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 .
Claim Rejections - 35 USC § 103
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
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.
Claim(s) 1-4, 6-11 & 14-16, 18 & 19 is/are rejected under 35 U.S.C. 103 as being unpatentable over Francisco (US20210296690).
Regarding Claim 1, Francisco discloses a sulfide-based solid electrolyte (sulfide solid electrolyte, [0022]) comprising Lithium (Li), boron (B), and a halogen element ([0022]),
Wherein the sulfide-based solid electrolyte comprises at least one crystalline phase ([008], [0018]),
Wherein the crystalline phased comprises a face-centered cubic (FCC) structure (the crystalline structure leads to the space grouping of F-43m, which is an FCC structure, [0082]).
Francisco does not directly disclose wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Francisco discloses wherein the solid electrolyte material comprising a crystalline argyrodite-type phase comprises 50% or more by mol of total phased present ([0019]), which overlaps the instant claim range of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Regarding Claim 2, Francisco discloses the limitations as set forth above.
Francisco discloses wherein the crystalline phased has a space group of F-43m (the crystalline structure leads to the space grouping of F-43m, [0082]).
Regarding Claim 10, Francisco discloses a method of manufacturing a sulfide-based solid electrolyte (sulfide solid electrolyte, [0022]) comprising:
Preparing a starting material comprising Li3PS4, LiBH4 and LiX1, wherein X1 comprises F, CL, BR, or I, ([0011-0014],[0022]).
Wherein the sulfide-based solid electrolyte comprises comprising Lithium (Li), boron (B), and a halogen element ([0022]), and comprises at least one crystalline phase ([008], [0018]),
Wherein the crystalline phased comprises a face-centered cubic (FCC) structure (the crystalline structure leads to the space grouping of F-43m, which is an FCC structure, [0082]).
Francisco does not directly disclose wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Francisco discloses wherein the solid electrolyte material comprising a crystalline argyrodite-type phase comprises 50% or more by mol of total phased present ([0019]), which overlaps the instant claim range of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Regarding Claim 3 & 15, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein the crystalline phase further comprises one or more selected from the group consisting of α-Li3PS4 phase, a β-Li3PS4 phase, and γ- Li3PS4 phase.
Francisco discloses wherein the crystalline phase comprises Li3PS4 compounds ([0029], [0034], Examples 1-10). Francisco discloses that the sulfide-solid electrolyte is measured using X-ray diffraction using a CuKα measurement ([009]). Francisco further discloses Example 1 of a sulfide solid electrolyte that has diffraction angles of 2ϴ = 15.5o ± 0.5o, 18.0o ± 0.5, 25.0 o ± 0.5o, 30.0 o ± 0.5o, 31.0 o ± 0.5o,39.5 o ± 0.5o (Fig. 3a, [0068]). Francisco further discloses wherein the sulfide solid electrolyte is formed mixing Li3PS4 and LiBH4 precursor phases ([0068]). Francisco further discloses wherein the crystalline structure leads to the space grouping of F-43m ([0082]). Francisco discloses wherein the method for producing the solid electrolyte material comprises mixing a raw lithium materials together to have a substantially amorphized or alloyed structure to create a final composition ([0023]). Francisco further discloses wherein sulfide solid electrolyte comprising Lithium (Li), boron (B), and a halogen element ([0022]).
The examiner notes that the instant application’s lithium phosphate sulfide crystalline particle is formed using ball-mill mixing of Li3PS4 and LiBH4 precursor phases, to form amorphized structure, with the diffraction angles when measured using X-ray diffraction of angles of 2ϴ = 15.5o ± 0.5o, 18.0o ± 0.5, 25.0 o ± 0.5o, 30.0 o ± 0.5o, 31.0 o ± 0.5o,39.5 o ± 0.5o.
Therefore, it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the crystalline phase further comprises one or more selected from the group consisting of α-Li3PS4 phase, a β-Li3PS4 phase, and γ- Li3PS4 phase.
Regarding Claim 4 & 16, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein the sulfide-based solid electrolyte further comprises an amorphous phase between crystalline phases.
