CN1841815A - Negative pole, its preparation method and lithium secondary battery using same - Google Patents
Negative pole, its preparation method and lithium secondary battery using same Download PDFInfo
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- CN1841815A CN1841815A CNA2005100339384A CN200510033938A CN1841815A CN 1841815 A CN1841815 A CN 1841815A CN A2005100339384 A CNA2005100339384 A CN A2005100339384A CN 200510033938 A CN200510033938 A CN 200510033938A CN 1841815 A CN1841815 A CN 1841815A
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- carbon nano
- tube
- secondary battery
- lithium
- lithium secondary
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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
Abstract
The invention relates to a Li second time cell negative electrode, its preparing method and a Li second time cell for using the negative electrode. The negative electrode comprises a conductive base material and a carbon nanometer pipe layer formed on the (CH2CH2O)n bridge of the conductive base material surface. The carbon nanometer pipe of the (CH2CH2O)n bridge comprises a plurality of carbon nanometer pipe single bodies; a plurality of (CH2CH2O)n are connected with the adjacent carbon nanometer pipe single body. The Li second time cell comprises a casing and the negative electrode, anode, electrolyte and isolating film in the casing, wherein the negative electrode is connected with the anode by the isolating film.
Description
[technical field]
The present invention relates to the lithium secondary battery of a kind of lithium secondary battery anode, its preparation method and this negative pole of use, relate in particular to a kind of lithium secondary battery that utilizes carbon nano-tube as negative material.
[background technology]
Battery is the device that chemical energy is converted into electric energy, and battery product develops into present lithium battery from early stage lead-acid battery, nickel-cadmium cell and Ni-MH battery.Wherein, lead-acid battery and nickel-cadmium cell are because problem of environmental pollution is replaced by lithium battery gradually.The present also branch of lithium battery and chargeable lithium cell once of lithium battery, chargeable lithium battery is a lithium secondary battery, be with an organic solvent with the maximum difference of conventional batteries and non-aqueous solution as electrolyte.
The lithium secondary battery range of application is quite extensive, mainly comprises consumption electronic products (ConsumerElectronic Products), computer (Computer) and communication product (CommunicationProducts), generally abbreviates 3C Product as.For satisfying the needs of various products, the developing direction of lithium secondary battery comprises: (1) prolongs battery useful life; (2) increase battery capacity density; (3) volume requirement microminiaturization; (4) remove the capacity memory effect.
Raising energy density key is the exploitation of the electrode material of high capacity capacity, for reversible electrode material, has open structural materials such as stratiform or tunnel structure for the most suitable.In lithium secondary battery, this class formation provides the lithium ion pipeline and mobility fast of turnover easily, can increase the cycle life of battery.At present, the commercialization product uses carbon materials as negative material mostly, as native graphite, and class graphite, coke, carbon black etc.
At present, the research of carbon nano-tube becomes the new direction of carbon element negative pole research material again.Carbon nano-tube is a kind of new carbon, find in 1991 by Japanese scientist Iijima, see also " Helicalmicrotubules of graphitic carbon ", S Iijima, Nature, vol.354, p56 (1991), it and graphite, diamond be allotrope each other, and the branch of Single Walled Carbon Nanotube and multi-walled carbon nano-tubes is arranged.People such as Jijun Zhao study the character of embedding lithium carbon nano-tube, be published in Physical Review Letters, vol.85, p1707～1709 (2000), the result shows that the space all can embed lithium between Single Walled Carbon Nanotube inside and pipe, and it is similar to graphite that the lithium of Single Walled Carbon Nanotube embeds electromotive force, but embed density apparently higher than graphite, can reach Li
0.5C.
