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 .
Status of Application
Claim 1, 16 and 20 are amended, claim 11 is cancelled and claim 21 is new, submitted on 2/2/2026. Claim 16 remains withdrawn. Claims 1-8, 10, 12-15, and 17-21 are presented for examination.
Claim Rejections - 35 USC § 103
1. 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.
2. The factual inquiries set forth in Graham v. John Deere Co., 383 U.S. 1, 148 USPQ 459 (1966), that are applied 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.
3. 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.
4. Claims 1, 3, 10, 12, 17, and 19-21 are rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia (https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024), in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1).
Regarding claim 1, Soichiro discloses a negative electrode active material layer ([0015]) composed of a composite of silicon particles and carbon ([0014]), an amorphous surface layer 101 may include amorphous carbon ([0034] and FIG. 1a and FIG. 2c), and silicon particles 100 may be 5 to 200 nm, ([0033] and FIG. 1a and FIG. 2c), which reads on the claimed “comprising: an amorphous carbon matrix; and silicon nanoparticles dispersed in the amorphous carbon matrix”.
Soichiro further discloses a negative electrode active material comprising a silicon-carbon composite 110 containing at least one member selected from the group consisting of graphene structured carbon particles 112, fibrous carbon 113, and carbon black 114 ([0039] and FIGs. 2a and 2b) and the fibrous carbon particles 113 may include one or more types selected from the group consisting of carbon nanofibers and carbon nanotubes ([0044]). A skilled artisan would find it obvious to select fibrous carbon 113 from the above finite list of carbon choices to form the silicon-carbon composite particles 110 ([0039] FIG. 2b) and it would be further obvious to select carbon nanotubes as the fibrous carbon 113 ([0044] and [0140]), as taught by Soichiro.
According to definitions from Wikipedia, Carbon nanofibers and carbon nanotubes are crystalline carbon structures with graphene layers, and carbon nanofibers with graphene layers wrapped into perfect cylinders are called carbon nanotubes (Carbon nanofiber, Wikipedia https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024). This means carbon nanotube is a species of carbon nanofibers, and carbon nanotube taught by modified Soichiro corresponds to crystalline carbon fibers in the instant claim.
Thus, it would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to arrive at the claimed “the negative electrode active material comprising crystalline carbon fibers; and the silicon nanoparticles being in contact with a portion or all of the crystalline carbon fibers” because FIG. 2b shows silicon particles 111 are in contact with a portion or all of the fibrous carbon 113 which has been selected to be carbon nanotubes.
However, modified Soichiro does not explicitly disclose the crystalline carbon fibers (carbon nanotubes) dispersed in the amorphous carbon matrix.
Soichiro further discloses the electronic conductivity of the secondary battery negative electrode can be improved by adding the conductive composition, and thus the performance of the battery can be improved ([0028]); matters regarding the silicon particle 100 and its surface layer 101 are the same as those described in the first embodiment ([0041-42] and FIG. 2c) and a sintering (calcination) process of drying and calcining the slurry to obtain a negative electrode active material may be further included, thereby producing silicon particles having a surface layer of amorphous carbon according to the first embodiment or silicon particles-carbon according to the second embodiment ([0067]) such as, mixing multi-layer carbon nano in a mixed solution([0104]) and later, the mixture was heat-treated at 800° C in an argon gas atmosphere in a sintering furnace to prepare a silicon-lithium ion inorganic solid electrolyte-carbon composite ([0108]). Thus, It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to use the silicon particle-carbon composite of FIG. 2b instead of silicon particles, having the silicon particle-carbon composite of FIG. 2b covered with an amorphous carbon layer as taught by Soichiro, and arrive at the claimed “crystalline carbon fibers dispersed in the amorphous carbon matrix” without undue experimentation and with a reasonable expectation of success.
Therefore, it would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to arrive at the claimed “a negative electrode active material composite, comprising: an amorphous carbon matrix; and silicon nanoparticles and crystalline carbon fibers dispersed in the amorphous carbon matrix, and the silicon nanoparticles being in contact with a portion or all of the crystalline carbon fibers in the amorphous carbon matrix” as taught by Soichiro, without undue experimentation and with a reasonable expectation of success.
However, while modified Soichiro further discloses the desire of solving the problems with silicon caused volume expansion of about four times ([0005]) and improving electronic conductivity of the cathode ([0036]) (Examiner notes: the terminology of “cathode” and “anode” are used or translated interchangeably in Soichiro), modified Soichiro does not explicitly disclose the amorphous carbon matrix completely fills any space between the crystalline carbon fibers and the silicon nanoparticles.
Yu teaches similar concerns about silicon as a negative electrode, such as low electrical conductivity and large volume expansion caused capacity decay ([0002]), and provides a textured carbon-coated nano-silicon composite powder aiming to improve the technical problem that the existing carbon-coated nano-silicon composite powder cannot effectively inhibit the volume expansion of the silicon system during the lithium ion insertion and extraction process, resulting in poor electrochemical performance ([0004] and FIGs. 1-3). Yu further teaches the textured carbon coating layer includes pyrolytic amorphous carbon and a plurality of graphene nanosheets distributed at intervals with each graphene nanosheet being connected to the surface of nano-scale silicon powder and extending radially of the nano-scale silicon powder; and the pyrolytic amorphous carbon fills the gap between two adjacent graphene nanosheets ([0005] and FIGs. 1-3) by first forming a plurality of graphene nanotubes extending radially along the nano-silicon powder on the surface of the nano-silicon powder to obtain an intermediate; and then filling the gaps between the graphene nanosheets of the intermediate with pyrolyzed amorphous carbon ([0031]); and the pyrolytic amorphous carbon is always filled in the gaps of the graphene nanosheet, beneficial to maintain the structural stability of the entire textured carbon-coated nano-silicon composite powder ([0006] and FIGs. 1-3), which teaches the amorphous carbon matrix completely fills any space between the crystalline graphene nanosheets and the silicon nanoparticles.