Francisco discloses wherein the method for producing the solid electrolyte material comprises mixing a raw lithium materials together to have a substantially amorphized or alloyed structure to create a final composition ([0023]). Francisco further discloses wherein the crystalline structure can be semi-crystalline ([0034]).
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte further comprises an amorphous phase between crystalline phases.
Regarding Claim 6 & 18, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein the sulfide-based solid electrolyte shows diffraction peaks at diffraction angles of 2ϴ = 15.5o ± 0.5o, 18.0o ± 0.5, 25.0 o ± 0.5o, 30.0 o ± 0.5o, 31.0 o ± 0.5o,39.5 o ± 0.5o, 44.5 o ± 0.5o, 47.5 o ± 0.5o, 52.0 o ± 0.5o, and 54.5 o ± 0.5o in an XRD spectrum using CuKα rays.
Francisco discloses that the sulfide-solid electrolyte is measured using X-ray diffraction using a CuKα measurement ([009]). Francisco further discloses Example 1 of a sulfide solid electrolyte that has diffraction angles of 2ϴ = 15.5o ± 0.5o, 18.0o ± 0.5, 25.0 o ± 0.5o, 30.0 o ± 0.5o, 31.0 o ± 0.5o,39.5 o ± 0.5o (Fig. 3a, [0068]). Francisco further discloses wherein the sulfide solid electrolyte is formed mixing Li3PS4 and LiBH4 precursor phases ([0068]). Francisco further discloses wherein the crystalline structure leads to the space grouping of F-43m ([0082]). Francisco discloses wherein the method for producing the solid electrolyte material comprises mixing a raw lithium materials together to have a substantially amorphized or alloyed structure to create a final composition ([0023]). Francisco further discloses wherein sulfide solid electrolyte comprising Lithium (Li), boron (B), and a halogen element ([0022]). Francisco discloses wherein the composition is milled using a ball mill wherein the mixing time can be optimized to allow for appropriate homogenization and reaction of the precursor to generate the solid electrolyte ([0042]). Francisco further discloses wherein the appropriate mixing can be accomplished over 10 minutes to 40 hours ([0042]).
The examiner notes that the diffraction measurements disclose by Francisco, up to the 2ϴ=40 are the same as the instant claim, the sulfide electrolyte material is formed through mixing crystalline Li3PS4 and LiBH4, which is the same as the instant application and comprises boron and a halogen element, which is the same as the instant application. Furthermore, the method of forming the crystalline structure by mixing Li3PS4 and LiBH4 precursor phases and is formed through ball mill mixing to form a crystalline and amorphous structure, which is the same as the instant application.
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte shows diffraction peaks at diffraction angles of 2ϴ = 15.5o ± 0.5o, 18.0o ± 0.5, 25.0 o ± 0.5o, 30.0 o ± 0.5o, 31.0 o ± 0.5o,39.5 o ± 0.5o, 44.5 o ± 0.5o, 47.5 o ± 0.5o, 52.0 o ± 0.5o, and 54.5 o ± 0.5o in an XRD spectrum using CuKα rays.
Regarding Claim 7 & 18, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein sulfide-based solid electrolyte comprising a compound represented by Chemical Formula 1: (Li-3PS4)*a(LiBH4)*b(LiX), wherein X comprises F, Cl, Br or I, with 1 ≤ a ≤ 6 and 0 < b ≤ 4.
Francisco discloses wherein the sulfide solid electrolyte composition is formed to create Li3PS4LiBH4 ([0029]). Francisco further discloses wherein the solid electrolyte material comprises a formula LPSX.zLiX, where LPSX comprising a mixture of Li.sub.2S, P.sub.2S.sub.5 and LiX in a glass forming ratio or Li.sub.2S, B.sub.2S.sub.3 and LiX in a glass forming ratio, where LiX comprises one or more of LiCl, LiBr, LiI, LiBH.sub.4, LiBF.sub.4, LiNH.sub.2, and LiNO.sub.3, and 0<z≤25 ([0014]).
