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 .
Claims 1-4, 7-12 and 14-20 are pending in application.
Election/Restrictions
Applicant’s election without traverse of claims 1-4 and 14-16 in the reply filed on 07/10/2026 is acknowledged.
Claims 7-12 and 17-20 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected invention, there being no allowable generic or linking claim. Election was made without traverse in the reply filed on 07/10/2026.
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.
7. 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.
8. 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.
9. Claims 1-4 and 14-16 are rejected under 35 U.S.C. 103 as being unpatentable over Osawa (WO 2020149079 A1) in view of Li (CN 112701267 A).
Regarding claim 1, Osawa discloses a negative electrode material comprising an active material (title) with a negative electrode active material layer (6th paragraph of page 6, ref. 12, Fig. 1) comprising a silicon oxygen compound with the formula SiOx (2nd to last paragraph of page 4). The negative electrode active material layer further comprises at least two lithium silicate compounds (2nd to last paragraph of page 4), Li2SiO-3 which is a more water-soluble lithium silicate and Li2Si2-O5 which is a water in-soluble lithium silicate (2nd full paragraph of page 8). Both lithium silicate species, Li2SiO-3 and Li2Si2-O5, form a skeleton structure on the surface of the silicon-oxygen compound particles, as each lithium silicate species is generated inside or on the surface of the silicon-oxygen particles as the result of inserting Li into the particles of the silicon-oxygen compound (5th full paragraph of page 8), resulting in the silicon-oxygen material being embedded on the lithium silicate skeleton structure. Osawa further discloses a strongest XRD peak intensity P1 obtained from an XRD pattern associated with Li2Si2-O5 and a strongest XRD peak intensity P3 associated with Li2SiO-3 obtained from an XRD pattern wherein the ratio of P1 to P3 may satisfy the relationship 0.01≤P1/P3≤1 (2nd full paragraph of page 8), overlapping the claimed range. MPEP § 2144.05 I.
However, Osawa fails to teach two lithium silicate skeleton structures with one inside the active material and one on the surface layer of the active material where the two skeleton structures are linked.
Li discloses a silicon-oxygen composite negative electrode material (title) comprising a pre-lithiated silicon-oxygen core having the formula SiOx-Li (5th paragraph of page 2). Furthermore, water soluble Li-2SiO3 can be formed inside the silicon-oxygen material, resulting in a skeleton structure inside the active material, and water insoluble Li2Si2O5 can be formed on the surface of the active material (3rd to last paragraph of page 2), resulting in a skeleton of water-insoluble silicate on the surface of the active material. The resulting core-shell structure is represented in a cross-sectional view of the pre-lithiated silicon-oxygen composite material (Fig. 1) in which the skeleton of water insoluble lithium silicate Li2Si2O5 is linked with the skeleton of water-soluble lithium silicate Li-2SiO3.
Furthermore, Li teaches that the cooperation of the core and the intermediate layer containing the water insoluble Li2Si2O5 results in a pre-lithiated silicon-oxygen composite material which is non-reactive with water and does not increase the pH during homogenization, inhibiting gas generation of the slurry without sacrificing first coulombic efficiency (6th paragraph of page 5). According to the 2nd paragraph on page 2 of the specification of the instant application, both excessively alkaline pH and gas generation are known problems for silicon-based active materials in the art.
Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have used the core-shell structure with a water insoluble lithium silicate shell and a core comprising a water-soluble lithium silicate as taught by Li to produce a negative electrode material which is insoluble in water to control pH and suppress gas generation while maintaining high first coulombic efficiency.
Regarding claim 2, Osawa discloses a negative electrode material comprising an active material (title) with a negative electrode active material layer (6th paragraph of page 6, ref. 12, Fig. 1) comprising a silicon oxygen compound with the formula SiOx (2nd to last paragraph of page 4). The negative electrode active material layer further comprises at least two lithium silicate compounds (2nd to last paragraph of page 4), Li2SiO-3 which is a more water-soluble lithium silicate and Li2Si2-O5 which is a water in-soluble lithium silicate (2nd full paragraph of page 8). Furthermore, the silicon oxygen compound particles, referred to by Osawa as the silicon compound particles, are contained in the lithium silicates Li2SiO-3 or Li2Si2-O5 as the lithium silicates are generated from the SiOx precursors on the surface and core (5th full paragraph of page 8). Osawa further discloses a strongest XRD peak intensity P1 obtained from an XRD pattern associated with Li2Si2-O5 and a strongest XRD peak intensity P3 associated with Li2SiO-3 obtained from an XRD pattern wherein the ratio of P1 to P3 may satisfy the relationship 0.01≤P1/P3≤1 (2nd full paragraph of page 8), overlapping the claimed range. MPEP § 2144.05 I.