Good and the Lv Changyue of the inventor Chen Jie of our company has disclosed a kind of carbon nano-tube material that adopts in No. 03113512.9 Chinese patent application be the lithium ion battery of negative pole, and it comprises a positive pole, a negative pole and osmotic isolating film, and this positive pole comprises Li
xCo
yNi
zO
2Nano particle, negative pole comprises the carbon nano-tube array that is made of multi-walled carbon nano-tubes, and each multi-walled carbon nano-tubes comprises a plurality of coaxial graphite-pipe layers, can embed lithium ion between the adjacent graphite-pipe layer, this osmotic isolating film has microcellular structure, ion is passed through and non-conductive.
But because the tiny tubular structure feature of carbon nano-tube makes lithium secondary battery when charging, lithium ion can embed the interior space of pipe of carbon nano-tube; And when discharge, lithium ion is difficult for taking off embedding the space in the pipe of carbon nano-tube, thereby the irreversible capacitance of part occurs, causes the loss of capacitance of lithium secondary battery.
In view of this, provide a kind of and reduce irreversible capacitance, and further improve negative pole, its preparation method of capacitance and use the lithium secondary battery of this negative pole to be necessity in fact.
[summary of the invention]
Below, will illustrate with some embodiment and a kind ofly reduce irreversible capacitance, and further improve the negative pole of capacitance.
And illustrate by these embodiment and a kind ofly to reduce irreversible capacitance, and further improve the preparation method of the negative pole of capacitance.
And illustrate by these embodiment and a kind ofly to reduce irreversible capacitance, and further improve the lithium secondary battery of capacitance.
For realizing foregoing, a kind of lithium secondary battery anode is provided, what it comprised that a conductive base and is formed at this surfaces of conductive substrates contains alkoxy chain ((CH
2CH
2O)
n) carbon nanotube layer of building bridge.
Preferably, this carbon nano-tube that contains the alkoxy chain bridge formation comprises a plurality of carbon nano-tube monomers, and a plurality of alkoxy chains connect adjacent carbon nano-tube monomer.
Further, this carbon nano-tube monomer is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
And, a kind of preparation method of lithium secondary battery anode is provided, its step comprises:
One conductive base is provided;
A plurality of carbon nano-tube monomers are provided, this monomer is carried out surfaction;
Carbon nano-tube monomer behind the upgrading and polyethylene glycol oxide polymerization are generated the carbon nano-tube that contains the alkoxy chain bridge formation;
Form one in this surfaces of conductive substrates and contain the carbon nanotube layer that alkoxy chain is built bridge.
Preferably, this monomer carries out surfaction and comprises surperficial carboxyl or hydroxylating upgrading.
And, a kind of lithium secondary battery is provided, and it comprises housing and places housing interior negative pole, positive pole, electrolyte and barrier film that wherein negative pole links to each other by this barrier film with anodal, this negative pole comprises a conductive base and is formed at one of this surfaces of conductive substrates and contains alkoxy chain ((CH
2CH
2O)
n) carbon nanotube layer of building bridge.
Compared with prior art, the technical program is because negative active core-shell material is to contain the carbon nano-tube formation that alkoxy chain is built bridge, form a plurality of spaces that separate between a plurality of alkoxy chains bridge formations and the carbon nano-tube monomer, it can be used for storing lithium ion, so, control by this alkoxy chain bridge formation length, can effectively utilize adjacent carbon nano-tube monomer gap length and control and reach the lithium ion maximum capacitance, and the lithium ion coil insertion device that reduces space in the pipe of carbon nano-tube monomer can reduce irreversible capacitance to reach; And this structure helps improving the conductive capability of negative pole.So, adopt the carbon nano-tube that contains the alkoxy chain bridge formation to have the advantage of high power capacity as the lithium secondary battery of negative active core-shell material.
[description of drawings]
Fig. 1 is the negative pole structure schematic diagram of the technical program first embodiment.
Fig. 2 is the lithium secondary battery structural representation of the technical program the 3rd embodiment.
Fig. 3 is a schematic arrangement behind the carbon nano tube surface upgrading of the technical program first embodiment.
Fig. 4 is the carbon nanotube molecule structural representation that alkoxy chain is built bridge that contains of the technical program first embodiment.
