Source: http://www.google.com/patents/US7541114?dq=5251294
Timestamp: 2017-04-28 06:35:55
Document Index: 377127546

Matched Legal Cases: ['Application No. 2007100081954', 'Application No. 2002', 'Application No. 2003', 'Application No. 2002', 'Application No. 10', 'Application No. 2000', 'application No. 2002']

Patent US7541114 - Anode active material, manufacturing method thereof, and non-aqueous ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsIn order to provide a 3V level non-aqueous electrolyte secondary battery with a flat voltage and excellent cycle life at a high rate with low cost, the present invention provides a positive electrode represented by the formula: Li2±α[Me]4O8−x, wherein 0≦α<0.4, 0≦x<2, and Me is a transition metal...http://www.google.com/patents/US7541114?utm_source=gb-gplus-sharePatent US7541114 - Anode active material, manufacturing method thereof, and non-aqueous electrolyte secondary batteryAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS7541114 B2Publication typeGrantApplication numberUS 10/506,298PCT numberPCT/JP2003/001997Publication dateJun 2, 2009Filing dateFeb 24, 2003Priority dateMar 1, 2002Fee statusPaidAlso published asEP1487039A1, EP1487039A4, US20050170250, WO2003075376A1Publication number10506298, 506298, PCT/2003/1997, PCT/JP/2003/001997, PCT/JP/2003/01997, PCT/JP/3/001997, PCT/JP/3/01997, PCT/JP2003/001997, PCT/JP2003/01997, PCT/JP2003001997, PCT/JP200301997, PCT/JP3/001997, PCT/JP3/01997, PCT/JP3001997, PCT/JP301997, US 7541114 B2, US 7541114B2, US-B2-7541114, US7541114 B2, US7541114B2InventorsTsutomu Ohzuku, Hiroshi Yoshizawa, Masatoshi Nagayama, Hizuru KoshinaOriginal AssigneePanasonic Corporation, Osaka City UniversityExport CitationBiBTeX, EndNote, RefManPatent Citations (101), Non-Patent Citations (42), Referenced by (37), Classifications (61), Legal Events (6) External Links: USPTO, USPTO Assignment, EspacenetAnode active material, manufacturing method thereof, and non-aqueous electrolyte secondary battery
In order to provide a 3V level non-aqueous electrolyte secondary battery with a flat voltage and excellent cycle life at a high rate with low cost, the present invention provides a positive electrode represented by the formula: Li2±α[Me]4O8−x, wherein 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, said active material exhibiting topotactic two-phase reactions during charge and discharge.
1. A positive electrode active material represented by the composition formula: Li2±α[Me]4O8−x, wherein 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, said active material exhibiting first and second topotactic two-phase reactions respectively during first and second stages of charge and discharge, and characterized in that the phase of the transition metal has a 2×2 superlattice.
(3) a step of subjecting the mixed compounds obtained by said step (2) to a first baking at a temperature of not less than 600° C.,
whereby a positive electrode active material represented by the formula: Li2±α[Me]4O8−x, where 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, said active material exhibiting first and second topotactic two-phase reactions respectively during first and second stages of charge and discharge is obtained.
17. The method for producing a positive electrode active material in accordance with claim 16, characterized in that said first baking is performed at a temperature of not less than 900° C.
19. The method for producing a positive electrode active material in accordance with claim 18, characterized in that said second baking is performed at a temperature of 350 to 950° C.
20. The method for producing a positive electrode active material in accordance with claim 18, characterized in that said second baking is performed at a temperature of 650 to 850° C.
22. The method for producing a positive electrode active material in accordance with claim 21, characterized in that said rapid cooling is performed at a temperature decrease rate of not less than 4.5° C./min.
24. The method for producing a positive electrode active material in accordance with claim 21, characterized in that said rapid cooling is performed at a temperature decrease rate of not less than 10° C./min.
