Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Priority
Acknowledgement has been made of applicant’s claim for priority under 35 USC 119 (a-d). The certified copy has been filed on 5/8/2024.
Information Disclosure Statement
An Information Disclosure Statement (IDS) has not been filed as of the mailing of this Office Action.
Drawings
The drawings received 5/8/2024 are acceptable for examination purposes.
Claim Rejections - 35 USC § 103
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
Claim(s) 1, 2, 4-10 are rejected under 35 U.S.C. 103 as being unpatentable over Park (US 2020/0006762) in view of Yang (CN 110190276), Wang (CN 103474655), Ding (CN 108832103), and Kawakita (WO 2020/174937, using US 2022/0033276 as translation).
Park discloses a preparation method for a high-nickel ternary cathode material, comprising the following steps of:
mixing a LiOH powder with a high-nickel ternary precursor according to a molar ratio of (0.6 to 0.95): 1, and performing primary sintering in an oxygen atmosphere to obtain a primary- sintered material ([0023, 0024, 0046] and see (M1, L1 and F1 in Figure 1).
Regarding claim 4, Park discloses the secondary sintering is performed at a temperature of 700 °C to 1,000 °C; and the secondary sintering is performed in an oxygen atmosphere [0026].
Regarding claim 1, Park discloses performing secondary sintering on the powder material to obtain a secondary-sintered material comprised a further addition of LiOH and a metal oxide additive such as W (tungsten) [0026, 0020], but does not disclose that the further addition of LiOH and a metal oxide was performed by adding a metal oxide into a LiOH solution to obtain a mixed solution, wherein the metal oxide is at least one of oxides of Mo, W or Sn; mixing the mixed solution with the primary-sintered material in a protective atmosphere to obtain a mixed material. Yang teaches a method of making a doped positive electrode active material by adding a lithium source Li2CO3 and dopants aluminum-source and niobium-source into ethanol to uniformly disperse the contents. The mixture is further mixed with a suspension of transition metal oxide precursors to be heat treated. (page3-4 of translation). It would have been obvious to one of ordinary skilled in the art at the time the invention was made to mix the LiOH and tungsten oxide of Park in a solution, as taught by Yang, to mix with the high-nickel ternary precursor of Park for the benefit of ensuring good distribution of the doping metal.
Regarding claim 1, drying and crushing the mixed material to obtain a power material, Yang teaches drying the active material slurry before the heat treatment, but does not teach crushing the dried mixture. Wang teaches making a positive active material electrode comprising mixing the metal precursors in liquid, and drying the obtained precipitate, performing heat treatment at high temperature, and crushing to obtain the final product. See Wang’s claim 1. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to crush the active material of Park before the second sinter, as taught by Wang, for the benefit of controlling the particle size.
Regarding claim 1, Park discloses a coating comprising boron (step A1 and A2 and [0027] of Park), but does not disclose spraying an atomized boric acid alcohol solution onto the secondary-sintered material. Ding teaches a ternary positive electrode material and its preparing method and application, covering a high-nickel ternary positive electrode material surface of the adhesion layer, the adhesion layer composed of boric acid coated on the high-nickel ternary positive electrode material surface spraying the boric acid solution to form coating the high-nickel ternary positive electrode material surface. The positive electrode material of the invention can realize the excellent balance of circulating, rate, safety and high voltage application performance. See Abstract. The method is good for forming a uniform coating of boron (page 5 of translation). It would have been obvious to one of ordinary skilled in the art at the time the invention was made to spray the application of coating comprising boron, as taught by Ding, for the benefit of forming a uniform coating layer.
Ding teaches that the high-nickel ternary positive electrode material and the mass ratio of the boric acid is 1: 0.0002-0.02 (page 5 of translation). Given the small amount of boric acid, it would have been obvious to one of ordinary skilled in the art at the time the invention was made to form the spray of boric acid in smallest droplets possible, and hence in an atomized sprayer, for the benefit of forming as uniform a coating a possible.
Regarding claim 7, a preparation process of the boric acid alcohol solution comprises: adding a boric acid into an alcohol solution to obtain a mixture and heating the mixture in water bath to obtain the boric acid alcohol solution; and the heating in water bath is performed at a temperature of 50 °C to 70 °C, Ding teaches dissolving boric acid in ethyl alcohol at a concentration of 1:10 mass ratio, adding the liquid storage tank of the spraying device (page 5 of translation). It would have been obvious to one of ordinary skilled in the art at the time the invention was made to heat the solution of boric acid of Ding for the benefit of trying the easily dissolve the boric acid in the solution.
Regarding claim 8, a concentration of B in the boric acid alcohol solution ranges from 15 g/L to 25 g/L, Ding teaches dissolving boric acid in ethyl alcohol at a concentration of 1:10 mass ratio, adding the liquid storage tank of the spraying device (page 5 of translation). It would have been obvious to one of ordinary skilled in the art at the time the invention was made to adjust the concentration of the boric acid in the solution for the benefit of forming a concentration that is easy to spray.
