DETAILED ACTION
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 .
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
Information Disclosure Statements
The Information Disclosure Statements filed on 11 September 2024 and 28 April 2025 have been received and considered by the Examiner.
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.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 1-9 and 11-13 are rejected under 35 U.S.C. 103 as being unpatentable over Yang et al. (TW I781427 B) in view of Azuma (JP 2016162601 A). The provided English machine translations of Yang (TW I781427 B) and Azuma (JP 2016162601 A) are used in the analysis below.
Regarding claim 1, Yang teaches a method for preparing a lithium-ion battery cathode material (abstract) comprising:
feeding a first reaction liquid into a Couette-Taylor reactor (continuous Taylor flow reactor), wherein the first reaction liquid is a multi-metal solution containing a nickel compound, a cobalt compound, and a manganese compound ([0080]);
feeding a second solution into the Couette-Taylor reactor to react with a first reaction liquid, so as to from a product stream including a cathode material precursor, wherein the second liquid contains an alkali precipitant comprising sodium hydroxide (At the same time, 4M NaOH precipitant and the required NH3 were also added; [0080]); and,
implementing a calcining operation including using high-temperature tubular furnace to calcine the cathode material precursor separated from the product stream to obtain the lithium-ion battery cathode material (the mixture was subjected to calcination heat treatment in a tubular furnace; [0087]).
Yang does not teach the second reaction solution containing a lithium compound or the cathode material precursor containing lithium elements.
However, Azuma also teaches the preparation of a lithium-ion battery cathode material comprising the combination of a mixed nickel/cobalt/manganese sulfate solution with aqueous ammonia and an alkali precipitant, where in this case the alkali precipitant is lithium hydroxide instead of sodium hydroxide (when carrying out the coprecipitation reaction, metal hydroxides are produced by using LiOH as the alkali instead of NaOH as in the conventional method when using Ni, Mn, and Co sulfates; [0021]). Azuma further teaches that the choice of lithium hydroxide allows for the co-precipitation of a product that does not contain sodium impurities, thereby significantly improving the battery’s cycle characteristics ([0021]). Additionally, Azuma teaches that the precursor materials obtained by using lithium hydroxide as the alkali precipitant contain lithium element ([0026] and Table 1, translated below).
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Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to replace the sodium hydroxide used in the method of Yang with lithium hydroxide and to obtain a cathode material precursor containing lithium elements, as taught by Azuma. One of ordinary skill in the art would have been motivated to do so because Azuma teaches that the use of lithium hydroxide in place of sodium hydroxide in a very similar method is able to reduce sodium impurities and increase the performance of batteries made from the resulting products.
Regarding claim 2, modified Yang teaches the method of claim 1, and Yang further teaches after the Couette-Taylor reaction operation and before the calcining operation, implementing a purification operation that includes filtering and drying the product stream to separate out the cathode material precursor in a powder form (the precipitate is filtered and washed several times …the sediment was placed in an oven and dried; [0080]).
Regarding claims 3 and 5, modified Yang teaches the method of claim 1, where Azuma teaches the lithium compound in the second reaction liquid being lithium hydroxide ([0021]), as analyzed for claim 1.
Regarding claim 4, modified Yang teaches the method of claim 1, where Yang teaches the nickel compound is nickel sulfate, the cobalt compound is cobalt sulfate, and the manganese compound is manganese sulfate ([0077] and [0080]; it is noted the subscripts have been lost in the provided translation, but they are apparent in the original, e.g. [0031]).
Regarding claim 6, modified Yang teaches the method of claim 5, where Azuma shows that when using NaOH in place of lithium hydroxide, no lithium is present in the cathode material precursor (Table 1). Therefore, one can conclude that the lithium compound (lithium hydroxide) is the source of the lithium elements in the cathode material precursor when lithium hydroxide is used.
Regarding claim 7, modified Yang teaches the method of claim 6, where Yang teaches that the second reaction liquid contains NH3 and NaOH, which will serve to regulates the pH value of the reaction mixture that includes the first reaction liquid and the second reaction liquid, wherein the pH value of the reaction mixture is adjusted to 10 to 12 ([0010]). Azuma likewise teaches that the alkali metal hydroxide is used to regulate the pH to between 10 and 12 (lithium hydroxide solution is added to adjust the pH to 10-12; [0021]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention adjust the pH of the reaction mixture to between 10 and 12 by using the second reaction liquid comprising lithium hydroxide to regulate the pH. One of ordinary skill in the art would have been motivated to do so because both Yang and Azuma teach that this pH is appropriate and that the alkali metal hydroxides are used to regulate the pH.
Regarding claim 8, modified Yang teaches the method of claim 7, where Azuma teaches that lithium hydroxide replaces sodium hydroxide in the second reaction liquid, and that such a change is necessary to keep sodium impurities out of the product ([0021]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use in the method of modified Yang a second reaction liquid that does not contain sodium hydroxide. One of ordinary skill in the art would have been motivated to do so because Azuma teaches that the sodium hydroxide should be replaced with lithium hydroxide, and because Azuma teaches that sodium present in the reaction liquid can lead to undesired impurities in the precipitated product.
