CA2123489A1 - Lithium secondary battery - Google Patents
Lithium secondary batteryInfo
- Publication number
- CA2123489A1 CA2123489A1 CA002123489A CA2123489A CA2123489A1 CA 2123489 A1 CA2123489 A1 CA 2123489A1 CA 002123489 A CA002123489 A CA 002123489A CA 2123489 A CA2123489 A CA 2123489A CA 2123489 A1 CA2123489 A1 CA 2123489A1
- Authority
- CA
- Canada
- Prior art keywords
- licoo2
- plane
- lithium secondary
- secondary battery
- ray diffraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/74—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by peak-intensities or a ratio thereof only
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
Abstract In order to improve a reversibility of LiCoO2 used for a positive active material of a lithium secondary battery, a peak strength of X-ray diffraction in (101) plane of LiCoO2 lies within a range of 5 to 15 when a peak strength of X-ray diffraction in (003) plane is 100.
Description
2~23~89 DESCRIPTION
Lithium secondary battery Tcchnical Field This invention relates to a lithium secondary battery, especially to its positive active material.
Background Art In resent years, studies have been carries actively on a lithium secondary battery and those having a working voltage of about 3V are now partially put in practical use. However, it can not be said that these lithium secondary batteries are provided with satisfactory characteristics with respect to energy density and service life.
Recently, batteries which utilize a positive active material having a working voltage of about 4V in order to increase the energy density and which utilize an organic burnt material as a negative electrode in order to prolong the service life, are reported and attract public attention.
The inventors begun investigations into 4V-group positive active materials having a working voltage of about 4V on the basis of consideration that, even when the service life was prolonged by utilizing the organic burnt material as the negative electrode, a battery having a high energy density could not be obtained if the working voltage of positive e~lectrode was not high. As the result, we came into conclusion that LiCoO2 shown by Mizushima et al., "Material Research Bulletin" vol. 15, pp. 783, 1980, was the favorable 4V-group positive active material in the present stage.
2 :1 2 ~ 3 However, the following problems have become clear from energetic studies on the LiCoO2. Although the LiCoO2 had a h:igh working voltage of about 4V and a high energy density, the reversibility of LiCoO2 was poor when it was subjected to deep charging and discharging. In other words, it was -d:ifficult to put the LiCoO2 into practical use as the positive active material of lithium secondary battery if the problem oE poor reversibility in the LiCoO2 was not improved.
An object of this invention is to improve the poor reversibility of LiCoO2 and to provide a lithium secondary battery having a large discharge capacity.
Disclosure of the Invention In a lithium secondary battery utilizing LiCoO2 as its positive active material, this invention is characterized by that a peak strength of X-ray diffraction in (101) plane of LiCoO2 lies within a range of 5 to 15 when a peak strength of X-ray diffraction in (003) plane is 100.
When the LiCoO2 is subjected to deep charging, a part of crystal structure changes to a discontinuous one. It can be considered that this change in crystal structure is a cause of the poor reversibility. It became clear from studies on the crystal structure that LiCoO2 prepared by an ordinary method, i.e. LiCoO2 obtained by mixing, burning and slowly cooling a raw material, had a high orientati~n to c-axis and its crystal grew remarkably in a direction of c-axis.
The inventors considered that the poor reversibility could be prevented when the crystal structure of high ~123~g9 orientation in c-axis was changed, so that we examined to optimize a superposition in c-axis direction and a spreading in a-axis direction. We found that LiCoO2 excellent in the reversibility and able to increase the discharge capacity could be obtained when the peak strength of X-ray diffraction in (101) plane able to represent the spreading in a-axis direction too, as mentioned above, lay within the range of 5 to 15, if the peak strength of X-ray diffraction in (003) plane representing the superposition in c-axis direction was l~DO.
The reason why the LiCoO2 excellent in the reversibility and able to increase the discharge capacity could be obtained is that an absolute value of change in crystal structure at time of charging can be restrained to a small by restraining the orientation in c-axis direction. In this case, the capacity will be decreased when the peak strength of X-ray diffraction in (101) plane in relation to (003) plane exceeds by excessively restraining the orientation in c-axis direction, and the reversibility will be decreased when the peak strength is smaller than 5.
Brief Description of the Drawinqs Fig. 1 is a characteristic diagram showing a discharge capacity of first cycle for a peak strength of X-ray diffraction in (101) plane in relation to (003) plane. Fig.
2 is a characteristic diagram showing a capacity retention -~
factor for a peak strenqth of X-ray diffraction in (101) plane in relation to (003) plane.