Therefore, it would have been obvious for a skilled artisan before the effective filing date of the claimed invention to add the pyrolyzed amorphous carbon taught by Yu, in the voids of modified Soichiro thus arriving the claimed “the amorphous carbon matrix completely filling any space between the crystalline carbon fibers and the silicon nanoparticles”, in order to effectively inhibit the volume expansion of the silicon system during the lithium ion insertion and extraction process, as desired by modified Soichiro.
Soichiro further discloses for Example M1 ([0100]), as a starting material, a mixed powder of 95 parts by weight of silicon powder and 5 parts by weight of graphite powder was used ([0102]), and Example M1, with 26 parts by weight of silicon and artificial graphite, 12 parts by weight of carbon nanotubes, an electrode layer forming slurry was prepared ([0140]), which translates to a weight ratio of the silicon nanoparticles and the crystalline carbon fibers of 2.06 : 1 {Calculation: (26% x 95%) / 12% = 2.06}; and Example M2 with 99% of silicon powder added with 0.1% of coal tar pitch by weight based on silicon ([0111]) followed by same forgoing mixing ratio ([0140]), which translates to a weight ratio of the silicon nanoparticles and the crystalline carbon fibers of 2.15 : 1 {Calculation: (26% x 99%) / 12% = 2.06}, thus falling out of the claimed range “a weight ratio of greater than or equal to 4”.
However, modified Soichiro does not limit the weight ratio between the silicon nanoparticle and the crystalline carbon fibers in the negative electrode active material composite, thus encompassing the claimed weight ratio of greater than or equal to 4.
Modified Soichiro further discloses the order of abundance of SiOx is Reference Example M2> Example M2> Reference Example M1> Example M1 ([0133]); and the testing data shown in Table 1 ([0155]), in that, the Reference Example M2 has overall better results regarding the current characteristics of Li desorption amount (capacity) under various current value C-rate when compared to that of the Reference Example M1. Therefore, It would have been obvious to a skilled artisan before the effective filing date of the claimed invention, a skilled artisan would use a higher weight ratio of silicon nanoparticles higher than 2.15 (Example M2) as taught by Table 1 testing results (Reference Example M2 vs. Reference Example M1) in order to improve current characteristics of Li desorption amount (capacity), and with a reasonable expectation of success in obtaining a negative electrode active material composite that includes a value of the weight ratio of the silicon nanoparticles and the crystalline carbon fibers that falls within the claimed range of greater than or equal to 4, under routine experimentation, absent evidence to the contrary for secondary consideration.
Modified Soichiro does not explicitly discloses D50 of the negative electrode active material composite is about 35 times to about 300 times that of the silicon nanoparticles.
Instead, modified Soichiro further discloses the average particle diameter of silicon powder observed with a scanning electron microscope was 50 to 200 nm ([0111]); and silicon-carbon composite 110 may have an average particle diameter of 5 to 20 µm ([0046]) corresponding to the claimed average particle diameter of the negative electrode active material composite, which translates to an average particle diameter of the negative electrode active material composite is about 25 times to about 400 times an average particle diameter of the silicon nanoparticles, encompassing the claimed range of about 35 times to about 300 times.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, under routine experimentation to arrive at a value that falls within the overlapping portion between the taught range and the claimed range (about 35 times to about 300 times), regarding an average particle diameter of the negative electrode active material composite and an average particle diameter of the silicon nanoparticles with a reasonable expectation of success in achieving a desired silicon-carbon composite negative electrode active material.
Modified Soichiro does not explicitly disclose Raman spectrum analysis of the carbon nanotubes (crystalline carbon fibers), a peak intensity ratio (ID/IG) of a peak intensity (ID) of a D peak (1350 to 1370 cm-1) to a peak intensity (ID') of a G peak (1570 to 1620 cm-1) is about 0.2 to about 0.5.
Azami teaches carbon nanotubes as conductive agent of an electrode for a secondary battery ([0010-0011]) and it is preferable that the average D/G ratio obtained from Raman spectroscopy is 0.2 or more, and 0.4 or less to improve charge-discharge cycle characteristics of the battery because the carbon nanotubes having D/G ratio within above range have few defects and low electronically resistance ([0060]) with G band near 1580 to 1600 cm-1 and D band near 1360 cm-1 ([0061]), which falls within the peak intensity ratio range, as well as the D peak and G peak ranges as claimed “wherein in Raman spectrum analysis of the crystalline carbon fibers, a peak intensity ratio (ID/IG) of a peak intensity (ID) of a D peak (1350 to 1370 cm-1) to a peak intensity (ID') of a G peak (1570 to 1620 cm-1) is about 0.2 to about 0.5”.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to choose carbon nanotubes as the crystalline carbon fiber that having characteristic of Raman spectrum analysis falling within the range as claimed “a peak intensity ratio (ID/IG) of a peak intensity (ID) of a D peak (1350 to 1370 cm-1) to a peak intensity (ID') of a G peak (1570 to 1620 cm-1) is about 0.2 to about 0.5”, as taught by Azami, by using carbon nanotubes having few defects and low electronically resistance, in order to improve charge-discharge cycle characteristics of the battery.
Regarding claim 3, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses the primary particle has the long diameter (a) > short diameter (b), and the long diameter may be 50 to 300 nm, the minor diameter may be 30 to 200 nm ([0037]), which translates to an aspect ratio of the silicon nanoparticles is between 1.7 to 10, falling within the claimed range of an aspect ratio of the silicon nanoparticles of about 1 to about 20.