For example, Japanese Laid-Open Patent Publication No. Hei 11-321951 proposes a positive electrode active material represented by the formula: Li(1+x)Mn(2−x−y)MyOz, where 0≦x≦0.2, 0.2≦y≦0.6, 3.94≦z≦4.06, and M is nickel or a compound composed of nickel as an essential component and at least one selected from aluminum and transition elements, and a method for synthesizing the positive electrode active material without an impurity of NiO. To be specific, a mixture comprising a manganese compound and a metal M compound is baked at 900 to 1100° C., and the mixture is baked again with a lithium compound.
This method, however, involves a reaction between manganese and a metal M, that is, a reaction between solids. Accordingly, it is difficult that the above two is incorporated uniformly. In addition, since the baking is performed at a high temperature of not less than 900° C., reactivity with lithium is reduced after the baking, making it difficult to obtain the desired positive electrode active material.
The present invention relates to a positive electrode active material represented by the composition formula: Li2±α[Me]4O8−x, where 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, the material exhibiting topotatic two-phase reactions during charge and discharge.
The phase of the transition metal preferably has a 2×2 superlattice in the positive electrode active material.
The present invention relates to a method for producing a positive electrode active material comprising: (1) a step of mixing Mn and a compound containing at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu to give a raw material mixture; or a step of synthesizing a eutectic compound containing a Mn compound and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu; (2) a step of mixing the raw material mixture or eutectic compound with a lithium compound; and (3) a step of subjecting the compound obtained by the step (2) to a first baking at a temperature of not less than 600° C., whereby a positive electrode active material represented by the formula: Li2±α[Me]4O8−x, where 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, said material exhibiting topotatic two-phase reactions during charge and discharge is obtained.
The first baking is preferably performed at a temperature of not less than 900° C.
In this case, the second baking is preferably performed at a temperature of 350 to 950° C.
More preferably, the second baking is performed at a temperature of 650 to 850° C.
The rapid cooling is preferably performed at a temperature decrease rate of not less than 4.5° C./min, more preferably at a temperature decrease rate of not less than 10° C./min.
FIG. 1 shows graphs illustrating the electrochemical characteristics of positive electrode active materials obtained by baking the mixture of a eutectic compound and a lithium compound in air at temperatures of 1000° C. (a), 900° C. (b), 800° C. (c), 700° C. (d) and 600° C. (e) for 12 hours (first baking).
FIG. 3 shows the charge/discharge curves of a positive electrode active material in accordance with the present invention obtained by the first baking at 1000° C. for 12 hours and then the second baking at 700° C. for 48 hours.
The present invention relates to a positive electrode active material represented by the composition formula: Li2±α[Me]4O8−x, were 0≦α<0.4, 0≦x<2, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu, the material exhibiting topotatic two-phase reactions during charge and discharge. The composition formula preferably satisfies 0≦x<1.3.
FIG. 1 shows graphs illustrating the electrochemical characteristics of the positive electrode active materials obtained by baking the mixture of the eutectic compound and the lithium compound in air at temperatures of 1000° C. (a), 900° C. (b), 800° C. (c), 700° C. (d) and 600° C. (e) for 12 hours (first baking). Specifically, [Ni1/4Mn3/4](OH)2 obtained through a eutectic reaction and LiOH.H2O were thoroughly mixed to give a mixture, which was then formed into pellets and the resulting formed product was baked to give a Li[Ni1/2Mn3/2]O4.
First, 80 parts by weight of Li[Ni1/2Mn3/2]O4, 10 parts by weight of acetylene black as a conductive agent and 10 parts by weight of polyvinylidene fluoride (PVdF) as a binder were mixed to give a mixture, which was then diluted with N-methyl-2-pyrrolidone (NMP) to give a paste. The paste was applied onto a current collector made of aluminum foil. The current collector with the paste applied was dried in a vacuum at 60° C. for 30 minutes, which was then cut into 15 mm×20 mm pieces. Subsequently, the cut piece of current collector was further dried in a vacuum at 150° C. for 14 hours to give a test electrode.
Lower limit: 600° C., preferably 900° C. Upper limit: 1000° C. Time: 2 to 72 hours Cooling rate
Lower limit: 4.5° C./min. Upper limit: 10° C./min.