~ ' ~
2~3'~
Best Mode for Carrvinq Out the Invention LiCoO2 forming the positive active material was prepared first in the following way. Lithium carbonate and cobalt carbonate were weighed so as to attain a molar ratio 1 of Li t:o Co, and completely mixed while being ground in a ball mill.
q'he obtained mixture was put in an alumina crucible and t:emporarily burnt at 650C for 5 hours in air, and then burnt at 900C for 20 hours. Thereafter, it was cooled and ground t:o be used for active materials.
In the above preparation, seven kinds of active materials were obtained by controlling a cooling speed after burning.
All of these seven kinds of active materials were measured by Y-ray diffraction, and it was ensured that these materials were all LiCoO2. Seven kinds of LiCoO2 were denoted as A, B, C, D, E, F and G respectively, and peak strengths of X-ray diffraction of in (101) plane in relation to (003) plane (expressed as I1ol/Ioo3 hereunder) were measured for each.
]Results are shown in Table 1.
[Table 1]
Active material A B C D E F ¦ G
I,ol/Ioo3 3.1 5.2 6.9 10.1 13.4 18.6 ¦35.5 Coin type lithium batteries A through G were made as trial in the following way by using LiCoO2 A through G as the positive active material respectively.
In the first place, the positive electrode was obtained as follows. LiCoO2 powder, acetylene-black powder and `~ L 2 ~
polytetrafluoroethylene powder were mixed with a weight ratio of 85 to 10 to 5, and thoroughly kneaded after adding isopropyl alcohol to them. The obtained mixture was formed by a roll press into a sheet having a thickness of 0.8 mm and then punched to circular articles having a diameter of 16 mm, and it was heat treated at 200C for 15 hours. The positive electrode was used by being pressed against a positive electrode can attached with a current collector.
A negative electrode was obtained by punching a lithium foil having a thickness of 0.3 mm into circular article having a diameter of 15 mm. The negative electrode was used by being pressed against a negative electrode can through a current collector.
A material prepared by dissolving LiBF~ of 1 mol/l to ~-butylolactone was used for an electrolyte, and a fine porous membrane made of polypropylene was used for a separator.
A coin type lithium battery having a diameter of 20 mm and a thickness of 1.6 mm was made up by using the above-mentioned positive electrode, negative electrode, electrolyte and separator.
In the second place, charge/discharge cycle tests were p~erformed on the obtained batteries A through G, with test conditions: charge current of 3mA, charge end voltage!of 4.5V, ~;
discharge current of 3mA and discharge end voltage of 3.0V.
Fig. 1 and Fig. 2 are characteristic diagrams showing results of the above tests. Fig. 1 shows a discharge capacity at first cycle in relation to Ilol/Ioo3~ and Fig. 2 shows a .. ..
-' 212348~
capacity retention factor in relation to Ilol/Ioo3. The capacity retention factor was calculated by the following equation.
Discharge capacity at 50th cycle Capacity retention factor(~) = x 100 Discharge capacity at first cycle As seen from Fig. 1, the discharge capacity decreased when I10l/IO03 exceeded 15- As seen from Fig. 2, the reversibility lowered when Ilol/Ioo3 became lower than 5, and the discharge capacity decreased with the cycle.
Consequently, an optimum Ilol/Ioo3 for LiCoO2 excellent in the reversibility and able to increase the discharqe capacity was 5 to 15.
Since the LiCoO2 having an Ilol/Ioo3 ranging from 5 to 15 is used for the positive active material as described above, this invention can provide a lithium secondary battery which is excellent in its reversibility and has a large discharge capacity even when it is subjected to the deep charging and d.ischarging.
In this invention, the start material and manufacturing method of positive active material, the positive electrode, t.he negative electrode, the electrolyte, the separator and the battery shape etc. are not limited to those described in the a.bove best mode. For example, a material synthesized from hydroxides or oxides may be used for the positive active material, an organic burnt material may be used for the negative electrode, and a solid electrolyte may be used in 2 123~9 p:Lace of the electrolyte and the separator.
., ~
Lithium secondary battery Tcchnical Field This invention relates to a lithium secondary battery, especially to its positive active material.
Background Art In resent years, studies have been carries actively on a lithium secondary battery and those having a working voltage of about 3V are now partially put in practical use. However, it can not be said that these lithium secondary batteries are provided with satisfactory characteristics with respect to energy density and service life.
Recently, batteries which utilize a positive active material having a working voltage of about 4V in order to increase the energy density and which utilize an organic burnt material as a negative electrode in order to prolong the service life, are reported and attract public attention.
