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 .
Continued Examination Under 37 CFR 1.114
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on June 13, 2025 has been entered.
Response to Amendment
Applicant’s amendments filed June 13, 2025 have been entered. Claim 5 has been amended to fix a typographical error. Claims 1-20 remain pending with claims 4-12 and 14-20 remaining withdrawn. Claims 1-3 and 13 have been examined on their merits in this office action.
Response to Arguments
Applicant’s arguments filed June 13, 2025 have been fully considered. Applicant argues a) the distinguishing feature of Li2Si2O5 crystalline grains having an average grain size of less than 20 interacts and cooperates with the other features in claim 1 to achieve unexpected results of significantly improving the cycle performance and rate capability of the negative electrode material and b) Matus discloses the average grain size of Si:LSC matrix instead of the average grain size of Li2Si2O5 crystalline grains.
Regarding argument A, while Pang does not explicitly teach the specific average grain size of Li2Si2O5 crystalline grains, Pang teaches a method of preparation of the negative electrode material with a substantially identical process as the one in the claimed invention.
Pang teaches the negative electrode material is prepared by (1) blending a carbon-coated silicon oxide and a lithium source by solid-phase mixing mode to implement primary treatment to form a pre-lithium precursor; and (2) heat-treating the pre-lithium precursor in vacuum or a non-oxidizing atmosphere to implement structural adjustment and secondary treatment to form the composite (see e.g., paragraph [0072]), wherein the carbon-coated silicon oxide is produced via a carbonization treatment at a temperature from 500 to 1300 °C and for a time of 1 to 10 hours (see e.g., paragraphs [0047] and [0050]-[0051]).
In the claimed invention, Applicant discloses the preparation of the negative electrode material includes the following steps: S100, performing heat treatment on a silicon oxygen material under a protective atmosphere or vacuum to obtain a heat-treated silicon oxygen material; S200, mixing the heat-treated silicon oxygen material with a lithium source under a protective atmosphere or vacuum, and then performing sintering to obtain a negative electrode material, wherein the negative electrode material includes nano-silicon, silicon oxide, and crystalline Li2Si2O5 (see e.g., Instant Specification paragraphs [0076]-[0078] of the Published Patent Application US 2022/0328816 A1). Specifically, Applicant teaches, in S100, the temperature of the heat treatment is 600 °C to 1000 °C and time of the heat treatment is 4 to 10 hours (see e.g., Instant Specification paragraphs [0085]-[0086]). Applicant teaches, in S200, the protective atmosphere includes at least one selected from the group consisting of nitrogen gas, helium gas, neon gas, argon gas, krypton gas, and xenon gas, and the temperature of sintering is 300 °C to 900 °C (see e.g., Instant Specification paragraphs [0100]-[0101]).
Pang teaches the method can effectively reduce or even avoid the agglomeration problem among nano-silicons, thereby reducing the silicon expansion problem in the process of application to a battery (see e.g., paragraph [0016]) and produces a battery that exhibits high delithiation capacity, high initial coulombic efficiency and good cycling performance, which has a charge capacity of 1920 mAh/g or more, a discharge capacity of 1768 mAh/g or more and an initial efficiency of 90.2% or more (see e.g., paragraph [0008]) similar to the discharging specific capacity and first efficiency results produced by Applicant in Table 1.
Therefore, while Pang does not explicitly teach the specific average grain size of Li2Si2O5 crystalline grains is less than 20 nm, this property is considered inherent in the prior art barring any difference shown by objective evidence between the negative electrode material disclosed in Pang and the Applicant. As the negative electrode taught by the prior art and the Applicant are identical within the scope of claim 1, Pang inherently teaches the crystalline grains of Li2Si2O5 have an average grain size of less than 20 nm. Where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established. In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977) (see MPEP 2112.01).
Therefore, Applicant’s argument has been fully considered but is not found to be persuasive.
Regarding argument B, Applicant’s argument has been fully considered but is considered moot in view of the new grounds of rejection below.
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.
(a)(2) the claimed invention was described in a patent issued under section 151, or in an application for patent published or deemed published under section 122(b), in which the patent or application, as the case may be, names another inventor and was effectively filed before the effective filing date of the claimed invention.
