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 .
Election/Restrictions
Applicant's election with traverse of Group I (claims 29-44) in the reply filed on 01/14/2026 is acknowledged. The traversal is on the ground(s) that there is no serious search burden between Group I and Groups II and III given the substantial overlap in subject matter between the groups. This is not found persuasive because both Group II and Group III contain limitations that are not found in any of the claims in Group I. Namely, dependent claim 46 in Group II requires a molarity range for an aqueous NaOH solution that is not present in Group I, and dependent claim 48 in Group III requires a step of grinding a stoichiometric amount of LiOH*H2O that is not present in Group I. What’s more, the divergent limitations in Groups II and III are directed toward a battery regeneration method; however, Group I mainly focuses on a leaching method for a battery. Thus, the different subject matter in Groups II and III would require further searching of battery regeneration methods not required for Group I, thereby creating a search burden for the examiner.
The requirement is still deemed proper and is therefore made FINAL.
Claims 45-48 are withdrawn from further consideration pursuant to 37 CFR 1.142(b), as being drawn to nonelected Groups II and III, there being no allowable generic or linking claim. Applicant timely traversed the restriction (election) requirement in the reply filed on 01/14/2026.
Claim Rejections - 35 USC § 102
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.
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
Claims 29-34, 36, and 38 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Chen et al. ("Synergistic leaching of valuable metals from spent li-ion batteries using sulfuric acid- l-ascorbic acid system") (Chen) (of record).
Regarding claim 29, Chen discloses a method of selectively leaching one or more manganese-containing phases (lithium manganese oxide) from a mixed-phase battery electrode material (title; abstract; see Table 3), the method comprising: treating the mixed-phase battery electrode material (cathode materials) with a solution of an acid, which is ascorbic acid (title; abstract; see also 3.2.1 Determination of the leaching system on pg. 4). Ascorbic acid is known to have a pKa of greater than or equal to -2. Chen further discloses that the ascorbic acid acts as both a leaching agent and a reducing agent (abstract; see also 3.2.1 Determination of the leaching system on pg. 4; see Fig. 1). Chen further discloses that the phases of the cathode material before leaching include carbon, lithium cobalt oxide, lithium manganese oxide, aluminum doped lithium cobalt oxide, and nickel doped lithium cobalt oxide (see Table 3). Chen further discloses that after leaching, the leaching residue no longer contains phases of lithium manganese oxide but does include at least one other phase of the cathode material (see Table 4), reading on the limitation that the leachate is manganese containing while leaving at least one phase of the battery electrode material un-leached. Thus, Chen reads on all of the limitations in claim 29.
Regarding claim 30, Chen discloses all of the limitations as set forth above for claim 29. Chen further discloses that the mixed-phase battery electrode material (cathode materials) is a cathode material from a lithium-ion battery having a blended cathode (see 2.1 Materials and reagent on pg. 3; 3.1 Characterization analysis of cathode material on pg. 4; see also Table 3).
Regarding claim 31, Chen discloses all of the limitations as set forth above for claim 29. As set forth above, Chen discloses that the acid is ascorbic acid (title; abstract; see also 3.2.1 Determination of the leaching system on pg. 4), which is an organic acid.
Regarding claim 32, Chen discloses all of the limitations as set forth above for claim 29. As set forth above, Chen discloses that the acid is ascorbic acid (title; abstract; see also 3.2.1 Determination of the leaching system on pg. 4), which is known to have a pKa value of about 4.1, reading on the claimed range of from 2 to 12.
Regarding claim 33, Chen discloses all of the limitations as set forth above for claim 29. Chen further discloses that the solution of ascorbic acid has a molarity of 1.25 M (see 3.2.1 Determination of the leaching system on pg. 4), reading on the claimed range of 0.25 M to 1.5 M.
Regarding claim 34, Chen discloses all of the limitations as set forth above for claim 29. Chen further discloses that when ascorbic acid is used alone in a single l-ascorbic acid system, the lithium manganese oxide phase (LMO) is completely leached out while at least some of the other phases of the cathode material remain (see Table 4), making the leaching selective toward LMO. Thus, since LMO is the only phase in the cathode material in which manganese makes up at least 20% of the transition metal content (see Table 3) and is the only phase that is completely leached out (see Table 4), Chen clearly reads on all of the limitations in claim 34.