However, Osawa fails to teach a water-insoluble silicate coated on a surface of the lithium silicate.
Li discloses a silicon-oxygen composite negative electrode material (title) comprising a pre-lithiated silicon-oxygen core having the formula SiOx-Li (5th paragraph of page 2). Furthermore, water soluble Li-2SiO3 can be formed inside the silicon-oxygen material and water insoluble Li2Si2O5 can be formed on the surface of the active material (3rd to last paragraph of page 2). The resulting core-shell structure is represented in a cross-sectional view of the pre-lithiated silicon-oxygen composite material (Fig. 1) in which the water insoluble lithium silicate Li2Si2O5 forms a coating on the surface of the water-soluble lithium silicate Li-2SiO3.
Furthermore, Li teaches that the cooperation of the core and the intermediate layer containing the water insoluble Li2Si2O5 results in a pre-lithiated silicon-oxygen composite material which is non-reactive with water and does not increase the pH during homogenization, inhibiting gas generation of the slurry without sacrificing first coulombic efficiency (6th paragraph of page 5). According to the 2nd paragraph on page 2 of the specification of the instant application, both excessively alkaline pH and gas generation are known problems for silicon-based active materials in the art.
Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have used the core-shell structure with a water insoluble lithium silicate shell and a core comprising a water-soluble lithium silicate as taught by Li to produce a negative electrode material which is insoluble in water to control pH and suppress gas generation while maintaining high first coulombic efficiency.
Regarding claim 3, Osawa further teaches that that the silicon oxygen material satisfies the formula SiOx where 0.5≤x≤1.6 (2nd to last paragraph of page 4) which overlaps the claimed range of 0.5≤x≤1.5. MPEP § 2144.05 I.
Regarding claim 4, Osawa also teaches that the silicon oxygen compound particles, which are referred to as the silicon compound particles by Osawa, are coated with a carbon film in the preferred embodiment of the disclosed invention (1st paragraph of page 6). Hence, Osawa discloses the carbon layer on the surface of the active material (Fig. 1). Furthermore, the average thickness of the carbon material is 100 nm (2nd to last paragraph of page 15) anticipating the claimed range of 30nm - 500 nm. MPEP § 2131.03 I.
Regarding claim 14, Osawa teaches that that the silicon oxygen material satisfies the formula SiOx where 0.5≤x≤1.6 (2nd to last paragraph of page 4) which overlaps the claimed range of 0.5≤x≤1.5. MPEP § 2144.05 I.
Regarding claim 15, Osawa also teaches that the silicon oxygen compound particles, which are referred to as the silicon compound particles by Osawa, are coated with a carbon film in the preferred embodiment of the disclosed invention (1st paragraph of page 6). Hence, Osawa discloses the carbon layer on the surface of the active material. Furthermore, the average thickness of the carbon material is 100 nm (2nd to last paragraph of page 15) anticipating the claimed range of 30nm - 500 nm. MPEP § 2131.03 I.
Regarding claim 16, Osawa further teaches that the silicon oxygen compound particles, which are referred to as the silicon compound particles by Osawa, are coated with a carbon film in the preferred embodiment of the disclosed invention (1st paragraph of page 6). Hence, Osawa discloses the carbon layer on the surface of the active material. Furthermore, the average thickness of the carbon material is 100 nm (2nd to last paragraph of page 15) anticipating the claimed range of 30nm - 500 nm. MPEP § 2131.03 I.
