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 .
Examiner’s Comments
The examiner has cited particular columns and line numbers, paragraphs, or figures in the references as applied to the claims for the convenience of the applicant. Although the specified citations are representative of the teachings in the art and are applied to the specific limitations within the individual claim, other passages and figures may apply as well. It is respectfully requested from the applicant, in preparing the responses, to fully consider the references in entirety as potentially teaching all or part of the claimed invention, as well as the context of the passage as taught by the prior art or disclosed by the examiner.
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 1-11 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 1-11 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being incomplete for omitting essential steps, such omission amounting to a gap between the steps. See MPEP § 2172.01.
Claim 1 recites a method of making a sulfide solid electrolyte, wherein the last process is a stage where it is in a liquid-phase state (emphasis added). The omitted steps are: claim 10.
Alternatively, the now amended claims requires to be in a liquid-phase state, however, the preamble is directed to a solid state. It is unclear to the examiner how can a liquid-phase state also can be a solid. Clarification is needed. For the purpose of this examination, the examiner is taking the position that claim 1 is an intermediate final-step process.
Claim Rejections - 35 USC § 102
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
Claims 1, 4, and 10 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Aotani et al. (JP 06-115911).
Regarding claim 1, Aotani discloses a manufacturing method of a sulfide solid electrolyte (Abstract) comprising heat-treating a starting material comprising a lithium element, a sulfur element, and a phosphorous element to obtain an intermediate [0013, 0018-0021], heating and melting the intermediate in an atmosphere of a sulfur gas comprising a sulfur element to introduce sulfur into the intermediate which has been melted and is in a liquid-phase state ([0006], [0013-0016]: molten would inherently be in a liquid-phase state).
Regarding claim 4, please see [0019].
Regarding claim 10, please see [0022].
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.
Claims 3 and 5 are rejected under 35 U.S.C. 103 as being unpatentable over Aotani et al. (JP 06-115911).
Regarding claim 3, please see [0013-0016], wherein excess sulfur is present. Thereby, it would have been obvious to one of ordinary skill in the art to use trace amount of gas derived from the first heat-treatment to also be used in the second heat-treatment absent of evidence the criticality of the amount of the gas that vaporizes. It is known in the art that hydrogen sulfide gas is a toxic material, thereby one of ordinary skill in the art would recognize to use all the necessary toxic gas in the formation of the sulfide solid electrolyte.
Regarding claim 5, given that Aotani discloses similar method as claimed and Li2S and P2S5, it would have been obvious to one of ordinary skill in the art to optimize the reaction to produce Li4P2S6 or Li3PS4, with reasonable expectation of success and undue experimentation, especially given that these are known electrolyte materials.
Claims 2 and 5-8 are rejected under 35 U.S.C. 103 as being unpatentable over Aotani et al. (JP 06-115911) in view of Takahashi et al. (WO 2020/095937) provided in the IDS. The Examiner notes that US 2022/0006117 is the English language equivalent of WO 2020/095937 and all citations will refer to US 2022/0006117.
Regarding claims 2 and 5-8, Aotani discloses the method of making a sulfide solid electrode as set forth above, however, fails to explicitly disclose heat treatment temperature of the starting material as claimed, Li3PS4 in the intermediate, and the starting material comprising LiCl, LiBr, and LiI, and the sulfide electrolyte is an argyrodite crystal.
Takahashi disclose a method of making a sulfide solid electrolyte comprising the heat treatment of the starting material is conducted within the claimed range [0095-0101], Li3PS4 in the intermediate [0115], starting material comprising halogen elements and LiCl, LiBr, and LiI [0093], and an argyrodite crystal structure ([0047-0050], [0115-0117] and [0158]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify Aotani’s method to have the heat treatment temperature as claimed and to incorporate the materials and structure as claimed, since Takahashi discloses that this is known in the art to suppress generation of hydrogen sulfide gas, which is known to be toxic [0018].
Claims 9-12 are rejected under 35 U.S.C. 103 as being unpatentable over Aotani et al. (JP 06-115911) in view of Sasaki (US 2018/0366777).
Regarding claims 9-12, Aotani discloses rapidly cooling a melt as claimed [0022], however, Aotani is silent that it is conducted by rapid cooling of 10ºC/sec or higher of a melt, wherein the melt comprises 0.01-1 mass% of crystal nucleus. Aotani also fails to disclose a post-annealing treatment of the solid.
Sasaki discloses a sulfide solid electrolyte material and a method thereof disclosing that appropriate heating temperature and quenching speeds gives sulfide solid electrode material with a desired crystallinity [0038]. Further, Sasaki discloses that post-heating of a solid is optional in order to obtain a suitable crystallinity. Thereby, quenching speeds and post heat treatment of a solid is a result effective variable in order to achieve a desirable crystal structure.
A person having ordinary skill in the art before the effective filling date of the invention would have arrived at the claimed invention by routine experimentation alone, without exercising undue experimentation.
Additionally, a person having ordinary skill in the art has good reason to pursue known option within his or her technical grasp. It would have been obvious to one or ordinary skill in the art before the effective filing date of the claimed invention was made to optimize the rapid cooling stage and the starting crystal seed and post-heat treatment of a solid, since it has been held that, where the general conditions of a claim are disclosed in the prior art, it is not invention to discover optimum or workable ranges by routine experimentation. In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955). The burden is upon the Applicant to demonstrate that the claimed amount is critical and has unexpected results. In the present invention, one would have been motivated to optimize the rapid cooling a melt of 10ºC/sec or more with a crystal nucleus of 0.01-1 mass% or less as a starting point and additional post heat-treatment, in order to obtained a desired crystallinity of the sulfide solid electrolyte.