[embodiment]
The present invention is described in further detail below in conjunction with drawings and Examples.
See also Fig. 1, the lithium secondary battery anode 10 of first embodiment of the invention comprises that conductive base 101 and is formed at the carbon nanotube layer 102 that alkoxy chain is built bridge that contains on conductive base 101 surfaces.This conductive base 101 is metal base or carbon-point, has excellent conductive performance.The carbon nano-tube that contains the alkoxy chain bridge formation comprises a plurality of carbon nano-tube monomers, and a plurality of alkoxy chains connect adjacent carbon nano-tube monomer, and alkoxy chain length controlled system, and wherein, this carbon nano-tube monomer is single multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.This carbon nano-tube that contains the alkoxy chain bridge formation is mainly by carbon nano-tube monomer and polyethylene glycol oxide (Poly Ethylene Oxide, PEO) (molecular formula: [CH through surfaction (Surface Modification)
2CH
2O]
n) polymerization is prepared from.Described carbon nano-tube monomer surfaction comprises the part surface upgrading.
See also Fig. 3, the carbon nano-tube monomer behind surfaction comprises three kinds of structure a, b, c.Wherein, structure a is that carbon nano tube surface is through the carboxyl (COOH) structure behind the change upgrading; Structure b is that carbon nano tube surface is through the hydroxyl (OH) structure behind the change upgrading; Structure c is the structure of carbon nano tube surface behind hydroxyl and carboxylated upgrading, and the hydroxyl of these relative both sides of structure or carboxyl can be symmetrical, also can be asymmetric.
See also Fig. 4, the structure that contains the carbon nano-tube 102 of alkoxy chain bridge formation mainly comprises three kinds of structure d, e, f.(structure a) forms with the polyethylene glycol oxide polymerization structure d, and its adjacent carbon nano-tube monomer is connected by alkoxy chain in carboxylated place by a plurality of carbon nano-tube monomers.Structure e is formed by a plurality of carbon nano-tube monomers (structure b) and the polymerization of polymerization polyethylene glycol oxide, and its adjacent carbon nano-tube monomer is connected by alkoxy chain in the hydroxylating place.Same, structure f is formed by a plurality of carbon nano-tube monomers (structure c) and polyethylene glycol oxide polymerization, and the hydroxyl or the carboxyl of its adjacent carbon nano-tube monomer correspondence are connected by alkoxy chain.In addition, the structure f hydroxyl that this carbon nano-tube monomer also can occur is connected by alkoxy chain with the carboxyl of adjacent carbon nano-tube monomer.
Below, be example with the carbon nano tube structure d that contains the alkoxy chain bridge formation, introduce the preparation method of the carbon nano-tube 102 that contains the alkoxy chain bridge formation in detail, it may further comprise the steps:
(1) provides a plurality of carbon nano-tube monomers, and should carry out carboxylated upgrading in a plurality of carbon nano-tube monomers surface.Its carboxylated upgrading step comprises: the sulfuric acid and the salpeter solution (sulfuric acid and nitric acid volume ratio are 3: 1) that the carbon nano-tube monomer powder of a Unit Weight are added four parts of Unit Weights; With said mixture ultrasonic oscillation three hours at room temperature; Dilute this mixture with 1: 5 volume ratio then; With PTFE (the Poly Tetra Fluoro Ethylene) filter membrane of this mixture by 10 μ m micropores; Clean the carbon nano-tube after residual acid obtains upgrading at last.
(2) carbon nano-tube monomer behind the carboxylated upgrading and polyethylene glycol oxide polymerization are generated the carbon nano-tube that contains the alkoxy chain bridge formation.Its polymerization procedure comprises: the carbon nano-tube monomer behind the upgrading is put into the acetone soln test tube, stirred one hour by sonication method (Sonication); Polyethylene glycol oxide is dissolved in another part acetone soln test tube; Stirred one hour with the mixing of two acetone soln test tubes and by the sonication method, be heated to 70 ℃ while shake then; Add potassium hydroxide catalyst reaction five hours.