Regarding claim 9, a content of boron in the high- nickel ternary cathode material ranges from 0.02wt% to 0.5wt%, Park teaches that a surface coating stabilizes the surface against unwanted side reaction between the electrolyte and cathode during cycling [0006]. Ding teaches that the amount of boron in the cathode active material is 0.0035% to 0.35 mass%. The positive electrode material of the invention can realize the excellent balance of circulating, rate, safety and high voltage application performance. See Abstract. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to adjust the amount of boron in the active material of Park modified by Yang, Wang, and Ding, for the benefit of having a protected surface against unstable electrolyte.
Regarding claim 1, then tempering to obtain the high-nickel ternary cathode material, Ding teaches sintering the boron coated product to sinter at 400C in air (page 6 of translation). Kawakita teaches forming a coating of boron on a positive active material lithium containing transition metal oxide. Regarding claim 10, Kawakita teaches the tempering is performed in an oxygen atmosphere; and the tempering is performed at a temperature of 200 °C to 350 0C [0052]. Kawakita notes that the heat treatment temperature is higher than the melting point of the boron compound, and hence, it is able to melt the boron compound at this temperature range [0021]. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to heat treat the boron-coated positive active material, as taught by Kawakita, for the benefit of heat treating the active material with a boron compound of Park modified by Yang, Wang, and Ding, as taught by Kawakita, for the benefit of melting the boron.
Regarding claim 2, the primary sintering is performed at a temperature of 500 °C to 650 °C, Park teaches a typical temperature range for the 1st sintering is 650° C. to 850° C. If the temperature is too low the reaction is not complete. If the temperature is too high the metal of the tube tends to react with the lithiated NMC [0045]. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to adjust the temperature of the first sintering below 650 C should the reaction complete below the temperature 650 C to ensure that the metal of the tube does not react by lowering the temperature and increasing the reaction time.
Regarding claim 5, the protective atmosphere is nitrogen, oxygen, argon or compressed air with CO2 removed, Park discloses that if high Ni excess cathodes are the target, oxygen might be a preferred choice. Generally lithium deficiency allows to reduce the carbonate impurity in the intermediate NMC. Whereas a fully lithiated NMC will take up CO2 from the air to form Li.sub.2CO.sub.3, a lithium deficient NMC has a stronger tendency not to react with the CO2 in the air or even to decompose the Li2CO3 impurity during the 1st sintering. Thus the lithium deficiency is critically linked to the use of air during the 1st sintering [0046]. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to use oxygen should a high Ni excess cathode is desired, or to avoid the formation of lithium carbonate.
Regarding claim 6, Park discloses the secondary-sintered material is a cathode material with a primary particle coated with an ionic conductor, but does not disclose that the ionic conductor is at least one of Li2MoO4, Li2WO4 or Li2SnO3, and a coating amount of the ionic conductor is 0.05wt% to 0.8wt% of the secondary-sintered material in terms of a total amount of Mo, W and Sn in the ionic conductor. Park discloses that the coating is WO3. Kawakita teaches a tungsten coating comprising Li2WO4 [0017]. The tungsten coating lower the resistance of a lithium-containing transition metal oxide [0005]. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to coat Li2WO4 on the particle of Park as a coating, as taught by Kawakita, for the benefit of lowering the resistance of the active material of Park.
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Park (US 2020/0006762) in view of Yang (CN 110190276), Wang (CN 103474655), Ding (CN 108832103), and Kawakita (WO 2020/174937, using US 2022/0033276 as translation) as applied to claim 1, further in view of Awano (US 2012/0015249).
Regarding claim 3, a concentration of Li in the mixed solution ranges from 10 g/L to 37 g/L, Yang teaches the Li2CO3 is 0.01-0.3 parts by weight. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to adjust the concentration or the amount of Li along with the dopant solution for the benefit of adjusting the amount of lithium deposition.
Regarding claim 3, a liquid-solid ratio of the mixed solution to the primary-sintered material is 0.25 mL/g to 1 mL/g, Awano teaches wet mixing the raw material of cathode active material by mixing a lithium source phosphorus source, and Me metal element sources in a slurry along with a carbon precursor in a solid concentration of 10-50 mass% [0058]. It would have been obvious to one of ordinary skilled in the art at the time the invention was made to adjust the solids concentration in the mixture of Park modified by Yang, Wang, and Ding, as taught by Awano, for the benefit of forming a easy slurry to mix.
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to CYNTHIA KYUNG SOO WALLS whose telephone number is (571)272-8699. The examiner can normally be reached on M-F until 5pm.
If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Jonathan Leong can be reached at 571-270-1292. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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/CYNTHIA K WALLS/ Primary Examiner, Art Unit 1751
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