FIG. 2 shows the TG curve (thermogravimetric analysis) of a positive electrode active material after the first baking. The positive electrode active material used here was obtained by baking Li[Ni1/2Mn3/2]O4 at a low temperature of 500° C. This positive electrode active material was heated with the temperature increased by 50° C. from 700 to 850° C. The positive electrode active material was held at each temperature and the temperature was increased stepwise. When the temperature was decreased, the temperature was controlled in the same manner. The temperature increase rate was 10° C./min. and the ambient atmosphere was air.
In FIG. 2, “a” represents temperature, “b” represents weight change when the temperature was increased, and “c” represents weight change when the temperature was decreased. In FIG. 2, there is observed a random weight reduction, which is considered to be due to moisture. In the temperature increase from 400 to 1000° C., the weight monotonously decreased in the range of 700 to 1000° C. On the other hand, when the weight change when the temperature was decreased is observed, the weight was increased (recovered) in an amount equal to the amount of weight decreased, following the rate of this experiment. It is apparent that the weight was almost completely recovered although the rate was slower until 700° C. This weight increase is presumed to be because oxygen once released at a high temperature returned to the positive electrode active material by re-baking (second baking), in other words, by reoxidation of the positive electrode active material. Accordingly, it suggests that the temperature of the positive electrode active material obtained after the first baking is preferably decreased at a rate of not greater than 10° C./min.
Then, the charge/discharge curves of the positive electrode active material obtained by the first baking at 1000° C. for 12 hours and then the second baking at 700° C. for 48 hours are shown in FIG. 3. The results show that the positive electrode active material has a charge/discharge capacity of about 135 mAh/g, a voltage difference of about 15 mAh/g at around 4 V, and excellent polarization characteristics.
As described above, it is even possible to control the voltage difference at around 4 V in the positive electrode active material, which is obtained by baking at a high temperature of 1000° C. (first baking), by re-baking (second baking) the positive electrode active material, for example, at a lower temperature of 700° C. like the positive electrode active material baked at 700° C. as shown in FIG. 1.
Since the positive electrode active material subjected to the first and second bakings has been baked at 1000° C. once, it possesses grown crystalline particles having no micropores and therefore has a high packing density. In addition, this positive electrode active material is superior in polarization characteristics.
First baking Lower limit: 600° C., preferably 900° C.
Upper limit: 1000° C. Time: 2 to 72 hours Second baking Lower limit: 350° C., preferably 650° C.
Upper limit: 950° C., preferably 850° C. Time: 2 to 72 hours From the results and the electrochemical characteristics evaluation shown in FIG. 2, it is clear that it is preferred that the first baking is performed at 600 to 1000° C. or more, preferably 900 to 1000° C., the temperature is rapidly cooled to 350 to 950° C., and then the second baking is performed at 350 to 950° C., preferably 650 to 850° C.
It is possible to improve the polarization characteristics of the positive electrode active material to be obtained and, at the same time, to appropriately control the difference that appears at around 4 V in the charge/discharge curves. In the above experiment, the temperature increase rate during baking was 7.5° C./min. and the temperature decrease rate was 4.5° C./min.
In view of this, the present inventors extensively studied the preferred particle morphology of the positive electrode active material in accordance with the present invention and the control of the particle morphology thereof. As previously stated, in the method for producing the positive electrode active material in accordance with the present invention, it is preferred to perform the first baking at a high temperature (not less than 900° C.) and then the second baking intended for reoxidation.
Accordingly, a cross-section image of a particle of the positive electrode active material in accordance with the present invention obtained by the first baking at 1000° C. for 12 hours and the second baking at 700° C. for 48 hours was taken by SEM. The obtained SEM image is shown in FIG. 4( a) (magnification: 300000 times). FIG. 4( b) shows an SEM image of a positive electrode active material obtained in the same manner as the positive electrode active material of FIG. 4( a) was obtained, except that the second baking was not performed.
From FIG. 4, it is clear that the crystalline particle of the positive electrode active materials is well grown because they were once baked at 1000° C. It is also clear that the particle has no micropores inside thereof, and therefore is a particle with a high packing density although it is a primary particle with a size of 2 to 3 μm.