Claims 1-3 and 13 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Pang et al. (CN 106816594 A, citations from corresponding patent application US 2020/0058924 A1), hereinafter referred to as Pang.
Regarding claim 1, Pang teaches a negative electrode material (see e.g., Abstract, an electrode material), wherein the negative electrode material comprises nano-silicon (see e.g., paragraph [0011], said composite comprising nano silicon), silicon oxide (see e.g., paragraph [0011], said composite further comprises silicon oxide), and crystalline Li2Si2O5 (see e.g., paragraph [0025], the silicon compound comprises Li2Si2O5).
Pang teaches an SEM image of the compound (see e.g., Figure 3) in which it can been that dark regions formed by a nano-silicon inlaid lithium-containing compound were uniformly distributed in the particle, which formed a sea-island structure in which the lithium-containing compound inlaid with nano-silicon was served as islands, and silicon oxide was served as the sea (see e.g., paragraph [0082]). In the SEM image of the compound, the grain sizes of the lithium-containing compound are on the scale of the recited 20 nm in the claimed invention.
Pang does not explicitly teach the specific average grain size of Li2Si2O5 crystalline grains.
However, Pang teaches the negative electrode material is prepared by (1) blending a carbon-coated silicon oxide and a lithium source by solid-phase mixing mode to implement primary treatment to form a pre-lithium precursor; and (2) heat-treating the pre-lithium precursor in vacuum or a non-oxidizing atmosphere to implement structural adjustment and secondary treatment to form the composite (see e.g., paragraph [0072]), wherein the carbon-coated silicon oxide is produced via a carbonization treatment at a temperature from 500 to 1300 °C and for a time of 1 to 10 hours (see e.g., paragraphs [0047] and [0050]-[0051]). Specifically, Pang teaches embodiments of the heat treatment under specific conditions comprises being under an argon atmosphere and heat treated at 500 °C for 2 hours (see e.g., Examples 1-4), under an argon atmosphere and heat treated at 500 °C for 1.5 hours (see e.g., Example 5), under a nitrogen atmosphere and heat treated at 300° C. for 6 h (see e.g., Example 6), and under an argon atmosphere at 900° C. for 2 h (see e.g., Example 7).
In the claimed invention, Applicant discloses the preparation of the negative electrode material includes the following steps: S100, performing heat treatment on a silicon oxygen material under a protective atmosphere or vacuum to obtain a heat-treated silicon oxygen material; S200, mixing the heat-treated silicon oxygen material with a lithium source under a protective atmosphere or vacuum, and then performing sintering to obtain a negative electrode material, wherein the negative electrode material includes nano-silicon, silicon oxide, and crystalline Li2Si2O5 (see e.g., Instant Specification paragraphs [0076]-[0078] of the Published Patent Application US 2022/0328816 A1). Specifically, Applicant teaches, in S100, the temperature of the heat treatment is 600 °C to 1000 °C and time of the heat treatment is 4 to 10 hours (see e.g., Instant Specification paragraphs [0085]-[0086]). Applicant teaches, in S200, the protective atmosphere includes at least one selected from the group consisting of nitrogen gas, helium gas, neon gas, argon gas, krypton gas, and xenon gas, and the temperature of sintering is 300 °C to 900 °C (see e.g., Instant Specification paragraphs [0100]-[0101]).
Therefore, while Pang does not explicitly teach the specific average grain size of Li2Si2O5 crystalline grains is less than 20 nm, this property is considered inherent in the prior art barring any difference shown by objective evidence between the negative electrode material disclosed in Pang and the Applicant. As the negative electrode taught by the prior art and the Applicant are identical within the scope of claim 1, Pang inherently teaches the crystalline grains of Li2Si2O5 have an average grain size of less than 20 nm. Where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established. In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977) (see MPEP 2112.01).