Regarding claim 36, Chen discloses all of the limitations as set forth above for claim 29. Chen further discloses experimental examples in which the treating of the electrode material involves exposing the electrode material to the acid for a period of less than ten minutes (see Fig. 7b which includes experiments performed at approximately two minutes and 5 minutes; see also 3.2.3 Effect of temperature and time on pg. 5).
Regarding claim 38, Chen discloses all of the limitations as set forth above for claim 29. Chen further discloses that the treating of the electrode material can be performed at a temperature of 333 K (abstract; see Figs. 5 and 6), which is equal to about 60oC, reading on the claimed range of between 20oC and 90oC.
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.
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 29-36 and 38-39 are rejected under 35 U.S.C. 103 as being unpatentable over Ku et al. ("Recycling of spent lithium-ion battery cathode materials by ammoniacal leaching") (Ku) in view of Li et al. ("Ascorbic-acid-assisted recovery of cobalt and lithium from spent Li-ion batteries") (Li).
Regarding claim 29, Ku discloses a method of leaching a mixed-phase battery electrode material (cathode materials) (title; abstract). Specifically, Ku discloses that the electrode material comprises a blended cathode of LMO (LiMn2O4) and a layered oxide (LiCoxMnyNizO2). Ku fails to disclose, however, that the method comprises treating the mixed-phase battery electrode material with an acid solution. However, Ku also discloses that the method only leads to a maximum leaching efficiency of cobalt of 94%, while having a negligible leaching efficiency on manganese and no disclosed leaching of lithium (see Fig. 4a; Col. 1, pg. 143; abstract; conclusions). Furthermore, Ku discloses that the highest leaching of cobalt only occurs after two hours (see Fig. 5a; 3.2 Effect of leaching time and temperature). Thus, one of ordinary skill in the art would have been motivated to look to other methods that lead to higher leaching efficiencies for at least cobalt, lithium, and/or manganese for smaller amounts of time.
Li teaches a similar leaching method for a mixed-phase battery electrode material (cathode materials) (title; abstract), wherein the method involves treating the mixed-phase battery electrode material with a solution of ascorbic acid (title; abstract), the ascorbic acid acting as both a leaching agent and a reducing agent (abstract; see Fig. 6). Furthermore, Li teaches that the pKa of ascorbic acid can be either 4.10 or 11.6 (see Col. 3, pg. 24), which are both greater than -2. Li further teaches that leaching with ascorbic acid leads to a leaching efficiency as much as 94.8% for cobalt and 98.5% for lithium at a leaching time of only 20 minutes (abstract; Col. 2, pg. 25; conclusions). Furthermore, Li teaches that the use of ascorbic acid is more environmentally friendly compared with other methods (see conclusions; introduction).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have modified the method disclosed by Ku to involve treating the mixed-phase battery electrode material with a solution of ascorbic acid, as taught by Li, instead of with an agent based on ammonia because they would have had a reasonable expectation that doing so would lead to a higher leaching efficiency of at least lithium for a smaller amount of time while also being more environmentally friendly.
Regarding the limitation “so as to form a manganese-containing leachate whilst leaving at least one phase of the battery electrode material unleached,” the instant application is clear that leaching of mixed-phase LMO/layered oxide cathodes with a solution of ascorbic acid leads to selective leaching of one or more manganese-containing phases so as to form a manganese-containing leachate while leaving at least one phase of the battery electrode material unleached (see [0168]-[0169] and [0225]-[0226] of the PGPub of the instant application). Therefore, since the method in modified Ku involves treating a mixed-phase LMO/layered oxide cathode material with the solution of ascorbic acid taught by Li which is substantially identical to that of the claims, it is clear that modified Ku would inherently meet the claimed limitations. Thus, modified Ku satisfies all of the limitations in claim 29.
Regarding claim 30, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the mixed-phase electrode material is a cathode material from a lithium-ion battery having a blended cathode (Ku: title; abstract).