Be understandable that, but the appropriate change experiment condition is selected carboxyl or carboxylated upgrading in the carbon nano-tube monomer surfaction process of the technical program, as select suitable acid and its consumption etc. for use; Three kinds of structure d that contain the carbon nano-tube of alkoxy chain bridge formation, e, f all can satisfy the function that the gap of adjacent carbon nano-tube monomer is separated into several spaces, and these several spaces can effectively embed lithium ion or make lithium ion take off embedding in charge and discharge process, improves the capacitance of battery; And this structure helps improving the conductive capability of negative pole.
The preparation method of the lithium secondary battery anode 10 of second embodiment of the invention may further comprise the steps: (1) provides a conductive base 101; (2) provide a plurality of carbon nano-tube monomers, this monomer is carried out surperficial carboxyl or hydroxylating upgrading; (3) carbon nano-tube monomer behind the upgrading and polyethylene glycol oxide polymerization are generated the carbon nano-tube that contains the alkoxy chain bridge formation; (4) form one in this surfaces of conductive substrates and contain the carbon nanotube layer 102 that alkoxy chain is built bridge, this step can adopt methods such as coating or deposition.Wherein, step (2) and step (3) can be in detail with reference to first embodiment.
See also Fig. 2, the lithium secondary battery 20 of third embodiment of the invention comprises a housing (figure indicate) and places positive pole 11 in the housing, electrolyte 12, barrier film 13 and the negative pole 10 that provides of first embodiment as described above, and wherein negative pole 10 and positive pole 11 link to each other by this barrier film 13.
Above-mentioned lithium secondary battery 20 comprises lithium ion battery and high-polymer lithium battery.The positive pole 11 of lithium ion battery and high-polymer lithium battery mainly comprises conductive base and is formed at the active material of surfaces of conductive substrates, as the composite oxides of lithium such as lithium manganese oxide, lithium nickel oxide, lithium and cobalt oxides and transition metal.
For lithium ion battery, electrolyte 12 is general organic electrolyte solution, can be added one or more solvable lithium salts by the mixed solvent that a kind of organic solvent or several organic solvent are formed and form.Organic solvent is propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, 1 for example, 2-dimethoxy-ethane etc.Typical solvable lithium salts such as lithium perchlorate, LiBF4, lithium hexafluoro phosphate, trifluoromethyl sulfonic acid lithium, hexafluoroarsenate lithium etc.
For high-polymer lithium battery, electrolyte 12 is polymer dielectric, as contains polyethylene oxygen alkane, polypropylene oxygen alkane, polyvinyl chloride, Kynoar of lithium salts such as lithium perchlorate, LiBF4, lithium hexafluoro phosphate, trifluoromethyl sulfonic acid lithium, hexafluoroarsenate lithium etc.
Lithium secondary battery 20 housings comprise metal, alloy, plastics or its combination.
Lithium secondary battery 20 of the present invention can have Any shape, as cylindric, prism-shaped, sheet or button-type.
The preparation of lithium secondary battery of the present invention can be adopted the known method for preparing lithium secondary battery of any public.Particularly, a kind of method commonly used is included in the negative pole 10 placed in the housing (figure do not show) by barrier film 13 couplings and anodal 11, subsequently toward wherein injecting electrolyte and with its sealing.The electrolytical method of preferred vacuum injection conduct injection, but it is not had special restriction.Also electrode 10,11 preceding in placing housing of coupling can be flooded with electrolyte solution.