Regarding claim 2, Pang teaches the instantly claimed invention of claim 1, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions a-c:
a chemical formula of the silicon oxide is SiOx, where 0 < x ≤ 1 (see e.g., paragraph [0012], the chemical composition of the silicon oxide is SiOx, x is more than 0 and less than < 2, wherein x can be 0.1, 0.2, 0.5, 0.6, 0.8, 1, 1.2, 1.5, 1.75 or 1.8); and
the silicon oxide and the Li2Si2O5 have the nano-silicon dispersed therein (see e.g., Figure 2 and paragraph [0078], reference number 2 represents a lithium-containing compound, reference number 3 represents nano-silicon, and reference number 4 represents a silicon oxide and Figure 2 shows the silicon oxide and the Li2Si2O5 have the nano-silicon dispersed therein);
the Li2Si2O5 covers at least part of the nano-silicon (see e.g., Figure 2 and paragraph [0078], reference number 2 represents a lithium-containing compound, reference number 3 represents nano-silicon, and reference number 4 represents a silicon oxide and Figure 2 shows the Li2Si2O5 covers at least part of the nano-silicon)
Regarding claim 3, Pang teaches the instantly claimed invention of claim 1, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions a:
a carbon coating layer is formed on a surface of the negative electrode material (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound).
Regarding claim 13, Pang teaches the instantly claimed invention of claim 2, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions a:
a carbon coating layer is formed on a surface of the negative electrode material (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound).
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.
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 2-3 and 13 are rejected under 35 U.S.C. 103 as being unpatentable over Pang et al. (CN 106816594 A, citations from corresponding patent application US 2020/0058924 A1).
Regarding claim 2, Pang teaches the instantly claimed invention of claim 1, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions f: the negative electrode material has an average grain size of 1 µm to 50 µm (see e.g., Figure 3, in the SEM image, the grain sizes of the composite appear to have an average grain size of less than 10 µm); it has been held in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art,” and because the average grain size of less than 10 µm overlap with the recited range, a “primia facie” case of obviousness exists (see MPEP 2144.05(l)).
Regarding claim 3, Pang teaches the instantly claimed invention of claim 1, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions b and c:
a carbon coating layer is formed on a surface of the negative electrode material, and the carbon coating layer has a thickness of 10 nm to 2000 nm (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound; see e.g., paragraph [0045], the carbon coating has a thickness of 3-800 nm); it has been held in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art,” and because thickness of 3-800 nm overlap with the recited range, a “primia facie” case of obviousness exists (see MPEP 2144.05(l)); and
a carbon coating layer is formed on a surface of the negative electrode material, and a mass fraction of the carbon coating layer in the negative electrode material is 1 wt% to 10 wt% (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound; see e.g., paragraph [0055], he mass ratio of the carbon-coated silicon oxide to the lithium source in step (1) is 1:(0.01-0.3)); it has been held in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art,” and because thickness of 0.01-0.3 overlap with the recited range, a “primia facie” case of obviousness exists (see MPEP 2144.05(l)).
Regarding claim 13, Pang teaches the instantly claimed invention of claim 2, as previously described.
Pang teaches the negative electrode material, satisfying at least one of following conditions b and c:
a carbon coating layer is formed on a surface of the negative electrode material, and the carbon coating layer has a thickness of 10 nm to 2000 nm (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound; see e.g., paragraph [0045], the carbon coating has a thickness of 3-800 nm); it has been held in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art,” and because thickness of 3-800 nm overlap with the recited range, a “primia facie” case of obviousness exists (see MPEP 2144.05(l)); and
a carbon coating layer is formed on a surface of the negative electrode material, and a mass fraction of the carbon coating layer in the negative electrode material is 1 wt% to 10 wt% (see e.g., paragraph [0073], a carbon coating coated on the surface of the composite comprising nano-silicon, a silicon oxide, a lithium-containing compound; see e.g., paragraph [0055], he mass ratio of the carbon-coated silicon oxide to the lithium source in step (1) is 1:(0.01-0.3)); it has been held in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art,” and because thickness of 0.01-0.3 overlap with the recited range, a “primia facie” case of obviousness exists (see MPEP 2144.05(l)).
Conclusion
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/KATHERINE N HIGGINS/Examiner, Art Unit 1728
/MATTHEW T MARTIN/Supervisory Patent Examiner, Art Unit 1728