Regarding claim 31, modified Ku discloses all of the limitations as set forth above for claim 29. As set forth above, Li teaches that the acid is ascorbic acid (Li: title; abstract), which is an organic acid.
Regarding claim 32, modified Ku discloses all of the limitations as set forth above for claim 29. As set forth above, Li teaches that ascorbic acid can have a pKa of either 4.10 or 11.6 (Li: see Col. 3, pg. 24), suggesting the claimed range of from 2 to 12.
Regarding claim 33, modified Ku discloses all of the limitations as set forth above for claim 29. Li further teaches that the ascorbic acid solution can have a molarity of 1.25 M (Li: abstract), suggesting the claimed range of from 0.25 M to 1.5 M. Therefore, since modified Ku includes the teachings from Li regarding the ascorbic acid solution, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention for modified Ku to have satisfied all of the limitations in claim 33.
Regarding claim 34, modified Ku discloses all of the limitations as set forth above for claim 29. The instant specification is clear that treating mixed-phase LMO/layered oxide cathodes with a solution of ascorbic acid leads to leaching of substantially only phases in which manganese makes up at least 20% of the transition metal content (see [0181] of the PGPub of the instant application). Therefore, since the method in modified Ku involves treating a mixed-phase LMO/layered oxide cathode material with the solution of ascorbic acid taught by Li which is substantially identical to that of the claims, it is clear that modified Ku would inherently meet the claimed limitations. Thus, modified Ku satisfies all of the limitations in claim 34.
Regarding claim 35, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the electrode material is a blended cathode of LMO and a layered oxide (Ku: abstract). Furthermore, modified Ku discloses that the electrode material originates as a cathode strip (Ku: see Fig. 1; 2.1 Materials and methods on pg. 139-140). Furthermore, the instant specification is clear that leaching of mixed-phase LMO/layered oxide cathodes with a solution of ascorbic acid leads to selective leaching of the LMO while leaving the layered oxide at least substantially intact (see [0168]-[0169] and [0225]-[0229] of the PGPub of the instant application). Therefore, since the method in modified Ku involves treating a mixed-phase LMO/layered oxide cathode material with the solution of ascorbic acid taught by Li which is substantially identical to that of the claims, it is clear that modified Ku would inherently meet the claimed limitations. Thus, modified Ku satisfies all of the limitations in claim 35.
Regarding claim 36, modified Ku discloses all of the limitations as set forth above for claim 29. Li further teaches that the ascorbic acid treating method can be conducted for a period as low as 5 minutes (Li: see 2.2 Experimental procedure on pg. 22; 3.2.1 Effect of temperature and time on leaching; see Figs. 8(a) and 8(b)), suggesting the claimed range of less than ten minutes. Therefore, since modified Ku includes the teachings from Li regarding the ascorbic acid leaching method, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention for modified Ku to have satisfied all of the limitations in claim 36.
Regarding claim 38, modified Ku discloses all of the limitations as set forth above for claim 29. Li further teaches that the treating of the electrode material can be performed at a temperature of 70oC (Li: abstract), suggesting the claimed range of between 20oC and 90oC. Therefore, since modified Ku includes the teachings from Li regarding the ascorbic acid leaching method, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention for modified Ku to have satisfied all of the limitations in claim 38.
Regarding claim 39, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the electrode material originates as an un-shredded cathode strip (Ku: see Fig. 1; 2.1 Materials and methods on pg. 139-140), suggesting all of the limitations in claim 39.
Claim 37 is rejected under 35 U.S.C. 103 as being unpatentable over Ku et al. ("Recycling of spent lithium-ion battery cathode materials by ammoniacal leaching") (Ku) in view of Li et al. ("Ascorbic-acid-assisted recovery of cobalt and lithium from spent Li-ion batteries") (Li) as applied to claim 29 above, and further in view of Park (KR 102132120 with English Machine Translation).
Regarding claim 37, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the electrode material comes from end-of-life batteries (spent LIBs) (Ku: abstract; see introduction). However, modified Ku fails to explicitly disclose that the electrode material also comes from quality-control rejected new batteries.