10. Claims 1-4 and 14-16 are rejected under 35 U.S.C. 103 as being unpatentable over Li (CN 112701267 A) in view of Hirose (US PG Pub 2019/0123344 A1) as evidenced by Padden et al. Anal. Chem. 1999, 71, 3325-3331 and Ahmad, B. ‘Understanding XRD peaks for crystal structure analysis’.
Regarding claim 1, Li discloses a silicon-oxygen composite active negative electrode material (title) comprising a pre-lithiated silicon-oxygen core having the formula SiOx-Li (5th paragraph of page 2). Furthermore, water soluble Li-2SiO3 can be formed inside the silicon-oxygen material, resulting in a lithium silicate skeleton structure inside the active material, and water insoluble Li2Si2O5 can be formed on the surface (3rd to last paragraph of page 2), resulting in a skeleton of water-insoluble silicate on the surface of the active material. The resulting core-shell structure is represented in a cross-sectional view of the pre-lithiated silicon-oxygen composite material (Fig. 1) in which the skeleton of water insoluble lithium silicate Li2Si2O5 is linked with the skeleton of water-soluble lithium silicate Li-2SiO3 and the silicon-oxygen material is embedded in the core of the lithium silicate skeleton (5th paragraph of page 2).
However, Li fails to teach that the intensity of a strongest diffraction characteristic peak from an XRD pattern of the water-soluble lithium silicate, IB, to the lithium silicate, IA, is within the claimed range of 0.03≤IB/IA≤0.2.
Hirose teaches a negative electrode active material (title) comprising a silicon oxygen compound with the formula SiOx in addition to a water-soluble lithium silicate, Li-2SiO3, and a water-soluble lithium silicate, Li2Si2O5 (para. [0029]). Furthermore, Hirose discloses the greatest 29Si-MAS-NMR spectrum peak intensity associated with Li-2SiO3, A, and associated with Li2Si2O5, C (para. [0027]), according to the preferred embodiment in formula 2 where 5C≤A (para. [0030]). Therefore, it can be concluded that the following relationship must be true: C/A≤1/5, which overlaps the claimed range. MPEP 2144.05 I. It is known in the art as evidenced by Padden et al. that magic-angle spinning (MAS) NMR can be used analytically to characterize crystals (1st full paragraph of page 2) and that the peak intensity ratio associated with two crystal forms producing peaks at unique chemical shifts can be used to approximate the relative composition of each crystal form (2nd full paragraph of page 4). Furthermore, it is known in the art as evidenced by Ahmad that the peak intensity in an XRD pattern is associated with the abundance and orientation of the crystal planes producing the peak (6th paragraph). Because the negative electrode active material of Li is a core-shell particle which is an isotropic structure, the abundance of crystal forms should primarily govern peak intensity. Therefore, the NMR peak intensity ratio should approximate the XRD peak intensity ratio for associated with Li-2SiO3 and Li2Si2O5.
Furthermore, Hirose teaches that when the content of Li-2SiO3 is high relative to Li2Si2O5 the Si crystallinity is suppressed, improving cycle characteristics (para. [0070]). Furthermore, when the ratio of Li2Si2O5 to Li-2SiO3 is further suppressed, cycle characteristics are further improved (para. [0072]).
Therefore, it would have been obvious to one of ordinary skill in the art before the time of the effective filing date of the claimed invention to have reduced the ratio of Li2Si2O5 to Li-2SiO3 to less than 1/5 as taught by Hirose to improve cycle characteristics in the composite active negative electrode material of Li.
Regarding claim 2, Li discloses a silicon-oxygen composite active negative electrode material (title) comprising a pre-lithiated silicon-oxygen core having the formula SiOx-Li (5th paragraph of page 2). Furthermore, water soluble Li-2SiO3 can be formed inside the silicon-oxygen material and water insoluble Li2Si2O5 can be formed on the surface (3rd to last paragraph of page 2). The resulting core-shell structure is represented in a cross-sectional view of the pre-lithiated silicon-oxygen composite material (Fig. 1) in which the lithium silicate contains the silicon oxygen material in the core (5th paragraph of page 2).
However, Li fails to teach that the intensity of a strongest diffraction characteristic peak from an XRD pattern of the water-soluble lithium silicate, IB, to the lithium silicate, IA, is within the claimed range of 0.03≤IB/IA≤0.2.