Regarding claim 10, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses the amorphous surface layer 101 may include amorphous carbon ([0034]), and it is possible to generate amorphous carbon on the surface of the silicon particles by irradiating ultrasonic energy to a slurry in which silicon particles are dispersed in a solution of coal tar pitch, petroleum pitch, or polycyclic aromatic compound to form carbon-coated silicon particles ([0065]), additionally, a sintering (calcination) process of drying and calcining the slurry to obtain a negative electrode active material may be further included ([0067]), which inherently reads on the claimed “the amorphous carbon matrix includes soft carbon, hard carbon, a mesophase pitch carbonized product, or a mixture thereof.” because coal tar pitch and petroleum pitch are well-known precursors to form soft carbon such as activated carbon, hard carbon, or a mesophase pitch carbonized product, or a mixture thereof, with calcination.
Regarding claim 12, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses by using the negative electrode active material in the negative electrode, electrical storage devices such as lithium secondary batteries can have the performance of high energy density, high power density, and longer charge and discharge cycle life ([0026]); and for Example M1 ([0100]), as a starting material, a mixed powder of 95 parts by weight of silicon powder and 5 parts by weight of graphite powder was used ([0102]), and Example M1, after mixing and kneading to obtain 49 parts by weight, 12 parts by weight of carbon nanotubes, and 12 parts by weight of polyamic acid solids, an electrode layer forming slurry was prepared ([0140]). It would have been obvious for a skilled artisan before the effective filing date of the claimed invention, to arrive at the claim limitation “based on a total weight of the negative electrode active material composite, the silicon nanoparticles are included in an amount of about 40 wt% to about 70 wt%, the crystalline carbon fibers are included in an amount of about 1 wt% to about 20 wt%” as taught by Example M1 of Soichiro with a reasonable expectation of success.
Although, Soichiro does not explicitly disclose that the amorphous carbon matrix is included in an amount of about 10 wt% to about 50 wt% based on a total weight of the negative electrode active material composite, the Example M1 data indicates the maximum amount of amorphous carbon matrix would be 27% (calculation: 1-49%-12%-12%= 27%), which falls within the claimed weight ratio range of about 10 wt% to about 50 wt%.
Alternatively, Soichiro further discloses the electronic conductivity of the cathode can be improved through carbonization or graphitization of the carbon precursor through sintering ([0035]); the thickness of the amorphous surface layer 101 may be 1 to 10 nm. If the thickness of the amorphous surface layer 101 is less than 1 nm, it is insufficient to prevent oxidation of the silicon particles 100 because the surface layer 101 is too thin, and if it is larger than 10 nm, insertion of lithium ions into the active materials is inhibited ([0036]). A skilled artisan would be motivated to optimize the thickness of the amorphous carbon matrix to obtain a good balance between preventing oxidation of the silicon-carbon composite and improving efficiency of lithium ion insertion, and therefore, would have a reasonable expectation of such optimization would arrive at the claimed weight ratio range for the amorphous carbon matrix with a desired balance, in order to achieve the performance of high energy density, high power density, and longer charge and discharge cycle life, as desired by Soichiro.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to arrive at the claimed “based on a total weight of the negative electrode active material composite, the amorphous carbon matrix is included in an amount of about 10 wt% to about 50 wt%” without undue experimentation and with a reasonable expectation of success, as taught by Soichiro, in order to achieve the performance of high energy density, high power density, and longer charge and discharge cycle life for the negative electrode active material composite.
Regarding claim 17, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses a method of manufacturing an electrode structure for a negative electrode of a storage device such as a lithium secondary battery ([0014]) and that referring to FIG. 6, the eighth embodiment may be a negative electrode structure 305 including a conductive metal (current collector) 300 and a negative electrode material layer 304 formed on the conductive metal 300 ([0088]), which reads on the claimed “a negative electrode for a rechargeable lithium battery, the negative electrode comprising a current collector and a negative electrode active material layer on the current collector, the negative electrode active material layer including the negative electrode active material composite as claimed in claim 1.”
Regarding claim 19, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses a rechargeable lithium battery ([0026]), comprising: a positive electrode ([0025]); a negative electrode ([0026]); and an electrolyte ([0025]), wherein the negative electrode is the negative electrode as claimed in claim 17 ([0026]).
Regarding claim 20, modified Soichiro discloses all of the limitations as set forth above. As established above, modified Soichiro has silicon nanoparticles in contact with the fibrous carbon 113 which has been selected to be carbon nanotubes (FIG. 2b)as the crystalline carbon fibers. Modified Soichiro further discloses since the fibrous carbon is electronically conductive among other alternatives, any one or more of them exists in contact with the silicon particles, thereby improved battery performance can be achieved by improving the electronic conductivity ([0047]). It would have been obvious to a skilled artisan before the effective filing date of the claimed invention to have ensured that all silicon particles are in contact with the crystalline carbon fibers in order to achieve an optimized electronic conductivity of the obtained negative electrode active material composite and thereby improved battery performance, with a reasonable expectation of success without undue experimentation, absent evidence to the contrary for secondary consideration.