The technical program is because negative active core-shell material is to contain the carbon nano-tube formation that alkoxy chain is built bridge, form a plurality of spaces that separate between a plurality of alkoxy chains bridge formations and the carbon nano-tube monomer, it can be used for storing lithium ion, so, control by this alkoxy chain bridge formation length, the gap length control that can effectively utilize adjacent carbon nano-tube monomer to be reaching the lithium ion maximum capacitance, and the lithium ion coil insertion device that reduces space in the pipe of carbon nano-tube monomer can reduce irreversible capacitance to reach; And this structure helps improving the conductive capability of negative pole.So, adopt the carbon nano-tube that contains the alkoxy chain bridge formation to have the advantage of high power capacity as the lithium secondary battery of negative active core-shell material.
In addition, those skilled in the art also can do other variations in spirit of the present invention, certainly, the variation that these are done according to spirit of the present invention, all should be included in the present invention's scope required for protection in.
Claims (21)
1. lithium secondary battery anode, it comprises a conductive base, it is characterized in that further comprising one be formed at this surfaces of conductive substrates contain alkoxy chain ((CH
2CH
2O)
n) carbon nanotube layer of building bridge.
2. lithium secondary battery anode as claimed in claim 1 is characterized in that the carbon nano-tube that contains the alkoxy chain bridge formation comprises a plurality of carbon nano-tube monomers, and a plurality of alkoxy chains connect adjacent carbon nano-tube monomer.
3. lithium secondary battery anode as claimed in claim 2, the carbon nano-tube monomer surface that it is characterized in that containing the carbon nano-tube that alkoxy chain builds bridge is by carboxylated, and adjacent carbon nano-tube monomer is connected by alkoxy chain in carboxylated place.
4. lithium secondary battery anode as claimed in claim 2, the carbon nano-tube monomer surface that it is characterized in that containing the carbon nano-tube that alkoxy chain builds bridge is by hydroxylating, and adjacent carbon nano-tube monomer is connected by alkoxy chain in the hydroxylating place.
5. lithium secondary battery anode as claimed in claim 2, the carbon nano-tube monomer surface that it is characterized in that containing the carbon nano-tube that alkoxy chain builds bridge is by carboxyl and hydroxylating, the hydroxyl or the carboxyl of adjacent carbon nano-tube monomer correspondence are connected by alkoxy chain, or the hydroxyl of adjacent carbon nano-tube monomer is connected by alkoxy chain with carboxyl.
6. as any described lithium secondary battery anode in the claim 2 to 5, it is characterized in that carbon nano-tube monomer comprises multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
7. lithium secondary battery anode as claimed in claim 1 is characterized in that conductive base comprises metal base or carbon-point.
8. the preparation method of a lithium secondary battery anode, its step comprises:
One conductive base is provided;
A plurality of carbon nano-tube monomers are provided, this monomer is carried out surfaction;
Carbon nano-tube monomer behind the upgrading and polyethylene glycol oxide polymerization are generated the carbon nano-tube that contains the alkoxy chain bridge formation;
Form one in this surfaces of conductive substrates and contain the carbon nanotube layer that alkoxy chain is built bridge.
9. preparation method as claimed in claim 8 is characterized in that conductive base comprises metal base or carbon-point.
10. preparation method as claimed in claim 8 is characterized in that carbon nano-tube monomer comprises multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
11. preparation method as claimed in claim 8 is characterized in that this monomer is carried out surfaction be may further comprise the steps:
The carbon nano-tube monomer powder is added sulfuric acid and salpeter solution;
Ultrasonic oscillation is handled said mixture;
Dilute this mixture;
Filter and clean this mixture.
12. preparation method as claimed in claim 8 is characterized in that carbon nano-tube monomer behind the upgrading and polyethylene glycol oxide polymerization be may further comprise the steps:
Carbon nano-tube monomer behind the upgrading is put into acetone soln;
Stir above-mentioned mixed solution by the sonication method;
Polyethylene glycol oxide is dissolved in another part acetone soln;
Two acetone solns are mixed stirring and heating;
And add potassium hydroxide catalyst to above-mentioned mixed solution simultaneously.
13. preparation method as claimed in claim 8 is characterized in that forming a carbon nanotube layer that contains the alkoxy chain bridge formation in this surfaces of conductive substrates comprises that employing applies or deposition process.