Hirose teaches a negative electrode active material (title) comprising a silicon oxygen compound with the formula SiOx in addition to a water-soluble lithium silicate, Li-2SiO3, and a water-soluble lithium silicate, Li2Si2O5 (para. [0029]). Furthermore, Hirose discloses the greatest 29Si-MAS-NMR spectrum peak intensity associated with Li-2SiO3, A, and associated with Li2Si2O5, C (para. [0027]), according to the preferred embodiment in formula 2 where 5C≤A (para. [0030]). Therefore, it can be concluded that the following relationship must be true: C/A≤1/5, which overlaps the claimed range. MPEP 2144.05 I. It is known in the art as evidenced by Padden et al. that magic-angle spinning (MAS) NMR can be used analytically to characterize crystals (1st full paragraph of page 2) and that the peak intensity ratio associated with two crystal forms producing peaks at unique chemical shifts can be used to approximate the relative composition of each crystal form (2nd full paragraph of page 4). Furthermore, it is known in the art as evidenced by Ahmad that the peak intensity in an XRD pattern is associated with the abundance and orientation of the crystal planes producing the peak (6th paragraph). Because the negative electrode active material of Li is a core-shell particle which is an isotropic structure, the abundance of crystal forms should primarily govern peak intensity. Therefore, the NMR peak intensity ratio should approximate the XRD peak intensity ratio for associated with Li-2SiO3 and Li2Si2O5.
Furthermore, Hirose teaches that when the content of Li-2SiO3 is high relative to Li2Si2O5 the Si crystallinity is suppressed, improving cycle characteristics (para. [0070]). Furthermore, when the ratio of Li2Si2O5 to Li-2SiO3 is further suppressed, cycle characteristics are further improved (para. [0072]).
Therefore, it would have been obvious to one of ordinary skill in the art before the time of the effective filing date of the claimed invention to have reduced the ratio of Li2Si2O5 to Li-2SiO3 to less than 1/5 as taught by Hirose to improve cycle characteristics in the composite active negative electrode material of Li.
Regarding claim 3, Li teaches that the lithium silicate comprises Li-2SiO3 and Li2Si2O5 (para. [0029]).
Regarding claim 4, Li further teaches that negative electrode material is further coated with a carbon layer (3rd paragraph of page 2, Fig. 1), and that the thickness of the carbon layer is less than 200 nm (7th paragraph of page 3) hence overlapping the claimed range of 30 nm – 500 nm. MPEP 2144.05 I.
Regarding claim 14, Li teaches that the lithium silicate comprises Li-2SiO3 and Li2Si2O5 (para. [0029]).
Regarding claim 15, Li teaches that the negative electrode material is further coated with a carbon layer (3rd paragraph of page 2), and that the thickness of the carbon layer is less than 200 nm (7th paragraph of page 3) hence overlapping the claimed range of 30 nm – 500 nm. MPEP 2144.05 I.
Regarding claim 16, Li teaches that the negative electrode material is further coated with a carbon layer (3rd paragraph of page 2, Fig. 1), and that the thickness of the carbon layer is less than 200 nm (7th paragraph of page 3) hence overlapping the claimed range of 30 nm – 500 nm. MPEP 2144.05 I.
Conclusion
11. The prior art made of record and not relied upon is considered pertinent to applicant's disclosure. Jiang (KR 20210096289A) teaches an anode active material (title) which comprises silicon monoxide doped with carbon (abstract) which has a carbon mass content of 0.5% to 10% in one embodiment. Takeshita (US Patent 10,427,943 B2) teaches a negative electrode material (Col. 1 Ln. 6-10) comprising silicon oxide powder with the formula SiOx where 0.5≤x≤1.5.
12. Any inquiry concerning this communication or earlier communications from the examiner should be directed to NATHAN ANDREW JON MCMULLEN whose telephone number is (571)270-0127. The examiner can normally be reached 7:30 am - 5:00 pm.
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/N.A.M./
Nathan A McMullen
Examiner, Art Unit 1788
08/20/2026
/Alicia Chevalier/Supervisory Patent Examiner, Art Unit 1788
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