The first baking was performed by increasing the temperature from room temperature to 1000° C. for about 3 hours and holding the temperature at 1000° C. for 12 hours. After the first baking, the temperature was decreased from 1000° C. to room temperature for 2 hours (cooling rate of 8° C. /min.).
The first baking was performed by increasing the temperature from room temperature to 1000° C. for about 3 hours and holding the temperature at 1000° C. for 12 hours. The second baking was performed by decreasing the temperature from 1000 to 700° C. for 30 minutes and holding the temperature at 700° C. for 48 hours.
After the second baking, the temperature was decreased from 700° C. to room temperature for 1.5 hours (cooling rate of 7.5° C./min.).
The first baking was performed by increasing the temperature from room temperature to 1000° C. for about 3 hours and holding the temperature at 1000° C. for 12 hours. After the first baking, the temperature was rapidly cooled from 1000° C. to room temperature.
The second baking was performed by increasing the temperature to 700° C. for about 1 hour and holding the temperature at 700° C. for 48 hours.
After the second baking, the temperature was decreased from 700° C. to room temperature for 1.5 hours.
Roughly classified, Cases 3 and 4 included a rapid cooling step while Cases 2 and 3 included a reoxidation (second baking) step at 700° C.
10° C./min. or more, preferably 20° C./min. or more, most preferably 50° C./min. or more Second baking
Lower limit: 350° C., preferably 650° C. Upper limit: 950° C., preferably 850° C. Time: 2 to 72 hours
In terms of crystal structure, the positive electrode active material in accordance with the present invention has a spinel-framework-structure. FIG. 9 shows the X-ray diffraction patterns of the positive electrode active materials in accordance with the present invention produced at different temperatures in the first baking. In FIG. 9, (a) to (e) show the X-ray diffraction patterns of the positive electrode active materials produced by the first baking at 600° C., 700° C., 800° C., 900° C. and 1000° C., respectively. The composition of the positive electrode active material was Li [Ni1/2Mn3/2]O4.
Then, the FT-IR analysis results of the positive electrode active material shown by (a) to (e) in FIG. 9 are shown by (a) to (e) in FIG. 10. Eight sharp peaks are observed in the case (b) of the positive electrode active material obtained at 700° C., and it is obvious that the peaks become broad in both cases of over 700° C. and less than 700° C. This indicates that the fist baking at 700° C. is preferred in terms of crystal arrangement.
It can be said that the positive electrode active material in accordance with the present invention has the formula: Li2±α[Me]4O8−x, where 0≦α<0.4, 0≦x<2, preferably 0≦x<1.3, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu. In the following, an explanation is given using a specific example in which α is set to 0 (α=0) in order to make it easier to understand.
When the X-ray diffraction pattern of the sample of the positive electrode active material produced by the first baking and the rapid cooling (without the second baking, in other words, without reoxidation) is analyzed, it was found that the X-ray diffraction pattern could be well fitted by assuming that Me was present in the 8a sites at about 1/5, in the 16c sites at 2/5 and in the 16d sites at 7/4. From this, it is presumed that the oxygen in the spinel structure leaves as the temperature is increased to 1000° C., thereby the transition metal is reduced and considerable amounts of lithium element and transition metal element respectively move to the 8a sites and 16c sites. Because of this phenomenon, a rock-salt-type-structure is formed in a part of the spinel structure of the positive electrode active material in accordance with the present invention.
Further, the X-ray diffraction patterns shown in FIG. 11 indicate that the rock-salt-type-structures reversibly return to the spinel structures by the reoxidation (second baking) in the positive electrode active material (a) which was obtained by the first baking, the rapid cooling and the reoxidation (second baking) at 700° C., and the positive electrode active material (c) which was obtained by the first baking (1000° C.), and subsequently the reoxidation (second baking) at a lower temperature of 700° C. Such flexible crystal structures of the positive electrode active material contribute to the stability of the crystal structure in the case where a stress is given to the positive electrode active material due to high rate charge/discharge cycles; as a result, presumably a long life can be achieved.