Regarding claim 21, modified Soichiro discloses all of the limitations as set forth above. As established above in claim 1, Soichiro further discloses for Example M1 ([0100]), as a starting material, a mixed powder of 95 parts by weight of silicon powder and 5 parts by weight of graphite powder was used ([0102]), and Example M1, with 26 parts by weight of silicon and artificial graphite, 12 parts by weight of carbon nanotubes, an electrode layer forming slurry was prepared ([0140]), which translates to a weight ratio of the silicon nanoparticles and the crystalline carbon fibers of 2.06 : 1 {Calculation: (26% x 95%) / 12% = 2.06}; and Example M2 with 99% of silicon powder added with 0.1% of coal tar pitch by weight based on silicon ([0111]) followed by same forgoing mixing ratio ([0140]), which translates to a weight ratio of the silicon nanoparticles and the crystalline carbon fibers of 2.15 : 1 {Calculation: (26% x 99%) / 12% = 2.06}, thus falling out of the claimed range “a weight ratio of greater than or equal to 9”.
However, modified Soichiro does not limit the weight ratio between the silicon nanoparticle and the crystalline carbon fibers in the negative electrode active material composite, thus encompassing the claimed weight ratio of greater than or equal to 9.
Modified Soichiro further discloses the order of abundance of SiOx is Reference Example M2> Example M2> Reference Example M1> Example M1 ([0133]); and the testing data shown in Table 1 ([0155]), in that, the Reference Example M2 has overall better results regarding the current characteristics of Li desorption amount (capacity) under various current value C-rate when compared to that of the Reference Example M1. Therefore, It would have been obvious to a skilled artisan before the effective filing date of the claimed invention, a skilled artisan would use a higher weight ratio of silicon nanoparticles higher than 2.15 (Example M2) as taught by Table 1 testing results (Reference Example M2 vs. Reference Example M1) in order to improve current characteristics of Li desorption amount (capacity), and with a reasonable expectation of success in obtaining a negative electrode active material composite that includes a value of the weight ratio of the silicon nanoparticles and the crystalline carbon fibers that falls within the claimed range of greater than or equal to 9, under routine experimentation, absent evidence to the contrary for secondary consideration.
5. Claims 2 and 13 are rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia (https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024), in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1), as applied to claim 1, further in view of Park (CA 3235877 A1).
Regarding claim 2, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses the obtained slurry was dried and the average particle diameter of silicon powder observed with a scanning electron microscope was 50 to 200 nm ([0111]), which reads on the claimed “an average particle diameter (D50) of the silicon nanoparticles is about 50 nm to about 200 nm”.
While Soichiro discloses the challenge to suppress agglomeration of particles during post-drying and a method of pulverizing silicon materials into fine particles ([0007]), Soichiro does not explicitly disclose a maximum particle diameter (Dmax) is about 80 nm to about 300 nm.
Park teaches the active material layer of the second electrode may include a silicon-based negative electrode active material and a carbon-based negative electrode active material (Ln9-10/P14). Park further teaches when Dmax of the positive electrode material satisfies a range, resistance characteristics and capacity characteristics are more excellent. If Dmax of the positive electrode active material is too large, aggregation has occurred between single particles, and the lithium movement path inside the agglomerated particles is lengthened, resulting in poor lithium mobility, which may increase resistance. Meanwhile, if Dmax of the positive electrode active material is too small by excessive crushing process, causes particles breakage during rolling and deteriorates thermal stability (Ln20/P92-Ln4/P93). Examiner notes even though Park takes positive electrode active material as an example, to explain the rationale for determining the Dmax range, same rationale applies to determining Dmax for negative electrode active material as well.
A skilled artisan would have found it obvious to control the Dmax of the silicon nanoparticles of Soichiro as taught by Park, in view of the average particle diameter of silicon powder being 50 to 200 nm, in order to achieve an optimized balance between resistance characteristics and capacity characteristics.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to control the Dmax of the silicon nanoparticles of Soichiro as taught by Park, and arrive at the claimed “a maximum particle diameter (Dmax) is about 80 nm to about 300 nm” with a reasonable expectation of success that selection of this range would provide an optimized balance between resistance characteristics and capacity characteristics.
Regarding claim 13, modified Soichiro discloses all of the limitations as set forth above. Soichiro further discloses the silicon-carbon composite 110 may have an average particle diameter of 5 to 20 µm ([0046]), which encompasses the claimed range of 7 to 15 µm for an average particle diameter (D50) of the negative electrode active material composite, establishing a prima facie case of obviousness. It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to select the overlapping portion of the range with a reasonable expectation of successfully arriving at a desired silicon-carbon composite.
Regarding the maximum particle diameter (Dmax) of the negative electrode active material composite, while Soichiro discloses the challenge to suppress agglomeration of particles during post-drying and a method of pulverizing silicon materials into fine particles ([0007]), Soichiro does not explicitly disclose a maximum particle diameter (Dmax) is about 10 µm to about 30 µm.
Park teaches the active material layer of the second electrode may include a silicon-based negative electrode active material and a carbon-based negative electrode active material (Ln9-10/P14). Park further teaches when Dmax of the positive electrode material satisfies a range, resistance characteristics and capacity characteristics are more excellent. If Dmax of the positive electrode active material is too large, aggregation has occurred between single particles, and the lithium movement path inside the agglomerated particles is lengthened, resulting in poor lithium mobility, which may increase resistance. Meanwhile, if Dmax of the positive electrode active material is too small by excessive crushing process, causes particles breakage during rolling and deteriorates thermal stability (Ln20/P92-Ln4/P93). Examiner notes even though Park takes positive electrode active material as an example, to explain the rationale for determining the Dmax range, same rationale applies to determining Dmax for negative electrode active material as well.
A skilled artisan would have found it obvious to control the Dmax of the silicon nanoparticles of Soichiro as taught by Park, in view of the average particle diameter of silicon-carbon composite 110 being 5 to 20 µm, in order to achieve an optimized balance between resistance characteristics and capacity characteristics.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to control the Dmax of the of the negative electrode active material composite of Soichiro as taught by Park, and arrive at the claimed “a maximum particle diameter (Dmax) is about 10 µm to about 30 µm” with a reasonable expectation of success that selection of this range would achieve an optimized balance between resistance characteristics and capacity characteristics.