Therefore it is the examiner’s position that the formula of (Li-3PS4)*a(LiBH4)*b(LiX), wherein X comprises F, Cl, BR or I, with 1 ≤ a ≤ 6 and 0 < b ≤ 4 can be achieved by mixing the Li2S with B2S3 with LiX, where X can be Cl, Br, I and BH4 to form Formula 1.
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francis so to have wherein sulfide-based solid electrolyte comprising a compound represented by Chemical Formula 1: (Li-3PS4)*a(LiBH4)*b(LiX), wherein X comprises F, Cl, BR or I, with 1 ≤ a ≤ 6 and 0 < b ≤ 4.
Regarding Claim 8 & 19, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein sulfide-based solid electrolyte comprising a compound represented by Chemical Formula 1: (Li-3PS4)*a(LiBH4)*d(LiX1)*e(LiX2), wherein X1 and X2 comprise different halogen element, and each X1 and X2 independently comprises F, Cl, Br or I, with 1 ≤ c ≤ 6 and 0 < d ≤ 2 ,and 0 < e ≤ 2.
Francisco discloses wherein the sulfide solid electrolyte composition is formed to create Li3PS4LiBH4 ([0029]). Francisco further discloses wherein the solid electrolyte material comprises a formula LPSX.zLiX, where LPSX comprising a mixture of Li.sub.2S, P.sub.2S.sub.5 and LiX in a glass forming ratio or Li.sub.2S, B.sub.2S.sub.3 and LiX in a glass forming ratio, where LiX comprises one or more of LiCl, LiBr, LiI, LiBH.sub.4, LiBF.sub.4, LiNH.sub.2, and LiNO.sub.3, and 0<z≤25 ([0014]).
Therefore it is the examiner’s position that the formula of (Li-3PS4)*a(LiBH4)*d(LiX1)*e(LiX2), wherein X comprises F, Cl, BR or I, with 1 ≤ a ≤ 6 and 0 < b ≤ 4 can be achieved by mixing the Li2S with B2S3 with LiX, where X can be Cl, Br, I and BH4 to form Formula 2.
Therefore it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein sulfide-based solid electrolyte comprising a compound represented by Chemical Formula 1: (Li-3PS4)*a(LiBH4)*d(LiX1)*e(LiX2), wherein X1 and X2 comprise different halogen element, and each X1 and X2 independently comprises F, Cl, Br or I, with 1 ≤ c ≤ 6 and 0 < d ≤ 2 ,and 0 < e ≤ 2.
Regarding Claim 9, Francisco discloses the limitations as set forth above.
Francisco does not directly disclose wherein the sulfide-based solid electrolyte has lithium-ion conductivity of about 5 mS/cm or greater measured at a temperature of about 20 o C to 30 o C.
Francisco discloses wherein the conductivity of the solid electrolyte when measured at room temperature, can be 7.2, 8.2 or 6.6 5mS/cm (Fig. 6a, [0032]).
Therefore, it would be obvious to one using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte has a lithium-ion conductivity of about 5 mS/cm or greater measured at a temperature of about 20 o C to 30 o C.
Regarding Claim 11, Francisco discloses the limitations as set forth above.
Fancisco does not directly disclose wherein the starting material further comprises LiX2, wherein X2 comprises a halogen element different from X1, and X2 comprises F, Cl, Br, or I.
Francisco discloses wherein the sulfide solid electrolyte composition is formed to create Li3PS4LiBH4 ([0029]). Francisco further discloses wherein the solid electrolyte material comprises a formula LPSX.zLiX, where LPSX comprising a mixture of Li.sub.2S, P.sub.2S.sub.5 and LiX in a glass forming ratio or Li.sub.2S, B.sub.2S.sub.3 and LiX in a glass forming ratio, where LiX comprises one or more of LiCl, LiBr, LiI, LiBH.sub.4, LiBF.sub.4, LiNH.sub.2, and LiNO.sub.3, and 0<z≤25 ([0014]).