Now, an explanation is given on α and x values in the composition formula: Li2±α[Me]4O8−x, where 0≦α<0.4, 0≦x<2, preferably 0≦x<1.3, and Me is a transition metal containing Mn and at least one selected from the group consisting of Ni, Cr, Fe, Co and Cu.
α value is an element to be changed to control the particle growth. If the a value is less than 2 in the stoichiometric composition, it is possible to control the particle growth during the synthesis, and the surface area is likely to be increased. Conversely, if the α value is greater than that, it is possible to facilitate the particle growth. Accordingly, in the case of designing the particles according to the characteristics required for a battery, the particle growth can be controlled by changing the composition ratio of lithium. The range of the α value is substantially about ±0.4. If the range (range of variation) exceeds this value, the inherent function of the positive electrode active material could be harmed.
On the other hand, as previously stated, since the positive electrode active material obtained by the first baking at 1000° C. and the rapid cooling is represented by Li1.2Me2.4O4, the x value can be calculated to be 1.33. The x can be considered to be 2 because the amount of oxygen returns to the stoichiometric composition by reoxidation (second baking). However, the upper limit of the x is practically 1.3. In view of these facts, especially the fact that oxygen returns by the reoxidation, the present inventors set the x range to be 0≦x<1.3.
From the capacity and the shape of the discharge curves, it was found that the most preferred ratio between Mn and the other transition metal element was substantially 3:1. Although the specific cause thereof is not known, it is presumed that, when the ratio is 3:1, the transition metal phases in the framework of the spinel structure can form a superlattice of [2×2] and this effect has some influence thereon. From the electron beam diffraction analysis, superlattice spots are observed in this direction, so that the formation of the superlattice of [2×2] can be confirmed.
Contrary to the above, it is also possible to prevent this difference from appearing. FIG. 20 shows an example thereof. It is apparent that any clear difference did not appear even after the load was increased. The positive electrode active material used here was prepared by the first baking at 1000° C. and the second baking (reoxidation) at 700° C. Additionally, (a) to (e) in FIG. 20 respectively represent discharge behaviors at a current density of 0.17 mA/cm2, 0.33 mA/cm2, 1.0 MA/cm2, 1.67 mA/cm2 and 3.33 mA/cm2.
In such cases, in the above-mentioned porous film having micropores, needle-like metal deposits can be suppressed by physical force, whereas, in a separator with larger micropores such as non-woven fabric, a micro short-circuit occurs in a short period of time. Further, separators have a shutdown function to suppress the increase of battery temperature at the time of overcharging in order to secure the safety against overcharging in the case where a charger is out of order. The function is to stop the current between electrodes by crushing the micropores of a separator when the temperature reaches a certain temperature (about 135° C.). For the above reason, an expensive porous film has been used in a conventional LiCoO2/graphite type battery.
The preferred binder to be used in the positive electrode material mixture of the present invention is a polymer with a decomposition temperature of 300° C. or more. Examples thereof include polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), tetrafluoroethylene-hexafluoroethylene copolymer, tetrafluoroethylene-hexafluoropropylene copolymer (FEP), tetrafluoroethylene-perfluoroalkylvinylether copolymer (PFA), vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-chlorotrifluoroethylene copolymer, ethylene-tetrafluoroethylene copolymer (ETFE resin), polychlorotrifluoroethylene (PCTFE), vinylidene fluoride-pentafluoropropylene copolymer, propylene-tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer (ECTFE), vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer and vinylidene fluoride-perfluoromethylvinylether-tetrafluoroethylene copolymer. They may be used singly or in any arbitrary combination thereof within the scope that does not impair the effect of the present invention.