6. Claim 4 is rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia (https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024), in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1), as applied to claim 1, further in view of Daulay (South African Journal of Chemical Engineering 42 (2022) 32-41).
Regarding claim 4, Soichiro discloses all of the limitations as set forth above. Soichiro further discloses in Figure 1 (c) and (d) that the Si nanoparticles in the SEM and TEM photos ([0038]) appear to be nano crystal structure (FIG. 1 (c) and (d)). While Soichiro discloses the challenge to suppress agglomeration of particles during post-drying and a method of pulverizing silicon materials into fine particles ([0007]), and the electronic conductivity of the secondary battery negative electrode can be improved by adding the conductive composition, and thus the performance of the battery can be improved ([0028]), Soichiro does not explicitly disclose the silicon nanoparticles have a reading of about 0.3° to about 1.0° regarding a full width at half maximum of an X-ray diffraction angle using CuKa ray at the (111) plane of the silicon nanoparticles.
Daulay teaches Si nanoparticles synthesized from rice husk are very good as material active electrode on secondary cell battery, having an electrical conductivity of 2599.39 µS/cm and a resistance of 3.84 Ω at 1 V (Abstract), and an XRD analysis quantified in full width at half maximum (FWHM) in Table 1 that β=FWHM (degree) is 0.35 (Table 1 , P34), which is within the claimed “a full width at half maximum of an X-ray diffraction angle using CuKa ray at the (111) plane of the silicon nanoparticles is about 0.3° to about 1.0°.”
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to utilize the method for preparation of the silicon nanoparticles of Soichiro, as taught by Daulay and arrive at the claimed “a full width at half maximum of an X-ray diffraction angle using CuKa ray at the (111) plane of the silicon nanoparticles is about 0.3° to about 1.0°”, in order to obtain a very good silicon based electrode active material with high electrical conductivity.
7. Claims 5-7 are rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia (https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024), in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1), as applied to claim 1, further in view of Chen (US 20120164531 A1).
Regarding claim 5, Soichiro discloses all of the limitations as set forth above. While Soichiro further discloses the desire of lithium ions may easily transport to the surface of the silicon particles when the power storage device operates ([0048]); if the surface of the silicon particle is oxidized, this oxide layer is electrically insulating, so the electronic conductivity of the cathode manufactured using it decreases, which can ultimately deteriorate the performance of the cathode and the power storage device ([0054]), and fibrous carbon 113 are electronically conductive, and battery performance can be improved by improving the electronic conductivity ([0047]), the silicon-carbon composite 110 may have an average particle diameter of 5 to 20 µm ([0046]), Soichiro does not disclose an average particle diameter (D50) of the crystalline carbon fibers is about 0.5 µm to about 3.0 µm, and a maximum particle diameter (Dmax) is about 3.0 µm to about 5.0 µm.
Chen teaches an energy storage composite particle includes a carbon film, a conductive carbon component, an energy storage grain, and a conductive carbon fiber. The conductive carbon fiber is electrically connected to the conductive carbon component, the energy storage grain, and the carbon film([0009]); and the carbon conductive carbon fiber may extend from inside of the energy storage composite particle to the outside, which is beneficial to reducing the contact impedance of the energy storage composite particle, so that the energy storage composite particle has superior electronic conductive path, thus obtaining a high power characteristic ([0067]). Chen further teaches the carbon film 110 surrounds a space S. The conductive carbon component 120 and the energy storage grain 130 are disposed in the space S. The conductive fiber 140 is electrically connected to the conductive carbon component 120, the energy storage grain 130, and the carbon film 110, and the conductive carbon fiber 140 extends from the inside of the space S to the outside of the space S ([0022]). The conductive carbon fiber 140 shown in FIG.3B photo appears to be around 1 µm, which falls within the range of about 0.5 µm to about 3 µm for an average particle diameter (D50) of the crystalline carbon fibers as claimed “an average particle diameter (D50) of the crystalline carbon fibers is about 0.5 µm to about 3.0 µm”.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to select the D50 of the crystalline carbon fibers of Chen in order to have a high power characteristic and with a reasonable expectation of success, and thus arrive at a value that is within the claimed limitation “an average particle diameter (D50) of the crystalline carbon fibers is about 0.5 µm to about 3.0 µm”.
In light of the silicon-carbon composite 110 of Soichiro having an average particle diameter of 5 to 20 µm, a skilled artisan would further optimize the maximum particle diameter (Dmax ) of the crystalline carbon fibers to about 5 µm, aiming to extend from inside of the energy storage composite particle to the outside, reducing the contact impedance of the energy storage composite particle, so that the energy storage composite particle has superior electronic conductive path, as taught by Chen, in order to obtain a high power characteristic ([0067]). On the other hand, a skilled artisan would have known that the maximum particle diameter (Dmax ) of the crystalline carbon fibers should not be excessively long because it would be entangled with each other reducing the electrical conducting efficiency and capacity of the electrode.
It would have been further obvious for a skilled artisan, before the effective filing date of the claimed invention, to select the Dmax of the crystalline carbon fibers based on the average particle diameter of silicon-carbon composite 110 of Soichiro, as taught by Chen, and arrive at a value that is within the claimed limitation “a maximum particle diameter (Dmax) is about 3.0 µm to about 5.0 µm” with a reasonable expectation of success that selection of this range would achieve an optimized balance between resistance characteristics and capacity characteristics.
