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 .
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 8-9 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention.
Claim 8 recites the limitation "grinding is performed before heating the components". There is insufficient antecedent basis for this limitation in the claim. Nowhere in claims 1, 7 or 8 is a step of “heating” previously recited, therefore it is indefinite as to if the recitation of “before heating the components” is intended to preclude any and all heating from occurring prior to the grinding, or if the intention is to base the occurrence of the grinding step relative to a particular instance of heating, such as the heating step presently recited in dependent claim 2; or some other intention entirely. For purposes of examination this limitation will be interpreted as at least inclusive of any such scenario.
Claim 9 recites the limitation "grinding is performed after heating the components and before exposing". There is insufficient antecedent basis for this limitation in the claim. Nowhere in claims 1, 7 or 9 is a step of “heating” previously recited, therefore it is indefinite as to if the recitation of “after heating the components” is intended to actually require any type heating step from occurring prior to grinding, or if the intention is to base the occurrence of the grinding step relative to a particular instance of heating, such as the heating step presently recited in dependent claim 2; or some other intention entirely. For purposes of examination this limitation will be interpreted as at least inclusive of any such scenario.
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.
Claim(s) 1, 10, 13, and 20 is/are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Myoung et al (“Cobalt oxide preparation from waste LiCoO2 by electrochemical-hydrothermal method” Journal of Power Sources 112 (2002) 639-642;hereafter Myoung).
Claim 1: Myoung teaches a method for recycling an electrical energy storage device (See, for example, abstract, introduction, experimental sections), the method comprising:
exposing components of the electrical energy storage device to an acidic solution (such as HNO3 solution) to form a recovery solution (See, for example, abstract, introduction, experimental sections);
performing plating (electrodeposition)in the presence of the recovery solution and a conductive substrate (such as titanium cathode), metals of the recovery solution depositing on the conductive substrate (See, for example, abstract, experimental sections, and pg 640).
and oxidizing the metals deposited on the conductive substrate to form an electrode material (such as Co3O4) (See, for example, abstract, pg 641-642, wherein heat treatment oxidizes the cobalt of cobalt hydroxide formed from EC deposition to cobalt oxide).
Claim 10: Myoung further teaches wherein the acidic solution includes nitric acid (See, for example, experimental section).
Claim 13: Myoung further teaches wherein the conductive substrate includes titanium (see, for example, experimental section).
Claim 20: Myoung further teaches wherein oxidizing includes heating in an oxygen containing atmosphere (air) at a temperature of 400° C (See, for example, pg 641-642).
Claim(s) 1-2, 10, 12-13, and 16 is/are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Kim et al (“Selective cobalt and nickel electrodeposition for lithium-ion battery recycling through integrated electrolyte and interface control ” Nature Communications (2021) 12:6554 pg 1-10 and supplemental information (22 additional pgs); hereafter Kim).
Claim 1: Kim teaches a method for recycling an electrical energy storage device (Li-ion battery) (See, for example, abstract, introduction, experimental sections), the method comprising:
exposing components of the electrical energy storage device to an acidic solution (such as HCL) solution) to form a recovery solution (See, for example, abstract, pg 2, pg 7, pg 9, supplemental figure 21 and associated description following);
performing plating (electrodeposition)in the presence of the recovery solution and a conductive substrate (such as copper foil), metals (Co / Ni) of the recovery solution depositing on the conductive substrate (See, for example, abstract, pg 2-3, methods section of pg 8,).
and oxidizing the metals deposited on the conductive substrate to form an electrode material (such as oxidized Ni and Co compounds) (See, for example, end of pg 5 wherein XPS confirms the method results in presence of oxides of the metals due to surface oxidation of the deposited metals).
Claim 2: Kim further teaches heating the components of the electrical energy storage device prior to exposing (see, for example, pg 9 step (c) “NMP treatment” occurring prior to (d) Leaching).
Claim 10: Kim further teaches wherein the acidic solution includes HCL acid (See, for example, abstract, pg 2, pg 7, pg 9, supplemental figure 21 and associated description following);
Claim 12: Kim further teaches wherein the acidic solution is 10M HCL, which via calculation from pH=-log [H+] yields a pH of -1 (see, for example, pg 7, pg 9).