The binder used in the negative electrode material mixture may be a thermoplastic resin or a thermosetting resin, and preferred is a polymer with a decomposition temperature of 300° C. or higher. Examples include polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), styrene-butadiene rubber, tetrafluoroethylene-hexafluoropropylene copolymer (FEP), tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), vinylidene fluoride-hexafluoropropylene copolymer, vinylidene fluoride-chlorotrifluoroethylene copolymer, ethylene-tetrafluoroethylene copolymer (ETFE resin), polychlorotrifluoroethylene (PCTFE), vinylidene fluoride-pentafluoropropylene copolymer, propylene-tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer (ECTFE), vinylidene fluoride-hexafluoropropylene-tetrafluoroethylene copolymer and vinylidene fluoride-perfluoromethyl vinyl ether-tetrafluoroethylene copolymer. Styrene-butadiene rubber, polyvinylidene fluoride, styrene-butadiene rubber and the like can also be used.
As the separator, a non-woven fabric is particularly preferred as previously mentioned when a titanium oxide such as Li4Ti5O12(Li[Li1/3Ti5/3]O4) is used in the negative electrode active material. When a negative electrode active material other than the above is used, the following can be used. An insulating microporous thin film with high ion permeability and a certain mechanical strength can be used. The film preferably has the function of closing the pores and increasing the resistance at a temperature of 80° C. or higher. From the viewpoint of the resistance to an organic solvent and hydrophobicity, there is used a sheet or a non-woven fabric made of polypropylene, polyethylene, an olefin polymer prepared by combining the above, or glass fiber.
The pressing temperature is preferably from room temperature to 200° C. The ratio of the width of the positive electrode sheet to that of the negative electrode sheet is preferably 0.9 to 1.1, and more preferably 0.95 to 1.0.
The ambient temperature was increased from room temperature to 1000° C. for about 3 hours, maintained at 1000° C. for 12 hours and then decreased from 1000° C. to room temperature for 2 hours.
The ambient temperature was increased from room temperature to 1000° C. for about 3 hours, maintained at 1000° C. for 12 hours, decreased from 1000° C. to 700° C. for 30 minutes, maintained at 700° C. for 48 hours and then decreased from 700° C. to room temperature for 1.5 hours.
The ambient temperature was increased from room temperature to 1000° C. for about 3 hours, maintained at 1000° C. for 12 hours and rapidly cooled from 1000° C. to room temperature. Then, the ambient temperature was increased to 700° C. for about 1 hour, maintained at 700° C. for 48 hours and decreased from 700° C. to room temperature for 1.5 hours.
The electrochemical behaviors of the positive electrode active materials obtained in Production Examples 1 to 3 are shown as (a) to (c) in FIG. 22. Form FIG. 22, it is understood that all of the positive electrode active materials show small polarization and a flat charge/discharge curve. The positive electrode active material (a) of Production Example 1 exhibits a voltage difference at the end of discharging, which can be utilized for the detection of the remaining capacity. The difference is as small as only several V, so that the effective detection of remaining capacity can be achieved without the occurrence of a power-down due to lack of energy when it is used in a device. The positive electrode active material (b) obtained through the reoxidation at 700° C. does not show the difference. This shows that the voltage difference at the end of discharging can be freely controlled in this range by controlling the temperature and time of the reoxidation process. Similarly, the positive electrode active material (c) obtained through the rapid cooling process first and then the reoxidation process does not show the difference. This shows that a material with enhanced polarization and flatness can be obtained by controlling particles as previously stated in the rapid cooling process. Additionally, high density filling can be achieved.