Regarding claims 6 and 7, modified Soichiro discloses all of the limitations as set forth above. Chen further teaches a plurality of strip shaped the conductive carbon fiber 140 in FIG. 3B, which appears to have conductive carbon fiber of about 1 µm along its length, and 10 to 20 nm in its thickness direction (perpendicular to the length direction), which translates to an aspect ratio of about 50 to 100, falling within the aspect ratio range as claimed “wherein an aspect ratio of the crystalline carbon fibers is about 5 to about 300 (claim 6)”; and falling within the thickness range of the crystalline carbon fiber as claimed “wherein a thickness of the crystalline carbon fibers is about 10 nm to about 100 nm (claim 7).”
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to select the crystalline carbon fiber with an aspect ratio within the range of about 5 to about 300 (claim 6) or a thickness of the crystalline carbon fiber within the range of about 10 nm to about 100 nm (claim 7), as taught by Chen, in order to obtain an optimized balance between resistance characteristics and capacity characteristics, with reasonable expectation of success.
8. Claim 8 is rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia, in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1), as applied to claim 1, further in view of Watarai (JP 2004303613 A, see machine translation for citation).
Regarding claim 8, modified Soichiro discloses all of the limitations as set forth above. While modified Soichiro renders obvious the crystalline carbon fibers are carbon nanotubes that have few defects and low electronically resistance (Azami [0060]) as set forth above; and further discloses an attempt to increase conductivity by adding small amount of carbon nanotubes and carbon nanofibers to increase electrochemical reaction efficiency (Soichiro [0011]), modified Soichiro does not explicitly disclose that the carbon nanotubes measured by XRD provides an interplanar spacing d002 of the (002) plane is about 0.3354 nm to about 0.3365 nm.
Watarai teaches a negative electrode material that enables high rate charging and discharging, and a lithium ion secondary battery using the negative electrode ([0007]) with carbon nanotube (CNT) or carbon nanofibers (CNF) or both as main components ([0008]) which have high electrical conductivity because the stacking spacing d<sub>002</sub> of the graphite network plane of the tube body 11 or fiber body 21 is 0.3356 nm to 0.3450 nm, while the surface of the tube body 11 or fiber body 21 is covered with an amorphous carbon layer so that the surface activity is low and the material is chemically stable ([0008]). The d002 stacking spacing of 0.3356 nm to 0.3450 nm taught by Watarai encompasses the claimed range of about 0.3354 nm to about 0.3365 nm.
It would have been obvious for a skilled artisan, before the effective filing date of the claimed invention, to select carbon nanotube (CNT) as taught by Watarai, and arrive at the overlapping portion with the claimed range of the d002 stacking spacing, without undue experimentation and with a reasonable expectation of success that the selection would make the negative electrode have high electrical conductivity and enable high rate charging and discharging for a lithium ion secondary battery using the negative electrode.
9. Claims 14-15 and 18 are rejected under 35 U.S.C. 103 as being unpatentable over Soichiro (KR 20180117583, see machine translation for citation), as evidenced by Wikipedia (https://en.wikipedia.org/w/index.php?title=Carbon_nanofiber&oldid=1263732966, accessed December 30, 2024), in view of Yu (CN 114512654 A, see machine translation for citation), and further in view of Azami (US 20170309948 A1), as applied to claim 1 or claim 17, respectively, further in view of Green (US 20170133669 A1).
Regarding claim 14, modified Soichiro discloses all of the limitations as set forth above. While Soichiro further discloses the concern of volume expansion of about four times, resulting in a decrease in battery performance ([0005]), the desire that electronic conductivity of the secondary battery negative electrode can be improved by adding the conductive composition, and thus the performance of the battery can be improved ([0028]), and the primary particle has the long diameter (a) > short diameter (b) > thickness (d), and the long diameter may be 50 to 300 nm, the minor diameter may be 30 to 200 nm, and the thickness may be 10 to 50 nm ([0037]), Soichiro does not explicitly disclose an internal pore diameter of the negative electrode active material composite is about 5 nm to about 50 nm.
Green teaches a similar need for a silicon based electroactive material that is at least able to accommodate one or more of the stresses arising from the expansion and contraction of the material during the charging and discharging phases of the battery and which also has an improved capacity performance, a longer cycle life and a more cost-efficient method of manufacture ([0024]), and a composition comprising a plurality of elongated elements and a plurality of particles ([0025]), the inclusion of the elongated elements of high aspect ratio significantly increases the potential number of connection points between elements in the mix, whilst the inclusion of structurally simpler particles can reduce the overall manufacturing cost per unit mass. The inclusion of particles also increases the mass of silicon present in the electrode structure, thereby increasing the capacity of an electrode comparing this mixture relative to that of an electrode comprising elongated elements only. It is believed that the formation of an extended network of elongated elements and particles over the surface of the current collector improves both the connectivity within an electrode structure compared to known electrodes and the cycle life. In a preferred embodiment, the composition may optionally include, in addition to the silicon elements,…, a conductive material and non-silicon comprising electroactive material, such as graphite ([0032]).
Green further teaches compositions in which either the elongated elements partially fill the voids between particles or which comprise a network in which islands of particles are distributed within a matrix of elongated elements results in the formation of anodes, which exhibit better cycle-ability compared to an anode comprising silicon comprising particles only because it is better able to accommodate the stresses arising from the intercalation of lithium, whilst maintaining a good connectivity between all of the elements in the mix compared to an anode mix comprising silicon comprising particles only. The partial filling of the pores or voids in the electrode structure means that it also exhibits good capacity characteristics, higher than that attained with anode mixes comprising only elongated elements with a limit on the maximum achievable packing density, therefore able to exhibit good capacity characteristics over a prolonged period of time ([0044]).