Claims 1-12 are rejected under 35 U.S.C. 103 as being unpatentable over Nagakane et al. (JP 2012-043654) in view of Chiga et al. (JP 2019-169459).
Regarding claim 1, Nagakane discloses a manufacturing method of a sulfide solid electrolyte (Abstract) comprising heat-treating a starting material comprising a lithium element, a sulfur element, and a phosphorous element to obtain an intermediate ([0023-0024], [0044]), heating and melting the intermediate in an atmosphere of a gas into the intermediate which as been melted and is in a liquid-phase state ([0032-0037, 0045]: molten would inherently be in a liquid-phase state). Although Nagakane discloses that the atmosphere is in inert gas ([0033]: Ni or Ar), Nagakane fails to explicitly disclose that is it in an atmosphere in a sulfur element as presently claim.
Chiga discloses a manufacturing method of a sulfide solid electrolyte comprising a step of heating an electrolyte liquid using nitrogen, gas, or hydrogen sulfide, therefore Chiga establishes that sulfur shows that Chiga is an equivalent structure known in the art [0029]. Therefore, because these two materials were art-recognized equivalents at the time the invention was made, one of ordinary skill in the art would have found it obvious to substitute N or Ar gas for sulfur gas in the invention of Nagakane. Substitution of equivalents requires no express motivation as long as the prior art recognizes the equivalency. In re Fount 213 USPQ 532 (CCPA 1982); In re Siebentritt 152 USPQ 618 (CCPA 1967); Grover Tank & Mfg. Co. Inc V. Linde Air Products Co. 85 USPQ 328 (USSC 1950). Additionally, it would have been obvious to one or ordinary skill in the art before the effective filing date of the claimed invention to modify Nagakane’s inert gas to be sulfur gas, since Chiga discloses that this would prevent impurities [0029]. Therefore, in light of the sulfur gas atmosphere, it would have been obvious to one of ordinary skill in the art that at least trace elements of sulfur from the gas would be introduced into the intermediate.
Regarding claim 2, please see [0030].
Regarding claim 3, Nagakane in view of Chiga discloses heat-treating the starting material comprises of a sulfur element as set forth above, which would include trace amount of sulfur content as vaporizers. In light of Nagakane in view of Chiga disclosure of hydrogen sulfide gas in the heating treatment, it would have been obvious to one of ordinary skill in the art to use trace amount of gas derived from the first process to also be used in the second second process absent of evidence the criticality of the amount of the gas that vaporizes. It is known in the art that hydrogen sulfide gas is a toxic material, thereby one of ordinary skill in the art would recognize to use all the necessary toxic gas in the formation of the sulfide solid electrolyte.
Regarding claim 4, please see [0011-0012, 0024].
Regarding claim 5, please see [0026-0027, 0038].
Regarding claims 6-8, Nagakane fails to explicitly disclose the starting material comprising of halogen and the sulfide solid electrolyte is an argyrodite crystal structure as presently claimed.
Chiga discloses lithium chloride and the electrolyte is an argyrodite crystal structure (Abstract, and [0025],[0048]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify Nagakane to have the materials and crystal structure as claimed, since Chiga discloses that this would lead to an increase ion conductivity [0027].
Regarding claims 9-11, Nagakane discloses cooling a melt obtained by the heating and melting in a rate of 1K/sec or more [0037], wherein the electrolyte has a crystalline phase and could be adjusted [0039].
Given that Nagakane discloses a sulfide solid electrolyte material and a method thereof disclosing that appropriate heating temperature gives sulfide solid electrode material with a desired crystallinity [0039], the crystal nucleus is a result effective variable.
A person having ordinary skill in the art before the effective filling date of the invention would have arrived at the claimed invention by routine experimentation alone, without exercising undue experimentation.
Additionally, a person having ordinary skill in the art has good reason to pursue known option within his or her technical grasp. It would have been obvious to one or ordinary skill in the art before the effective filing date of the claimed invention was made to optimize the starting crystal seed, since it has been held that, where the general conditions of a claim are disclosed in the prior art, it is not invention to discover optimum or workable ranges by routine experimentation. In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955). The burden is upon the Applicant to demonstrate that the claimed amount is critical and has unexpected results. In the present invention, one would have been motivated to optimize the rapid cooling a melt with a crystal nucleus of 0.01-1 mass% or less as a starting point in order to obtained a desired crystallinity of the sulfide solid electrolyte.
Regarding claim 12, Nagakane discloses post heat treatment [0046].
Response to Arguments
Applicant’s arguments with respect to claim(s) 1-12 have been considered but are moot because the new ground of rejection does not rely on any reference applied in the prior rejection of record for any teaching or matter specifically challenged in the argument. Applicant has amended the claims to now reflect that the intermediate is in a liquid-phase state or molten state.
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 LINDA N CHAU whose telephone number is (571)270-5835. The examiner can normally be reached 9AM-5PM EST M-F.
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If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Mark Ruthkosky can be reached at (571)272-1291. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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Linda Chau
/L.N.C/ Examiner, Art Unit 1785
/Holly Rickman/ Primary Examiner, Art Unit 1785
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