Regarding claim 9, modified Yang teaches the method of claim 7, wherein the Couette-Taylor reaction operation further includes feeding a chelating agent liquid into the Couette-Taylor reactor to mix with the reaction mixture, wherein the chelating agent liquid is an ammonia solution (A metal ion source, [alkali precipitant] and ammonia water are simultaneously added to the reaction chamber of a continuous Taylor flow reactor…ammonia water …to be used as a chelating agent; [0010] and [0019]).
Regarding claim 11, modified Yang teaches the method of claim 1, where Yang teaches that the cathode material precursor formed by the Couette-Taylor reaction operation is a hydroxide of a metal alloy where the metal alloy includes nickel, cobalt, and manganese elements ([0080]), and where Azuma teaches that the cathode material precursor will also contain lithium when using LiOH as the alkali (Table 1).
Regarding claim 12, modified Yang teaches the method of claim 1, where Yang further teaches the calcining conditions of the calcining operation including filling an oxygen gas into the high temperature tubular furnace and heating the oxygen gas to a first temperature of 150 °C for 2 hours, and then heating the oxygen gas to a second temperature of 500 °C for 6 hours, and then heating the oxygen gas to a third temperature of 830 °C for 12 hours, so as to finally form the lithium ion-battery cathode material ([0090]).
Regarding claim 13, modified Yang teaches the method of claim 1, where after the Couette-Taylor reaction operation and before the calcining operation, the method includes a step of mixing and ball milling the cathode material precursor with a lithium hydroxide solution (LiOH in 99% methanol solvent; [0090]), which is not considered ball milling with solid lithium salt.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to not include a step of mixing and ball milling the cathode material precursor with a solid lithium salt, because Yang teaches using lithium salt solutions as an alternative for introducing lithium into the cathode material.
Claim 10 is rejected under 35 U.S.C. 103 as being unpatentable over Yang et al. (TW I781427 B) in view of Azuma (JP 2016162601 A), as applied to claim 1 above, and further in view of Babulal et al. (Chem. Eng. J. 2021, 413, 127150) and Seenivasan et al. (J. Alloys Compounds 2021, 857, 157594). The provided English machine translations of Yang (TW I781427 B) and Azuma (JP 2016162601 A) are used in the analysis below.
Regarding claim 10, modified Yang teaches the method of claim 1, wherein the Yang teaches the feed rate is 2.23 mL/min ([0010]), though it is unclear if this is the feed rate of the metal ion source, the alkali solution, the ammonia water, or some combination thereof.
However, Babulal also teaches the preparation of nickel manganese cobalt oxide cathode materials by co-precipitation from the metal sulfates in a Couette-Taylor reactor (Taylor flow reactor; abstract and Section 2.1), and Babulal further teaches that the flow rate of the transition metal solution is 1.7 mL/min, but does not specify the flow rate of the alkali solution (sodium hydroxide; Section 2.1).
Furthermore, Seenivasan also teaches using Couette-Taylor reactors for the precipitation of metal hydroxides by co-precipitation using ammonia and an alkali solution (abstract and Section 2.1), and further teaches that the flow rate of the alkali (NaOH) should be controlled and adjusted to maintain the pH of the reaction solution (pH of the reactant solutions in the reaction chamber was controlled precisely to 11.0 by adjusting the flow rate of the NaOH solution throughout the reaction process; Section 2.1).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use in the method of modified Yang a feed for the first reaction liquid with a flow rate of 1.7 mL/min, as taught by Babulal. One of ordinary skill in the art would have been motivated to do so because Babulal teaches that such a rate can be used successfully in a very similar method.
It would have been further obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to optimize by routine experimentation the flow rate of the second reaction liquid, including into the instantly claimed range of between 2.3 mL/min and 3.0 mL/min, and to a point where the flow rate ratio between the first reaction liquid flow rate and the second reaction liquid flow rate is between 1:1.12 and 1:2. One of ordinary skill in the art would have been motivated to do so because Seenivasan teaches that precise control of the flow rate of alkali is required in order to maintain a desired pH value.
Pertinent Prior Art
The following prior art made of record and not relied upon is considered pertinent to applicant's disclosure:
Park et al. (US 2016/0164090 A1) discloses the use of Couette-Taylor reactor for the preparation of lithium-ion battery cathode materials where lithium hydroxide is used as the precipitating alkali solution (abstract and [0036]-[0038]).
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to Nicholas A Piro whose telephone number is (571)272-6344. The examiner can normally be reached Mon-Fri, 8:00 am-5:00 pm.
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/NICHOLAS A. PIRO/Assistant Examiner, Art Unit 1738
/PAUL A WARTALOWICZ/Primary Examiner, Art Unit 1735
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