14. lithium secondary battery, it comprises housing and places housing interior negative pole, positive pole, electrolyte and barrier film, wherein negative pole links to each other by this barrier film with anodal, and what it is characterized in that this negative pole comprises that a conductive base and is formed at this surfaces of conductive substrates contains alkoxy chain ((CH
2CH
2O)
n) carbon nanotube layer of building bridge.
15. lithium secondary battery as claimed in claim 14 is characterized in that the carbon nano-tube that contains the alkoxy chain bridge formation comprises a plurality of carbon nano-tube monomers, a plurality of alkoxy chains connect adjacent carbon nano-tube monomer.
16. lithium secondary battery as claimed in claim 15 is characterized in that carbon nano-tube monomer comprises Single Walled Carbon Nanotube and multi-walled carbon nano-tubes.
17. lithium secondary battery as claimed in claim 14 is characterized in that positive pole comprises conductive base and the positive active material that is formed at surfaces of conductive substrates.
18. lithium secondary battery as claimed in claim 20, the positive active material that it is characterized in that comprises lithium manganese oxide, lithium nickel oxide, lithium and cobalt oxides.
19. lithium secondary battery as claimed in claim 14, the solvent that it is characterized in that electrolyte comprises propylene carbonate, ethylene carbonate, butylene carbonate, dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, 1, the group that 2-dimethoxy-ethane or its are constituted.
20. lithium secondary battery as claimed in claim 14 is characterized in that the solute of electrolyte comprises lithium perchlorate, LiBF4, lithium hexafluoro phosphate, trifluoromethyl sulfonic acid lithium, hexafluoroarsenate lithium.
21. lithium secondary battery as claimed in claim 14, it is characterized in that electrolyte is polymer dielectric, comprise the polyethylene oxygen alkane, polypropylene oxygen alkane, polyvinyl chloride or the Kynoar that contain one or more solubility lithium salts in lithium perchlorate, LiBF4, lithium hexafluoro phosphate, trifluoromethyl sulfonic acid lithium, the hexafluoroarsenate lithium.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100339384A CN100483798C (en) | 2005-03-31 | 2005-03-31 | Negative pole, its preparation method and lithium secondary battery using same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100339384A CN100483798C (en) | 2005-03-31 | 2005-03-31 | Negative pole, its preparation method and lithium secondary battery using same |
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| Publication Number | Publication Date |
|---|---|
| CN1841815A true CN1841815A (en) | 2006-10-04 |
| CN100483798C CN100483798C (en) | 2009-04-29 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315974B (en) * | 2007-06-01 | 2010-05-26 | 清华大学 | Lithium ionic cell cathode and method for producing the same |
| CN101409337B (en) * | 2007-10-10 | 2011-07-27 | 清华大学 | Lithium ion battery cathode, preparation method thereof and lithium ion battery applying the same |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4416200B2 (en) * | 1999-03-18 | 2010-02-17 | 富士通株式会社 | Solid electrolyte and battery using the same |
| SE518564C2 (en) * | 1999-12-20 | 2002-10-22 | Ericsson Telefon Ab L M | Polymer electrolyte, battery cell comprising the electrolyte, process for producing the electrolyte and use of the electrolyte and the battery cell |
| WO2004113443A1 (en) * | 2003-06-19 | 2004-12-29 | Daiso Co., Ltd. | Crosslinked polymer electrolyte and use thereof |
-
2005
- 2005-03-31 CN CNB2005100339384A patent/CN100483798C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101315974B (en) * | 2007-06-01 | 2010-05-26 | 清华大学 | Lithium ionic cell cathode and method for producing the same |
| CN101409337B (en) * | 2007-10-10 | 2011-07-27 | 清华大学 | Lithium ion battery cathode, preparation method thereof and lithium ion battery applying the same |
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| Publication number | Publication date |
|---|---|
| CN100483798C (en) | 2009-04-29 |
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