Claim 13: Kim further teaches wherein the conductive substrate includes copper (see, for example, abstract, pg 2-3, and pg 8 methods section).
Claim 16: Kim further teaches wherein the conductive substrate is a foil (such as copper foil) (see, for example, abstract, pg 2-3, and pg 8 methods section).
Claim Rejections - 35 USC § 103
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 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) 2-6 and 12 is/are rejected under 35 U.S.C. 103 as being unpatentable over Myoung as applied to claim 1 above and further in view of Yang et al (“Thermal treatment process for the recovery of valuable metals from spent lithium-ion batteries” Hydrometallurgy 165 (2016) 390-396; hereafter Yang).
Claim 2: Myoung teaches the method of claim 1 above directed to the recycling of electrical energy storage devices, further li-ion batteries, and uses spent LiCoO2 within its leaching and deposition process (see, for example, pg 639), but it is silent as to the steps of procuring such spent material from the used batteries, so it does not explicitly the various device pretreatment steps recited in claims 2-9. Yang teaches a method of recycling and recovery of lithium ion batteries and components thereof (See, for example, abstract, pg 1-2). Yang further teaches wherein performing a thermal pretreatment step prior to leaching improves the overall recovery efficiency of the valuable metals, and facilitates separation of the current collector and removal of the binder and carbonaceous materials (See, for example, abstract, section 4). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated heating the components of the electrical energy storage device prior to exposing since such a thermal pretreatment would predictably improve the overall recovery efficiency of the valuable metals, and facilitate separation of the current collector and removal of the binder and carbonaceous materials.
Claims 3-4: Yang further teaches wherein the heating includes heating in an inert atmosphere, further nitrogen (see, for example, abstract, section 2, section 4).
Claim 5: Yang further teaches wherein the heating includes heating at a temperature of 600° C. (See, for example, section 4.).
Claim 6: Yang further teaches heating is performed in a muffle furnace (tube furnace, with air purge and means to back fill inert atmosphere such as nitrogen) (See, for example, section 2.1, section 4).
Claim 12: Yang further teaches the predictability of leaching the thermally treated components in 4M H2SO4, (calculated pH of ~-0.6) (See, for example, section 3.2).
Claim(s) 2, 5-7, and 9 is/are rejected under 35 U.S.C. 103 as being unpatentable over Myoung as applied to claim 1 above and further in view of Chen et al (“Hydrometallurgy process for the recovery of metal values from spent lithium-ion batteries in citric acid media” WM&R 2014, Col 32(11) 1083-1093; hereafter Chen).
Claim 2: Myoung teaches the method of claim 1 above directed to the recycling of electrical energy storage devices, further li-ion batteries, and uses spent LiCoO2 within its leaching and deposition process (see, for example, pg 639), but it is silent as to the steps of procuring such spent material from the used batteries, so it does not explicitly the various device pretreatment steps recited in claims 2-9. Chen teaches a method of recycling and recovery of lithium ion batteries and components thereof (See, for example, abstract, pg 1083-1084). Chen further teaches wherein performing a thermal pretreatment step prior to leaching provides removal of the binder, impurities, and carbonaceous materials (See, for example, pg 1084). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated heating the components of the electrical energy storage device prior to exposing since such a thermal pretreatment would predictably facilitate removal of the binder, impurities, and carbonaceous materials.
Claim 5: Chen further teaches wherein the heating includes heating at a temperature of 800° C. (See, for example, pg 1084).
Claim 6: Chen further teaches heating is performed in a muffle furnace (See, for example, pg 1084).
Claim 7: refer to the rejection of claim 2 above, Chen further teaches grinding the components of the electrical energy storage device as it would facilitate reduction of the active material particle size thus promoting leaching efficiency (See, for example, pg 1084). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a grinding pretreatment step as it would predictably enhance leaching efficiency.
Claim 9: Chen further teaches wherein the grinding is performed after the heating step (of claim 2) and before exposing (See, for example, pg 1084).
