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and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114.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 23 January 2026 has been entered.
Response to Amendment
Applicant amended claims 1, 9, and 16; claims 1-4, 6-12, 14-20, and 22-26 are pending and considered in the present Office action.
The 103 rejections are withdrawn in view of the amendments; However, upon further consideration a new ground of rejection is necessitated by amendment and new art.
Response to Arguments
Applicant argues Zhou teaches a suspension in the first solution and a suspension in the third solution, and Katori teaches suspension when the first solution is mixed with Li2S. Both of these arguments are unpersuasive.
Regarding Zhou, the first solution of Zhou (i.e., suspension comprising 3:1 Li2S:P2S5 in THF) has been modified; thus, the fact that the it is a suspension is moot. Further, the third solution, which applicant alleges is a suspension is not accurate. The ethanol solvent dissolves the white precipitates of the suspension (i.e., 3:1 Li2S:P2S5 in THF) in the third solution. Stirring overnight forms unreacted precipitates, but these unreacted precipitates are removed to obtain a clear solution; hence, the third solution is a homogenous solution.
Regarding Katori, the suspension formed in Katori through the addition of Li2S is not used in the modification of Zhou. Rather, the 3:1 suspension of Zhou is modified in view of, among other things, the solution making step suggested by Katori. Further, Katori’s disclosure that a molar ratio 3:1 (i.e., Li2S:P2S5 suspension) leads to by-products is motivation modify the ratio by routine experimentation to reach another workable range; Katori suggest another molar ratio (e.g., 1.0 to 1.85), with the understanding that the ratio leads to a homogeneous solution, which is desirable from the standpoint to enabling homogenous mixing, as suggested by ‘997 (see new rejection for more details).
The test for obviousness is not whether the features of a secondary reference may be bodily incorporated into the structure of the primary reference; nor is it that the claimed invention must be expressly suggested in any one or all of the references. Rather, the test is what the combined teachings of the references would have suggested to those of ordinary skill in the art. See In re Keller, 642 F.2d 413, 208 USPQ 871 (CCPA 1981). In this case, the prior art provides motivation to modify the first solution (i.e., the suspension of 3:1 Li2S:P2S5 in THF) of Zhou and provides motivation for each of the first solution, the second solution, and the third solution to be homogenous solution.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 1-4, 6-12, 14-20, and 22-26 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention. Claims 1, 9 and 16 each recited “comprising the steps of” in line 2 of the claim, which lacks antecedent basis. Examiner assumes “comprising steps of”.
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claim(s) 1-4, 7, 9-12, 14, 16-20, and 22 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zhou (Solvent-Engineered Design of Argyrodite Li6PS5X (X = Cl, Br, I) Solid Electrolytes with High Ionic Conductivity, of record) in view of Katroi (US 2020/0358130, of record) and Katori (US 2020/0020977), hereinafter Zhou, Katori, and ‘977.
Regarding Claims 1, 6, 9, 16, and 18, Zhou suggests a method for producing a sulfide solid electrolyte material (e.g., Li6PS5X, with X = Cl, Br, I) comprising steps of combining an alkali metal salt (e.g., Li2S) and a sulfide compound (e.g., P2S5) containing at least one of P, B, Al, As, Sb, Bi, Si, Ge, and Sn with a polar aprotic solvent (i.e., THF on page S2; further, DME and ACN are also suitable solvents for the same purpose (MPEP 2144.06 II., 2144.07, and 2123 II.), see left column on page 266, where ACN is the nitrogen baring polar aprotic solvent) to form a first solution, see “Experimental methods” on page S2. The molar ratio of Li2S:P2S5 in the first solution of Zhou is 3:1, which is a suspension; thus, Zhou does not suggest the first solution has a molar ratio of the alkali metal salt to the sulfide compound of between 9:11 and 11:9, or that the first solution is a homogeneous solution. However, ‘997 suggests mixing methods for forming solid electrolytes using a solvent; specifically, raw materials dissolved in the solvent are preferable and lead to homogeneous mixing, [0034-0035]. It would be obvious to one having ordinary skill in the art the first solution of Zhou is a homogeneous solution provided there is an expectation of homogeneous mixing. Further, Katori suggests Li2S:P2S5 in a molar ratio of 3:1 generates by-products at the time of suspending and mixing, [0007], and a molar ratio for Li2S:P2S5 between 1.0 to 1.85 yields a homogeneous solution ([0027]), and the solution is made at room temperature, [0028]. Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. "[W]here the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation." In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955). See also, In re Hoeschele, 406 F.2d 1403, 160 USPQ 809 (CCPA 1969), where claimed elastomeric polyurethanes which fell within the broad scope of the references were held to be unpatentable thereover because, among other reasons, there was no evidence of the criticality of the claimed ranges of molecular weight or molar proportions. See MPEP 2144.05, II. One having ordinary skill in the art would be motivated to modify the molar ratio of Zhou by routine experimentation to discover another workable range given the expectation that the 3:1 ratio in Zhou is expected to generate by-products (as suggested by Katori at [0007]); further, it would be obvious to one having ordinary skill in the art modify the molar ratio of Li2S:P2S5 from 9:11 to 11:9 to form a homogeneous solution (suggested by Katori at [0027]), thereby enabling subsequent homogeneous mixing (as suggested by ‘997 at [0034]). Additionally, it would be obvious to one having ordinary skill in the art the molar ratio of Li2S:P2S5 is 9:11 to 11:9 provided the homogenous solution forms at room temperature (as suggested by Katori at [0027]), which is a scalable synthetic route and practically preferred for solid state batteries compared to conventional higher energy routes like ball milling, which are difficult to scale up hence impractical for solid state batteries (as suggested by Zhou in the abstract and right column on page 265 to the left column on page 266). The molar ratio in the prior art, i.e., 1.0 to 1.85, overlaps with that claimed, i.e., 0.88 (9:11) to 1.22 (11:9); hence, a prima facie case of obviousness exists, see MPEP 2144.05, I.