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X. et al., "Spinel Li[Li1/3Ti5/3]O4 as an anode material for lithium ion batteries" Energy Storage Materials Program, Institute for Superconducting and Electronic Materials, University of Wollongong, accepted Apr. 27, 1999.40West et al., "Introduction for Solid-State Chemistry," Kodansha-Scientific, Mar. 20, 1996, with partial translation.41Yoshio et al., "Lithium-ion Secondary Battery," Nikkan Kogyo Shinbunsha, Mar. 29, 1996, with partial translation.42Yoshio, M. et al., "Preparation and properties of LiCoyMnxNi1-x-yO2 as a chathode for lithium ion batteries," Journal of Power Sources, Aug. 17, 1998, p. 176-181, vol. 90, Elsevier.* Cited by examinerReferenced byCiting PatentFiling datePublication dateApplicantTitleUS7740985Apr 23, 2009Jun 22, 2010Medtronic, Inc.Lithium-ion batteryUS7794869Jul 29, 2009Sep 14, 2010Medtronic, Inc.Lithium-ion batteryUS7803481Sep 25, 2009Sep 28, 2010Medtronic, Inc,Lithium-ion batteryUS7807299Oct 29, 2004Oct 5, 2010Medtronic, Inc.Lithium-ion batteryUS7811705Oct 29, 2004Oct 12, 2010Medtronic, Inc.Lithium-ion batteryUS7816036Sep 9, 2002Oct 19, 2010Panasonic CorporationPositive electrode active material and non-aqueous electrolyte secondary cell comprising the sameUS7858236Jul 28, 2009Dec 28, 2010Medtronic, Inc.Lithium-ion batteryUS7875389 *May 21, 2009Jan 25, 2011Medtronic, Inc.Lithium-ion batteryUS7879495Oct 29, 2004Feb 1, 2011Medtronic, Inc.Medical device having lithium-ion batteryUS7883790Sep 22, 2009Feb 8, 2011Medtronic, Inc.Method of preventing over-discharge of batteryUS7927742 *Sep 29, 2008Apr 19, 2011Medtronic, Inc.Negative-limited lithium-ion batteryUS7931987May 27, 2010Apr 26, 2011Medtronic, Inc.Lithium-ion batteryUS8105714Jul 13, 2007Jan 31, 2012Medtronic, Inc.Lithium-ion batteryUS8178242Apr 6, 2011May 15, 2012Medtronic, Inc.Lithium-ion batteryUS8383269Apr 13, 2011Feb 26, 2013Medtronic, Inc.Negative-limited lithium-ion batteryUS8785046Aug 26, 2010Jul 22, 2014Medtronic, Inc.Lithium-ion batteryUS8980453Apr 30, 2008Mar 17, 2015Medtronic, Inc.Formation process for lithium-ion batteriesUS9065145Jul 13, 2007Jun 23, 2015Medtronic, Inc.Lithium-ion batteryUS9077022Dec 6, 2010Jul 7, 2015Medtronic, Inc.Lithium-ion batteryUS9115004 *Jun 11, 2012Aug 25, 2015Samsung Sdi Co., Ltd.Negative active material, negative electrode including the same, lithium secondary battery including negative electrode, and method of preparing negative active materialUS9287580Jul 27, 2011Mar 15, 2016Medtronic, Inc.Battery with auxiliary electrodeUS9391325 *May 11, 2006Jul 12, 2016Panasonic CorporationPositive electrode active material, production method thereof and non-aqueous electrolyte secondary batteryUS9587321Mar 31, 2015Mar 7, 2017Medtronic Inc.Auxiliary electrode for lithium-ion batteryUS20060275664 *May 11, 2006Dec 7, 2006Tsutomu OhzukuPositive electrode active material, production method thereof and non-aqueous electrolyte secondary batteryUS20080044728 *Jul 13, 2007Feb 21, 2008Medtronic, Inc.Lithium-ion batteryUS20090208845 *Apr 23, 2009Aug 20, 2009Medtronic, Inc.Lithium-ion batteryUS20090286151 *May 21, 2009Nov 19, 2009Medtronic, Inc.Lithium-ion batteryUS20090286158 *Jul 28, 2009Nov 19, 2009Medtronic, Inc.Lithium-ion batteryUS20100009245 *Jul 29, 2009Jan 14, 2010Medtronic,Inc.Lithium-ion batteryUS20100015528 *Sep 25, 2009Jan 21, 2010Medtronic, Inc.Lithium-ion batteryUS20100076523 *Sep 22, 2009Mar 25, 2010Medtronic, Inc.Method of preventing over-discharge of batteryUS20100279155 *Apr 30, 2009Nov 4, 2010Medtronic, Inc.Lithium-ion battery with electrolyte additiveUS20130004851 *Jun 11, 2012Jan 3, 2013Samsung Sdi Co., Ltd.Negative active material, negative electrode including the same, lithium secondary battery including negative electrode, and method of preparing negative active materialWO2014165748A1Apr 4, 2014Oct 9, 2014E. 