Claim(s) 2, 5, and 7-9 is/are rejected under 35 U.S.C. 103 as being unpatentable over Myoung as applied to claim 1 above and further in view of Dunn et al (“Material and Energy Flows in the Materials Production, Assembly, and End-of-Life Stages of the Automotive Lithium-Ion Battery Life Cycle” ANL/ESD/12-3 Rev. report Argonne National Laboratory Sept 2014, 62 pg; hereafter Dunn).
Claim 2: Myoung teaches the method of claim 1 above directed to the recycling of electrical energy storage devices, further li-ion batteries, and uses spent LiCoO2 within its leaching and deposition process (see, for example, pg 639), but it is silent as to the steps of procuring such spent material from the used batteries, so it does not explicitly the various device pretreatment steps recited in claims 2-9. Dunn teaches a method of recycling and recovery of lithium ion batteries and components thereof (See, for example, abstract, pg 1-3, pg 35-44). Dunn further teaches wherein performing a thermal pretreatment step (calcination) prior to leaching provides removal of the binder and carbonaceous materials (See, for example, pg 36, Fig 10 and pg 39). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated heating the components of the electrical energy storage device prior to exposing since such a thermal pretreatment would predictably facilitate removal of the binder, and carbonaceous materials.
Claim 5: Dunn further teaches wherein the heating includes heating at a temperature of 700° C / 1300oF. (See, for example, pg 36, Fig 10 and pg 39).).
Claim 7-9: refer to the rejection of claim 2 above, Dunn further teaches multiple grinding steps of the components of the electrical energy storage device, both before and after the calcination step to reduce particle sizes (See, for example, pg 36, Fig 10, pg 38-39, Table 29, first grinding step / crushing step in planetary ball mill, and “second grinding step” following calcination). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a grinding pretreatment step before and after heating as such grinding steps are conventional well known in the art of recycling such battery components as they assist in size reduction of spent battery material, which one of ordinary skill in the art would further readily understand would enhance surface area exposure for processes of calcination and leaching.
Claim(s) 11 is/are rejected under 35 U.S.C. 103 as being unpatentable over Myoung as applied to claim 10 above and further in view of Uchida et al (US 2008/0050295; hereafter Uchida).
Claim 11: Myoung teaches the method of claim 10 (above), and further teaches leaching in an acidic solution of nitric acid (See, for example, experimental section). Myoung does not explicitly teach the acidic solution includes aqua regia. Uchida teaches a method of recycling and recovery of lithium ion batteries and components thereof (See, for example, abstract). Uchida further teaches wherein acidic solution leaching acids for transition metals, such as Ni, Co, commonly include acids of nitric acid hydrochloric acid, and aqua regia (See, for example, [0027]). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated aqua regia as a leaching acid as it is predictably known and used in the art to leach transition metals, and since where two known alternatives are interchangeable for a desired function, an express suggestion to substitute one for the other is not needed to render a substitution obvious. In re Fout, 675 F.2d 297,301 (CCPA 1982); In re Siebentritt, 372 F.2d 566, 568 (CCPA 1967) and / or since “It is prima facie obvious to combine two compositions each of which is taught by the prior art to be useful for the same purpose, in order to form a third composition to be used for the very same purpose.... [T]he idea of combining them flows logically from their having been individually taught in the prior art.” In re Kerkhoven, 626 F.2d 846, 850, 205 USPQ 1069, 1072 (CCPA 1980).
Claim(s) 15-16 is/are rejected under 35 U.S.C. 103 as being unpatentable over Myoung as applied to claim 13 above and further in view of Lupi et al (“Nickel and cobalt recycling from lithium-ion batteries by electrochemical processes” Waste Management 25 (2005) 215-220; hereafter Lupi).