Therefore, it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the starting material further comprises LiX2, wherein X2 comprises a halogen element different from X1, and X2 comprises F, Cl, Br, or I.
Regarding Claim 14, Francisco discloses the limitations as set forth above.
Francisco discloses wherein the crystalline phased has a space group of F-43m (the crystalline structure leads to the space grouping of F-43m, [0082]).
Claim(s) 12 & 13 is/are rejected under 35 U.S.C. 103 as being unpatentable over Francisco (US20210296690) in view of Choi (US20220006116).
Regarding Claim 12, Francisco discloses the limitations as set forth above.
Francisco discloses wherein the composition is milled using a ball mill wherein the mixing time can be optimized to allow for appropriate homogenization and reaction of the precursor to generate the solid electrolyte ([0042]). Francisco further discloses wherein the appropriate mixing can be accomplished over 10 minutes to 40 hours ([0042]).
Francisco does not directly disclose wherein obtaining the sulfide-based solid electrolyte comprises subjecting the starting material to milling using a ball mill at about 500 rpm to 800 rpm for about 1 minute to 10 minutes and resting for about 1 minute to 5 minutes, or wherein repeating milling and resting about 10 to 20 times.
Choi discloses a method of forming a solid electrolyte ([002]). Choi further discloses wherein ball mill mixing is used, wherein a first-time interval and second time interval are used, where the first internal includes the ball-mixing and the second interval includes resting ([0143]). Choi further discloses wherein the first interval and second interval will have multiple cycle alternations ([0143]). Choi further discloses wherein the ball-mill mixing can be performed at 700 RPM ([0142]), which is within the instant claim range of 500 rpm to 800 rpm. Choi teaches that this alternation method provides a mixture of crystalline and amorphous phases ([0143]).
Therefore, it would be obvious to one of ordinary skill in the art to modify Francisco with the teachings of Choi to have wherein obtaining the sulfide-based solid electrolyte comprises subjecting the starting material to milling using a ball mill at about 500 rpm to 800 rpm for about 1 minute to 10 minutes and resting for about 1 minute to 5 minutes, or wherein repeating milling and resting about 10 to 20 times. This modification would yield the expected result of providing a mixture of crystalline and amorphous phases.
Response to Arguments
Applicant’s amendments, see Claims, filed June 26th, 2026, with respect to 35 USC 112(b) and 35 USC 102 have been fully considered and are persuasive. The 35 USC 112(b) rejection of Claims 11-20 has been withdrawn. The 35 USC 102 rejections of Claims 1, 2 & 10 have been withdrawn.
Applicant's arguments filed June 26th, 2026 have been fully considered but they are not persuasive.
Applicant argues that Francisco does not provide enough teaching to teach or suggest wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
The examiner notes that Francisco does not directly disclose wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Francisco discloses wherein the solid electrolyte material comprising a crystalline argyrodite-type phase comprises 50% or more by mol of total phased present ([0019]), which overlaps the instant claim range of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
The examiner further notes that the claim language only requires a sulfide based solid electrolyte that comprises at least one crystalline phase with an FCC structure. Therefore, it is the examiner’s position that the argyrodite-type phase crystalline material which has a face center cubic structure, meets the claim limitation the “crystalline phase”.
Therefore applicant’s arguments are not commensurate in scope with the claim language.
Therefore, it would be obvious to one of ordinary skill in the art using the disclosure of Francisco to have wherein the sulfide-based solid electrolyte comprises an amount of about 10 wt% to 90 wt% of the crystalline phase, based on the total weight of the sulfide-based solid electrolyte.
Conclusion
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 nonprovisional extension fee (37 CFR 1.17(a)) 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 mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to ANKITH R SRIPATHI whose telephone number is (571)272-2370. The examiner can normally be reached Monday - Friday: 7:30 am - 5:00pm.
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If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Matthew Martin can be reached at 571-270-7871. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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/ANKITH R SRIPATHI/Examiner, Art Unit 1728
/MATTHEW T MARTIN/Supervisory Patent Examiner, Art Unit 1728
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