However, it is known in the art to use battery recycling methods on both end-of-life batteries and quality-control rejected new batteries. For instance, Park discloses a similar battery recycling method (title) in which the cathode materials to be recycled come from both spent batteries and scraps produced during the manufacturing process of lithium-ion batteries (abstract; [0004]; [0007]-[0008]).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have included not only spent batteries but also quality-control rejected new batteries in the recycling method disclosed by modified Ku, as suggested by Park, because they would have had a reasonable expectation that doing so would lead to a higher volume of recycled battery materials and, thus, less waste.
Furthermore, Li teaches that the battery recycling method involves treating the electrode material with the ascorbic acid solution for anywhere between 5 and 50 minutes (Li: see 3.2.1 Effect of temperature and time on leaching on pg. 25; see also Figs. 8(a) and 8(b)). Thus, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have at least tried treating the electrode material from the end-of-life batteries for a longer time period than the electrode material from the quality-control rejected new batteries given the wide range of possible treating times disclosed by Li. Thus, modified Ku satisfies all of the limitations in claim 37.
Claim 40 is rejected under 35 U.S.C. 103 as being unpatentable over Ku et al. ("Recycling of spent lithium-ion battery cathode materials by ammoniacal leaching") (Ku) in view of Li et al. ("Ascorbic-acid-assisted recovery of cobalt and lithium from spent Li-ion batteries") (Li) as applied to claim 35 above, and further in view of Or et al. ("Recycling of mixed cathode lithium-ion batteries for electric vehicles: Current status and future outlook") (Or) (of record) as evidenced by Yang et al. ("Short process for regenerating Mn-rich cathode material with high voltage from mixed-type spent cathode materials via a facile approach") (Yang).
Regarding claim 40, modified Ku discloses all of the limitations as set forth above for claim 35. Modified Ku fails to disclose, however, that the method comprises regenerating an LMO phase from the leachate.
However, it is known in the art to regenerate different phases from the leachate of recycled batteries. For instance, Or teaches several known methods for regenerating cathode material phases from the leachate of recycled batteries (see Table 5 on pg. 31-34). Specifically, Or teaches a method for regenerating an LMO phase (Li2MnO3) from a leachate, wherein the regenerating involves drying the leachate so as to form a precipitate; grinding the precipitate; and annealing (sinter) the ground precipitate (see row 1 of Table 5 on pg. 32). Furthermore, the Yang reference that Or is referring to in Table 5 specifically teaches that this annealing process is performed in an air atmosphere (Yang: see 2.2 Regeneration on pg. 125). Or further teaches that this regeneration process leads to good electrochemical performance and capacity retention (see row 1 of Table 5 on pg. 32; see also conclusions on pg. 130 of Yang).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have modified the method disclosed by modified Ku to include the claimed regenerating method, as taught by Or and Yang, because they would have had a reasonable expectation that doing so would lead to good electrochemical performance and capacity retention in the regenerated electrode material.
Claims 41-44 are rejected under 35 U.S.C. 103 as being unpatentable over Ku et al. ("Recycling of spent lithium-ion battery cathode materials by ammoniacal leaching") (Ku) in view of Li et al. ("Ascorbic-acid-assisted recovery of cobalt and lithium from spent Li-ion batteries") (Li) as applied to claim 29 above, and further in view of Zou et al. ("A novel method to recycle mixed cathode materials for lithium ion batteries") (Zou).
Regarding claim 41, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the electrode material comprises LMO which is leached by the acid solution (Ku: abstract; Li: abstract). Modified Ku fails to disclose, however, the claimed generating method.