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Du Pont De Nemours And CompanyNonaqueous electrolyte compositions comprising lithium oxalato phosphates* Cited by examinerClassifications U.S. Classification429/322, 429/231.95, 429/224, 429/218.1International ClassificationH01M10/0569, H01M4/505, H01M4/525, H01M10/0525, H01M4/131, H01M10/05, H01M4/485, C01G45/00, C01G37/00, C01G51/00, C01G49/00, H01M4/66, H01M10/42, C01G53/00Cooperative ClassificationC01P2002/82, C01P2004/80, H01M2010/4292, H01M2004/027, H01M2004/021, H01M10/0585, H01M10/0562, H01M10/0525, H01M4/661, H01M4/5825, H01M4/525, H01M4/505, H01M4/485, H01M4/136, H01M4/131, C01P2004/62, C01P2004/03, C01P2002/88, C01P2002/77, C01P2002/76, C01P2002/74, C01P2002/32, C01G53/54, C01G51/54, C01G49/0072, C01G45/1235, C01G37/006, C01G23/005, H01M10/052, C01P2006/40, C01P2004/61, C01P2002/72European ClassificationC01G23/00F2, C01G45/12C4, C01G49/00C12, C01G51/54, C01G53/54, H01M4/58D, H01M4/525, C01G37/00D, H01M4/131, H01M4/505, H01M4/485Legal EventsDateCodeEventDescriptionSep 1, 2004ASAssignmentOwner name: MATSUSHITA ELECTRIC INDUSTRIAL CO., LTD., JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:OHKUKU, TSUTOMU;YOSHIZAWA, HIROSHI;NAGAYAMA, MASATOSHI;AND OTHERS;REEL/FRAME:016484/0073;SIGNING DATES FROM 20040609 TO 20040614Owner name: OSAKA CITY, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:OHKUKU, TSUTOMU;YOSHIZAWA, HIROSHI;NAGAYAMA, MASATOSHI;AND OTHERS;REEL/FRAME:016484/0073;SIGNING DATES FROM 20040609 TO 20040614Apr 25, 2006ASAssignmentOwner name: OSAKA CITY UNIVERSITY, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:OSAKA CITY;REEL/FRAME:017841/0408Effective date: 20060401May 9, 2006ASAssignmentOwner name: OSAKA CITY UNIVERSITY, JAPANFree format text: CORRECTIVE COVERSHEET TO CORRECT THE SPELLING OF THE FIRST AND LAST INVENTORS PREVIOUSLY RECORDED ON REEL/FRAME 016484/0073.;ASSIGNORS:OHZUKU, TSUTOMU;YOSHIZAWA, HIROSHI;NAGAYAMA, MASATOSHI;AND OTHERS;REEL/FRAME:017601/0803;SIGNING DATES FROM 20040609 TO 20040614Owner name: MATSUSHITA ELECTRIC INDUSTRIAL CO., LTD., JAPANFree format text: CORRECTIVE COVERSHEET TO CORRECT THE SPELLING OF THE FIRST AND LAST INVENTORS PREVIOUSLY RECORDED ON REEL/FRAME 016484/0073.;ASSIGNORS:OHZUKU, TSUTOMU;YOSHIZAWA, HIROSHI;NAGAYAMA, MASATOSHI;AND OTHERS;REEL/FRAME:017601/0803;SIGNING DATES FROM 20040609 TO 20040614Nov 18, 2008ASAssignmentOwner name: PANASONIC CORPORATION, JAPANFree format text: CHANGE OF NAME;ASSIGNOR:MATSUSHITA ELECTRIC INDUSTRIAL CO., LTD.;REEL/FRAME:021851/0224Effective date: 20081001Owner name: PANASONIC CORPORATION,JAPANFree format text: CHANGE OF NAME;ASSIGNOR:MATSUSHITA ELECTRIC INDUSTRIAL CO., LTD.;REEL/FRAME:021851/0224Effective date: 20081001Oct 1, 2012FPAYFee paymentYear of fee payment: 4Nov 17, 2016FPAYFee paymentYear of fee payment: 8RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services