A skilled artisan would have found it obvious before the effective filing date of the claimed invention, to control an internal pore diameter of the negative electrode active material composite to make sure the pores or voids being capable of partially filled in the electrode structure, as taught by Green, in order to be able to accommodate the stresses arising from the intercalation of lithium, while maintaining a good connectivity between all of the elements in the mix and therefore able to exhibit good capacity characteristics over a prolonged period of time. Further, in light of the primary particle has the long diameter (a) > short diameter (b) > thickness (d), and the thickness may be 10 to 50 nm ([0037]), a skilled artisan would have found it obvious to maintain an internal pore diameter a little smaller than the size of the thickness of the primary particle, 10 to 50 nm, to achieve partially filled pores or voids in the electrode structure, thus reasonably arrive at a value within the claimed “an internal pore diameter of the negative electrode active material composite is about 5 nm to about 50 nm” in order to achieve both good capacity characteristics and good capacity characteristics over a prolonged period of time.
It would have been obvious for one of ordinary skill in the art before the effective filing date of the claimed invention to adjust and maintain an internal pore diameter of the negative electrode active material composite within the claimed range of about 5 nm to about 50 nm, as taught by Green, in order to achieve both good capacity characteristics and good capacity characteristics over a prolonged period of time.
Regarding claim 15, modified Soichiro discloses all of the limitations as set forth above. While Soichiro further discloses the desire that electronic conductivity of the secondary battery negative electrode can be improved by adding the conductive composition, and thus the performance of the battery can be improved [0028] and the concern of volume expansion of about four times, resulting in a decrease in battery performance ([0005]), Soichiro does not explicitly disclose a BET specific surface area of the negative electrode active material composite is about 0.1 m2/g to about 5 m2/g.
Green teaches a similar need for a silicon based electroactive material that is at least able to accommodate one or more of the stresses arising from the expansion and contraction of the material during the charging and discharging phases of the battery and which also has an improved capacity performance, a longer cycle life and a more cost-efficient method of manufacture ([0024]), and a composition comprising a plurality of elongated elements and a plurality of particles ([0025]), the inclusion of the elongated elements of high aspect ratio significantly increases the potential number of connection points between elements in the mix, whilst the inclusion of structurally simpler particles can reduce the overall manufacturing cost per unit mass. The inclusion of particles also increases the mass of silicon present in the electrode structure, thereby increasing the capacity of an electrode comparing this mixture relative to that of an electrode comprising elongated elements only. It is believed that the formation of an extended network of elongated elements and particles over the surface of the current collector improves both the connectivity within an electrode structure compared to known electrodes and the cycle life. In a preferred embodiment, the composition may optionally include, in addition to the silicon elements,…, a conductive material and non-silicon comprising electroactive material, such as graphite ([0032]).
Green further teaches the inherent porosity (pores and voids) is important as it provides the silicon fibers with space into which they can expand in response to the intercalation or insertion of lithium that occurs during the charging cycle of the battery; and also provides a path by which the lithium can be intercalated into the bulk of the silicon material so that the lithiation of the silicon is as uniform as possible throughout the anode mass. However, the presence of an excessive number of pores within the anode structure means that the mass of anode active material per unit area is generally low compared to bulk silicon anodes or anode materials prepared using more closely packed particulate silicon, for example. This means that the inherent capacity of the anode is also correspondingly less ([0023]). Green further teaches the electrode materials can be characterized in relation to their density and their porosity. The electrode materials typically have density in the range 0.3 to 0.9 g/cm2, preferably 0.4 to 0.8 g/cm2; and a porosity in the range 65 to 95%, preferably 65 to 85% ([0072]). Green further teaches a BET value of around 5 m2/g for Example 1b ([0091]), which falls within the claimed range of 0.1 m2/g to about 5 m2/g for a BET specific surface area of the negative electrode active material composite.
A skilled artisan would have found it obvious before the effective filing date of the claimed invention, to control and optimize the porosity of the negative electrode active material composite of Soichiro, as taught by Green, in order to balance the expansion during charging cycles, efficiency of lithiation of silicon, and the inherent capacity of the negative electrode active material composite, and thus arrive at a range within the claimed range “a BET specific surface area of the negative electrode active material composite is about 0.1 m2/g to about 5 m2/g” without undue experimentation and with a reasonable expectation of success.
Regarding claim 18, modified Soichiro discloses all of the limitations as set forth above. While Soichiro further discloses and the concern of volume expansion of about four times, resulting in a decrease in battery performance ([0005]) and the desire that electronic conductivity of the secondary battery negative electrode can be improved by adding the conductive composition, and thus the performance of the battery can be improved [0028], Soichiro does not explicitly disclose if a rechargeable lithium battery including the negative electrode is subjected to 100 cycles as one cycle of charging with a constant current to 4.2 V at a rate of 0.5C and discharging with a constant current to 2.5 V at a rate of 0.5C, the negative electrode has a thickness expansion rate of according to Equation 1 of less than or equal to about 20%, and
[Equation 1]
Negative electrode thickness expansion rate [%] = [negative electrode thickness after 100 cycles / negative electrode thickness at first cycle] x 100.
Green teaches a similar need for a silicon based electroactive material that is at least able to accommodate one or more of the stresses arising from the expansion and contraction of the material during the charging and discharging phases of the battery and which also has an improved capacity performance, a longer cycle life and a more cost-efficient method of manufacture ([0024]), and a composition comprising a plurality of elongated elements and a plurality of particles ([0025]), the inclusion of the elongated elements of high aspect ratio significantly increases the potential number of connection points between elements in the mix, whilst the inclusion of structurally simpler particles can reduce the overall manufacturing cost per unit mass. The inclusion of particles also increases the mass of silicon present in the electrode structure, thereby increasing the capacity of an electrode comparing this mixture relative to that of an electrode comprising elongated elements only. It is believed that the formation of an extended network of elongated elements and particles over the surface of the current collector improves both the connectivity within an electrode structure compared to known electrodes and the cycle life. In a preferred embodiment, the composition may optionally include, in addition to the silicon elements,…, a conductive material and non-silicon comprising electroactive material, such as graphite ([0032]).