However, methods for regenerating cathode materials from the leachate of recycled batteries are known in the art. For instance, Zou teaches a method for recycling mixed cathode materials for lithium-ion batteries (title), wherein the method comprises generating a target LiNi0.33Mn0.33Co0.33O2 phase from a leachate (see pg. 1186-1187), the generating comprising: gravimetrically determining the amount of leached LMO (1185-1187), and, based on the gravimetrically determined amount of leached LMO: calculating a molar amount of cobalt- and nickel-containing sulfate, M(SO4)*nH2O (where M = Co and Ni), required to obtain the target composition from the leachate (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186; see also Table 6); and calculating a molar amount of Li2CO3 to obtain the target composition from the leachate (see Step 5 on pg. 1185), combining the calculated amount of M(SO4)*nH2O with the leachate (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186), adding a molar amount of a soluble source of a cation (NaOH) selected to trigger precipitation of a sulfate, so as to remove the sulfate from the leachate solution, the molar amount to add being calculated from the molar amount of M(SO4)*nH2O and the Co:Ni ratio of M to the leachate solution (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186; see also Waste products on pg. 1189); drying the leachate solution so as to form a precipitate; grinding the precipitate with the calculated amount of Li2CO3; and annealing the ground material in air (see Step 5 on pg. 1185). Zou further teaches that this generation method leads to excellent electrochemical performance for the generated cathode material as well as saved cost (see conclusions on pg. 1189-1190).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have modified the recycling method disclosed by modified Ku to include the generating method taught by Zou because they would have had a reasonable expectation that doing so would lead to excellent electrochemical performance for the generated cathode material as well as saved cost.
Regarding claim 42, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku further discloses that the electrode material comprises LMO which is leached by the acid solution (Ku: abstract; Li: abstract). Modified Ku fails to disclose, however, the claimed generating method.
However, methods for regenerating cathode materials from the leachate of recycled batteries are known in the art. For instance, Zou teaches a method for recycling mixed cathode materials for lithium-ion batteries (title), wherein the method comprises generating a target LiNi0.33Mn0.33Co0.33O2 phase from a leachate (see pg. 1186-1187), the generating comprising: gravimetrically determining the amount of leached LMO (1185-1187), and, based on the gravimetrically determined amount of leached LMO: calculating a molar amount of soluble source of cobalt and nickel required to obtain the target composition from the leachate (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186; see also Table 6); and calculating a molar amount of Li2CO3 to obtain the target composition from the leachate (see Step 5 on pg. 1185), combining the calculated amount soluble source of cobalt and nickel with the leachate (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186), adding an OH- source (NaOH) until a precipitate is formed (see Step 3 on pg. 1185; Precipitating Co, Ni and Mn hydroxide on pg. 1186); drying the leachate solution so as to form a precipitate; grinding the precipitate with the calculated amount of Li2CO3; and annealing the ground material in air (see Step 5 on pg. 1185). Zou further teaches that this generation method leads to excellent electrochemical performance for the generated cathode material as well as saved cost (see conclusions on pg. 1189-1190).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have modified the recycling method disclosed by modified Ku to include the generating method taught by Zou because they would have had a reasonable expectation that doing so would lead to excellent electrochemical performance for the generated cathode material as well as saved cost.
Regarding claim 43, modified Ku discloses all of the limitations as set forth above for claim 42. Zou further teaches that the amount of the hydroxide added to form the precipitate is the amount of the hydroxide required to bring the solution pH to 11 (see Step 3 on pg. 1185).
Regarding claim 44, modified Ku discloses all of the limitations as set forth above for claim 29. Modified Ku fails to explicitly disclose, however, the regenerating steps in claim 44.
However, methods for regenerating cathode materials from the leachate of recycled batteries are known in the art. For instance, Zou teaches a method for recycling mixed cathode materials for lithium-ion batteries (title), wherein the method comprises gravimetrically determining an amount of material lost from the mixed-phase battery electrode material into the leachate (1185-1187); and adding a stoichiometric amount of one or more reagents to the leachate to introduce desired metal cations so as to generate a desired battery cathode material (see Steps 1-5 on pg. 1184-1185). Zou further teaches that this generation method leads to excellent electrochemical performance for the generated cathode material as well as saved cost (see conclusions on pg. 1189-1190).
Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have modified the recycling method disclosed by modified Ku to include the generating method taught by Zou because they would have had a reasonable expectation that doing so would lead to excellent electrochemical performance for the generated cathode material as well as saved cost.
Conclusion
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/B.C.D./Examiner, Art Unit 1749
/KATELYN W SMITH/Supervisory Patent Examiner, Art Unit 1749