The inventors begun investigations into 4V-group positive active materials having a working voltage of about 4V on the basis of consideration that, even when the service life was prolonged by utilizing the organic burnt material as the negative electrode, a battery having a high energy density could not be obtained if the working voltage of positive e~lectrode was not high. As the result, we came into conclusion that LiCoO2 shown by Mizushima et al., "Material Research Bulletin" vol. 15, pp. 783, 1980, was the favorable 4V-group positive active material in the present stage.
2 :1 2 ~ 3 However, the following problems have become clear from energetic studies on the LiCoO2. Although the LiCoO2 had a h:igh working voltage of about 4V and a high energy density, the reversibility of LiCoO2 was poor when it was subjected to deep charging and discharging. In other words, it was -d:ifficult to put the LiCoO2 into practical use as the positive active material of lithium secondary battery if the problem oE poor reversibility in the LiCoO2 was not improved.
An object of this invention is to improve the poor reversibility of LiCoO2 and to provide a lithium secondary battery having a large discharge capacity.
Disclosure of the Invention In a lithium secondary battery utilizing LiCoO2 as its positive active material, this invention is characterized by that a peak strength of X-ray diffraction in (101) plane of LiCoO2 lies within a range of 5 to 15 when a peak strength of X-ray diffraction in (003) plane is 100.
When the LiCoO2 is subjected to deep charging, a part of crystal structure changes to a discontinuous one. It can be considered that this change in crystal structure is a cause of the poor reversibility. It became clear from studies on the crystal structure that LiCoO2 prepared by an ordinary method, i.e. LiCoO2 obtained by mixing, burning and slowly cooling a raw material, had a high orientati~n to c-axis and its crystal grew remarkably in a direction of c-axis.
The inventors considered that the poor reversibility could be prevented when the crystal structure of high ~123~g9 orientation in c-axis was changed, so that we examined to optimize a superposition in c-axis direction and a spreading in a-axis direction. We found that LiCoO2 excellent in the reversibility and able to increase the discharge capacity could be obtained when the peak strength of X-ray diffraction in (101) plane able to represent the spreading in a-axis direction too, as mentioned above, lay within the range of 5 to 15, if the peak strength of X-ray diffraction in (003) plane representing the superposition in c-axis direction was l~DO.
The reason why the LiCoO2 excellent in the reversibility and able to increase the discharge capacity could be obtained is that an absolute value of change in crystal structure at time of charging can be restrained to a small by restraining the orientation in c-axis direction. In this case, the capacity will be decreased when the peak strength of X-ray diffraction in (101) plane in relation to (003) plane exceeds by excessively restraining the orientation in c-axis direction, and the reversibility will be decreased when the peak strength is smaller than 5.
Brief Description of the Drawinqs Fig. 1 is a characteristic diagram showing a discharge capacity of first cycle for a peak strength of X-ray diffraction in (101) plane in relation to (003) plane. Fig.
2 is a characteristic diagram showing a capacity retention -~
factor for a peak strenqth of X-ray diffraction in (101) plane in relation to (003) plane.
~ ' ~
2~3'~
Best Mode for Carrvinq Out the Invention LiCoO2 forming the positive active material was prepared first in the following way. Lithium carbonate and cobalt carbonate were weighed so as to attain a molar ratio 1 of Li t:o Co, and completely mixed while being ground in a ball mill.
q'he obtained mixture was put in an alumina crucible and t:emporarily burnt at 650C for 5 hours in air, and then burnt at 900C for 20 hours. Thereafter, it was cooled and ground t:o be used for active materials.
In the above preparation, seven kinds of active materials were obtained by controlling a cooling speed after burning.
All of these seven kinds of active materials were measured by Y-ray diffraction, and it was ensured that these materials were all LiCoO2. Seven kinds of LiCoO2 were denoted as A, B, C, D, E, F and G respectively, and peak strengths of X-ray diffraction of in (101) plane in relation to (003) plane (expressed as I1ol/Ioo3 hereunder) were measured for each.
]Results are shown in Table 1.
[Table 1]
Active material A B C D E F ¦ G
I,ol/Ioo3 3.1 5.2 6.9 10.1 13.4 18.6 ¦35.5 Coin type lithium batteries A through G were made as trial in the following way by using LiCoO2 A through G as the positive active material respectively.
In the first place, the positive electrode was obtained as follows. LiCoO2 powder, acetylene-black powder and `~ L 2 ~
polytetrafluoroethylene powder were mixed with a weight ratio of 85 to 10 to 5, and thoroughly kneaded after adding isopropyl alcohol to them. The obtained mixture was formed by a roll press into a sheet having a thickness of 0.8 mm and then punched to circular articles having a diameter of 16 mm, and it was heat treated at 200C for 15 hours. The positive electrode was used by being pressed against a positive electrode can attached with a current collector.