Zhou suggests combining an alkali metal salt (e.g., Li2S, LiX) and a polar protonated solvent (e.g., ethanol) to form a second solution, wherein the second solution is a homogeneous solution, see e.g., page S2; and combining the first solution (suspension) and second solution (i.e., Li2S/LiX in ethanol) to form a third solution. It is noted that the white precipitates of the first solution suspension are dissolved in the Li2S/LiX ethanol solution, and any unreacted precipitates are removed to obtain a clear solution, thereby suggesting the third solution is a homogeneous solution. Further, the first solution suspension of Zhou was modified with Katori and ‘997, which suggests the first solution is a homogeneous solution; thus, upon mixing the homogeneous first solution with the homogenous second solution, a homogeneous third solution is expected, and/or any unreacted precipitates may be removed to obtain a clear solution, as was done in Zhou at S2, thereby suggesting a homogenous third solution.
Finally, Zhou suggests drying the third solution to produce a sulfide solid electrolyte material and further heating the sulfide solid electrolyte to a temperature higher than a drying temperature (i.e., clear solution is dried under vacuum at 140 °C to remove the solvents to yield a pale yellow powder which was further dried a temperature higher than the drying temperature (i.e., 550 °C is higher than 140 °C). Considering the temperature suggested by Zhou (i.e., 550 °C) is the same as that used in the instant disclosure (e.g., powders of instant Examples 3-5 were heated to 550 °C) the claimed increase in ionic conductivity of the sulfide solid electrolyte material is expected.
Regarding Claims 2-3, 10-11, 17, and 19, Zhou suggests an alkali metal halide (e.g., LiX) with the alkali metal salt selected from the group consisting Li2S and the polar protonated solvent (i.e., ethanol), see rejection of claim 1 and S2 of Zhou.
Regarding Claims 4, 12, and 20, Zhou does not disclose the particle size of the alkali metal salt (i.e., Li2S). However, Katori suggests a smaller particle size is better because the reaction rate becomes higher; specifically, Li2S preferably has a particle diameter between 10 nm to 30 µm, and more preferably 100 nm to 10 µm, [0029]. It would be obvious to one having ordinary skill in the art the particle size of Li2S is 20 µm or less with the expectation of achieving high reaction rate. The particle size in the prior art overlaps with that claimed; hence, a prima facie case of obviousness exists, see MPEP 2144.05, I.
Regarding Claims 7, 14, and 22, Zhou suggests the sulfide solid electrolyte material comprises a lithium argyrodite phase, see e.g., abstract and page 266.
Claim(s) 8, 15, and 23 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zhou, Katori, and ‘997 (cited above), in view of Kiyono (JP 2016-134316, of record), hereinafter Kiyono.
Regarding Claims 8, 15 and 23, the first solution of Zhou was modified in view of Katori and ‘977, which suggests stirring to form the homogenous solution is performed from 0.1 to 24 hours so that the reaction is complete and a solution is made, see e.g., [0037] of Katori. It would be obvious to one having ordinary skill in the art the first solution comprises stirring for 15 minutes to 12 hours with the expectation of completing the reaction, and to form a homogenous solution, which further enables subsequent homogenous mixing.
Zhou does not suggest the stirring time of the second solution (i.e., L2S/LiX in ethanol); while Zhou suggests the third solution is stirred overnight, an explicit suggestion of time is not disclosed. However, Katori suggests reaction time in solution making varies depending on the type of solvent, particle diameter and concentration of the raw materials; performing a reaction from 0.1 to 24 hours ensures a complete reaction, [0037]. Further, ‘997 states mixing time is sufficient when a homogenous mixture is ensured, typically 0.1 to 24 hours, see e.g., [0038]. Kiyono teaches stirring raw materials with solvent from 10 minutes to 100 hours or less to achieve sufficient contact time, 6-9/39. It would be obvious to one having ordinary skill in the art stirring in the second solution and the third solution is adjusted between 15 minutes to 12 hours with the expectation of ensuring sufficient contact time, and ensuring a homogenous mixture. Moreover, Kiyono suggests the contact time of the raw material and solvent is a result effective variable for reaction progression, see pages 6-9/39, i.e., amount of unreacted raw materials is dependent on contact time. It would be obvious to one having ordinary skill in the art to select a stirring time between 15 minutes to 12 hours with the expectation of achieving sufficient reaction time due to sufficient contact between the raw materials, as suggested by Kiyono. The presence of a known result-effective variable would be motivation for a person of ordinary skill in the art to experiment to reach another workable product or process. See MPEP2144.05, I. and II.
Claim(s) 24-26 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zhou, Katori, and ‘997, in view of Senga et al. (US 2019/0074544, of record), hereinafter Senga.
Regarding Claims 24-26, Zhou does not teach or suggest the drying step proceeds through spray drying. However, Senga reports on various ways to evaporate a solvent to finally form a solid electrolyte; spray drying allows for solvent removal and microparticulation to average particle diameters suitable as battery materials in a single step, leading to higher productivity compared to conventional methods, see e.g., [0022, 0054-0057, 0061, 0107] Fig. 2, Example 5. It would be obvious to one having ordinary skill in the art to utilize spray drying with the expectation of evaporating the solvent, and microparticulating the solid electrolyte to particle sizes suitable for battery materials in a single step, leading to higher productivity compared to conventional methods, as suggested by Senga.
Conclusion
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/ANNA KOROVINA/Examiner, Art Unit 1729
/ULA C RUDDOCK/Supervisory Patent Examiner, Art Unit 1729