manganese positive pole of rich lithium, is characterized in that: described in step (2), pH value range controls between 9 ~ 11.
4. the manufacture method of the high-energy-density secondary lithium battery of Si negative pole according to claim 3 and the rich manganese positive pole of rich lithium, it is characterized in that: the coprecipitated product described in step (3), molecular formula is M (OH)
2, wherein M=Ni, Co, Mn.
5. the manufacture method of the high-energy-density secondary lithium battery of Si negative pole according to claim 4 and the rich manganese positive pole of rich lithium, is characterized in that: the rich manganese material of the rich lithium of the target product described in step (4) is xLi
2mnO
3(1-x) LiMO
2wherein M=Ni, Co, Mn; X < 1.
6. the manufacture method of the high-energy-density secondary lithium battery of Si negative pole according to claim 5 and the rich manganese positive pole of rich lithium, is characterized in that: the rich manganese material of just very rich lithium of the full battery described in step (7), molecular formula is xLi
2mnO
3(1-x) LiMO
2, wherein M=Ni, Co, Mn, negative pole is Si 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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