A negative electrode was obtained by punching a lithium foil having a thickness of 0.3 mm into circular article having a diameter of 15 mm. The negative electrode was used by being pressed against a negative electrode can through a current collector.
A material prepared by dissolving LiBF~ of 1 mol/l to ~-butylolactone was used for an electrolyte, and a fine porous membrane made of polypropylene was used for a separator.
A coin type lithium battery having a diameter of 20 mm and a thickness of 1.6 mm was made up by using the above-mentioned positive electrode, negative electrode, electrolyte and separator.
In the second place, charge/discharge cycle tests were p~erformed on the obtained batteries A through G, with test conditions: charge current of 3mA, charge end voltage!of 4.5V, ~;
discharge current of 3mA and discharge end voltage of 3.0V.
Fig. 1 and Fig. 2 are characteristic diagrams showing results of the above tests. Fig. 1 shows a discharge capacity at first cycle in relation to Ilol/Ioo3~ and Fig. 2 shows a .. ..
-' 212348~
capacity retention factor in relation to Ilol/Ioo3. The capacity retention factor was calculated by the following equation.
Discharge capacity at 50th cycle Capacity retention factor(~) = x 100 Discharge capacity at first cycle As seen from Fig. 1, the discharge capacity decreased when I10l/IO03 exceeded 15- As seen from Fig. 2, the reversibility lowered when Ilol/Ioo3 became lower than 5, and the discharge capacity decreased with the cycle.
Consequently, an optimum Ilol/Ioo3 for LiCoO2 excellent in the reversibility and able to increase the discharqe capacity was 5 to 15.
Since the LiCoO2 having an Ilol/Ioo3 ranging from 5 to 15 is used for the positive active material as described above, this invention can provide a lithium secondary battery which is excellent in its reversibility and has a large discharge capacity even when it is subjected to the deep charging and d.ischarging.
In this invention, the start material and manufacturing method of positive active material, the positive electrode, t.he negative electrode, the electrolyte, the separator and the battery shape etc. are not limited to those described in the a.bove best mode. For example, a material synthesized from hydroxides or oxides may be used for the positive active material, an organic burnt material may be used for the negative electrode, and a solid electrolyte may be used in 2 123~9 p:Lace of the electrolyte and the separator.
., ~
Claims
1. A lithium secondary battery utilizing LiCoO2 as its positive active material, characterized by that a peak strength of X-ray diffraction in (101) plane of LiCoO2 lies within a range of 5 to 15 when a peak strength of X-ray diffraction in (003) plane is 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002123489A CA2123489A1 (en) | 1992-09-22 | 1992-09-22 | Lithium secondary battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002123489A CA2123489A1 (en) | 1992-09-22 | 1992-09-22 | Lithium secondary battery |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2123489A1 true CA2123489A1 (en) | 1994-03-31 |
Family
ID=4153585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002123489A Abandoned CA2123489A1 (en) | 1992-09-22 | 1992-09-22 | Lithium secondary battery |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA2123489A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000029331A1 (en) | 1998-11-13 | 2000-05-25 | Fmc Corporation | Layered lithium metal oxides free of localized cubic spinel-like structural phases and methods of making same |
| US6579475B2 (en) | 1999-12-10 | 2003-06-17 | Fmc Corporation | Lithium cobalt oxides and methods of making same |
-
1992
- 1992-09-22 CA CA002123489A patent/CA2123489A1/en not_active Abandoned
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000029331A1 (en) | 1998-11-13 | 2000-05-25 | Fmc Corporation | Layered lithium metal oxides free of localized cubic spinel-like structural phases and methods of making same |
| US6589499B2 (en) | 1998-11-13 | 2003-07-08 | Fmc Corporation | Layered lithium cobalt oxides free of localized cubic spinel-like structural phases and method of making same |
| US6620400B2 (en) | 1998-11-13 | 2003-09-16 | Fmc Corporation | Method of producing layered lithium metal oxides free of localized cubic spinel-like structural phases |
| US7074382B2 (en) | 1998-11-13 | 2006-07-11 | Fmc Corporation | Layered lithium metal oxides free of localized cubic spinel-like structural phases and methods of making same |
| US6579475B2 (en) | 1999-12-10 | 2003-06-17 | Fmc Corporation | Lithium cobalt oxides and methods of making same |
| US6932922B2 (en) | 1999-12-10 | 2005-08-23 | Fmc Corporation | Lithium cobalt oxides and methods of making same |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FZDE | Discontinued | ||
| FZDE | Discontinued |
Effective date: 19980922 |