Claim 15: Myoung teaches the method of claim 13 (above), and but does not explicitly teach wherein the conductive substrate for Co electrodeposition includes aluminum. Lupi teaches a method of recycling components of spent lithium ion batteries, particularly cobalt and nickel (See, for example, title, abstract). Lupi further teaches wherein aluminum acts predictably as the cathode for electrodeposition of Co from spent lithium batteries, and further provides improvements to deposit quality (See, for example, section 3). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated aluminum as the conductive substrate for the electrodeposition process as it performs predictably as the cathode for the electrodeposition and recovery of cobalt from spend lithium battery components, further providing improved deposit quality, and / or since where two known alternatives are interchangeable for a desired function, an express suggestion to substitute one for the other is not needed to render a substitution obvious. In re Fout, 675 F.2d 297,301 (CCPA 1982); In re Siebentritt, 372 F.2d 566, 568 (CCPA 1967).
Claim 16: refer to the rejection of claim 15 above, and Lupi additionally teaches wherein the conductive substrate is foil (See, for example, pg 216-218).
Claim(s) 1, 7-10, 12-14, and 17-19 is/are rejected under 35 U.S.C. 103 as being unpatentable over Kim et al (US2013/0312254; hereafter Kim254) in view of Tan et al (“Electrogenerative Removal of Cobalt from Sulfate Solutions Using a Batch Reactor” Clean-Soil, Air, Water 2011 39(5), 460-466; hereafter Tan.
Claim 1: Kim254 teaches a method for recycling an electrical energy storage device (Li-ion battery) (See, for example, abstract, Fig 1-2,) the method comprising:
exposing components of the electrical energy storage device to an acidic solution (acid leaching) solution) to form a recovery solution (See, for example, abstract, [0008-0009]);
and oxidizing metals, particularly Co, Mn, and Ni, from a processed recovery solution to form an electrode material (See, for example, Fig 1, [0019], [0060] mixing and sintering recovered precursor, such as metal / hydroxide/ acid solutions, into metal -oxide electrode active material).
Kim254 does not explicitly teach an intermediate step of performing plating in the presence of the recovery solution and a conductive substrate with metals of the recovery solution depositing on the conductive substrate. Tan teaches a method of Co recovery from waste streams (See, for example, abstract and introduction). Tan teaches an electrogenerative recovery process of Co which overcomes a number of drawbacks of conventional recovery processes in hydrometallurgical methods, while producing electrical energy (See, for example, pg 460). Tan teaches wherein the electrogenerative method involves performing plating of cobalt onto a conductive substrate (cathode) in the presence of an acid recovery solution, such as sulfate solution (See, for example, section 2.1 Fig 1). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated performing an electrogenerative method comprising plating in the presence of the recovery solution and a conductive substrate as such a method would predictably provide a means to recover metals, such as co, of the recovery solution via spontaneous deposition thereof onto the cathode of the galvanic cell, all while avoiding drawbacks of conventional separation / recovery methods and generating electrical energy.
Claim 7: Kim254 further teaches grinding the components of the electrical energy storage device (See, for example, [0014], pulverizing)
Claim 8: Kim254 further teaches grinding is performed before heating the components (see, for example [0101-0108], wherein following grinding, the articles are placed in a leaching solution heated to 60oC)
Claim 9: Kim254 further teaches grinding is performed after heating the components (dehydrating and drying at 60-90oC) (See, for example, [0070-0073]).
Claim 10: Kim254 further teaches wherein the acidic solution includes sulfuric acid (See, for example, [0019] of Kim254 );
Claim 12: Although Kim254 is silent as to an exemplary pH for its leaching acid, the examiner notes that one of ordinary skill in the art would readily appreciate that the pH of an acid would influence the rate of dissolution of not only the intended leaching target but of all the contacted materials, thus it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a pH within the claimed range of less than 1.5 since the pH is a result effective variable and discovery of an optimum value of a result effective variable in a known process is ordinarily within the skill of the art. In re Boesch, 617 F.2d 272, 276 (CCPA 1980) , and since generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical.(MPEP 2144.05 II A).
Claims 13-14: Tan further teaches wherein the conductive substrate includes graphite (See, for example, abstract, section 2.1
Claims 17-19: Tan further teaches wherein the plating is an electroless plating process further in a galvanic cell free from an external electric potential (simultaneous, electrogenerative), see, for example, pg 460-461).
Conclusion
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/NATHAN H EMPIE/ Primary Examiner, Art Unit 1712