Green further teaches batteries prepared using these compositions and charged and discharged under constant current conditions exhibit a capacity retention of 1200 mAh/g over more than 150 cycles ([0060]) or over more than 300 cycles ([0061]). A skilled artisan would reasonably acknowledge that the good cycling capacity retention performance over more than 150 or more than 300 cycles means that Green’s composition has solved the problem of stresses arising from the expansion and contraction of the material during the charging and discharging phases of the battery, which inherently teaches the silicon-based electroactive material of Green necessarily possesses the property for the negative electrode with a thickness expansion rate of less than or equal to about 20% under the same testing condition as claimed, absent evidence of secondary consideration.
It would have been obvious for a skilled artisan before the effective filing date of the claimed invention, to optimize the ratio of fibers and native particles of the composition and control of particle sizes of fibers and native particles of modified Soichiro, as taught by Green, and therefore inherently possesses the cycling property as claimed “if a rechargeable lithium battery including the negative electrode is subjected to 100 cycles as one cycle of charging with a constant current to 4.2 V at a rate of 0.5C and discharging with a constant current to 2.5 V at a rate of 0.5C, the negative electrode has a thickness expansion rate of according to Equation 1 of less than or equal to about 20%, and [Equation 1]
Negative electrode thickness expansion rate [%] = [negative electrode thickness after 100 cycles / negative electrode thickness at first cycle] x 100.”, in order to balance the expansion during charging cycles, efficiency of lithiation of silicon, and the inherent capacity of the negative electrode active material composite with a reasonable expectation of success.
Response to Arguments
10. Applicant’s arguments regarding the amended claim 1 filed on 2/2/2026 have been fully considered but are not found persuasive.
The Applicant argues that the cited references fail to teach or suggest a negative electrode active material composite that corresponds to the negative electrode active material composite presently recited in Ln10-15 of claim 1, in particular, referring to the limitations “wherein… in a weight ratio of greater than or equal to 4” and “wherein is about 35 times to about 300 times …of the silicon nanoparticles.” (Remarks P9-12).
First, Applicant argues Soichiro does not teach or suggest a negative electrode active material composite having the weight ratio of silicon nanoparticles and crystalline carbon fiber of greater than or equal to about 4.
Examiner respectfully submits that while Soichiro discloses Example M2 which has a calculated weight ratio of 2.15, being out of the claimed range of greater than or equal to about 4, Soichiro seems not setting an upper limit of the weight ratio with Example M2 as a convenient example for describing the method of making the negative electrode composite. Since Soichiro further discloses higher SiOx abundance would achieve a better battery capacity in view of the comparison of Reference Example 2 Vs. Reference Example M1 ([0133] and Table 1), a skilled artisan would reasonably being motivated to increase the weight ratio of the silicon particles in order to obtain a higher capacity, therefore, with a reasonable expectation under routine experimentation to arrive at a weight ratio value of silicon nanoparticles and crystalline carbon fiber that falls within the claimed range with expected successful results in terms of capacity improvements, absent evidence to the contrary.
Further, according to the instant disclosure [0014-0015] and [0066-0067], the weight ratio (silicon nanoparticles : crystalline carbon fibers) of greater than or equal to about 2, great than or equal to about 4, or greater than or equal to about 9 would not have drastic effects by increasing the weight ratio to 4 or 9, because [0066-0067] provides “within the above range, a capacity improvement effect of the rechargeable lithium battery by the silicon nanoparticles and the rate capability and cycle-life securing effect of the rechargeable lithium battery by the crystalline carbon fibers may be harmonized”.
Therefore, this argument is not found persuasive due to lacking criticality of the claimed weight ratio of silicon nanoparticles and crystalline carbon fiber. Similar rationale and rejection apply to the new claim 21.
Second, Applicant argues that the cited references fail to teach or suggest a negative active material composite wherein an average particle diameter (D50) of the negative electrode active material composite is about 35 times to about 300 times an average particle diameter (D50) of the silicon nanoparticles.
Examiner respectfully submits that Soichiro discloses the average particle diameter of silicon powder observed with a scanning electron microscope was 50 to 200 nm ([0111]); and silicon-carbon composite 110 may have an average particle diameter of 5 to 20 µm ([0046]), which is calculated to teach a D50 of the negative electrode active material composite is about 25 times to about 400 times that of the silicon nanoparticles, encompassing the claimed range of about 35 times to about 300 times. It would have been obvious to a skilled artisan simply by adjusting particle size of silicon-powder and the silicon composite within respectively taught ranges under routine experimentation, and have a reasonable expectation of success in obtaining a negative electrode active material composite which has a D50 value falling within the claimed range of about 35 times to about 300 times of the D50 of the silicon nanoparticle powder.
Further, Soichiro includes silicon-carbon composite 110 as a “giant matrix” that captures and encapsulates numerous silicon nanoparticles 111 and carbon fibers 113 (FIG. 2), which is not as Applicant argued, quote “a mere “particle coating” on silicon (as suggested by Soichiro reference)”. Examiner notes this in response to Applicant’s second paragraph statement on P11 of Remarks.
Thus, this argument is not found persuasive.
Conclusion
11. Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any extension fee pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the date of this final action.
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/K. L./Examiner, Art Unit 1751
6/8/2026
/Haroon S. Sheikh/Primary Examiner, Art Unit 1751
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