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 .
Priority
Receipt is acknowledged of certified copies of papers required by 37 CFR 1.55.
Information Disclosure Statement
The information disclosure statements (IDS) submitted on 03/11/2025 and 01/07/2026 are being considered 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 9 and 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.
Claim 9 recites the limitation "the fibrous carbon-based material" in line 4 of claim 9. It is unclear if this limitation is referring to “a fibrous carbon-based material” in line 3 of claim 9 or “a fibrous carbon-based material” in line 9 of claim 1. There is insufficient antecedent basis for this limitation in the claim. See MPEP 2173.05(e).
The examiner recommends that the limitation of “wherein the Li2S composite further comprises a carbon-based material, wherein the carbon-based material comprises a fibrous carbon-based material, wherein the fibrous carbon-based material comprises a carbon nanostructure, wherein the carbon nanostructure comprises carbon nanofibers, carbon nanotubes, carbon nanobelts, carbon nanorods, or a combination thereof,” be rewritten to “wherein the Li2S composite further comprises a carbon nanostructure, wherein the carbon nanostructure comprises carbon nanofibers, carbon nanotubes, carbon nanobelts, carbon nanorods, or a combination thereof,”.
Claim 11 recites the limitation "wherein the Li2S composite is a composite of Li2S, LiI, and a carbon-based material, a size of Li2S crystallites obtained from an XRD spectrum of the composite is less than about 9.9 nm, and the composite comprises a solid solution of Li2S and LiI.” in lines 1-5 of claim 11. It is unclear whether the “Li2S crystallites” being measure refer to Li2S crystallites, Li2S-LiI crystallites, or Li2S-LiI-carbon-based material crystallites.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or non-obviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 1,2, 4-9, 12-15, 17, and 18 are rejected under 35 U.S.C. 103 as being unpatentable over Liu et. al (CN 109509872, machine translation attached) and further in view of Pai et. al (US 20200313188).
Regarding claim 1, Liu teaches a positive electrode (cathode) with a positive electrode active material (cathode active material layer) [0007]. The cathode active material layer is coated on a side of an aluminum foil (cathode current collector) to make the cathode [0023]. Liu teaches that the cathode active material layer contains a positive electrode active material (cathode active material), a halogen inorganic salt, a conductive material, and a lithium-ion conductive material or sodium ion conductive material [0008]. The cathode active material may include lithium sulfide (Li2S), elemental sulfur, a carbon/sulfur complex, or a carbon/Li2S complex [0009], the halogen inorganic salt is AB1-3, where A may be Li and B = F, Cl, Br, I, or At [0010], the conductive material [0011], and the lithium-ion conductive material can include a polymer or sulfide type material (sulfide-based solid electrolyte) [0012]. The combination of Li2S or the carbon/Li2S complex with the halogen inorganic salt can correspond to the Li2S composite in the cathode active material. When the cathode active material is the carbon/sulfur complex, the preferred carbon material is carbon microspheres, graphene, carbon nanotubes, porous carbon, and graphitized carbon [0009, 0023]. When the cathode active material contains the carbon/sulfur complex and the carbon material is carbon nanotubes (fibrous carbon-based material), this combination corresponds to the sulfur-fibrous carbon-based material composite in the cathode active material layer. Liu does not explicitly teach that the sulfur-fibrous carbon-based material is together in the cathode active material layer with the Li2S or Li2S composite. Since Liu does teach that the cathode active material can be a carbon/sulfur complex and a carbon/lithium sulfide complex, it would have been obvious to one of ordinary skill in the art to combine the carbon/lithium sulfide complex with the carbon/sulfur complex to have an active material with a carbon-sulfur/lithium sulfide active material which corresponds to the claimed cathode active material layer comprising a cathode active material of Li2S and a sulfur-fibrous carbon-based material composite. Liu is silent on the crystal structure of the sulfur in the sulfur-fibrous carbon-based material composite.
Pai teaches a lithium-sulfur battery with a cathode and cathode current collector [0036, 0041]. Pai teaches that the cathode active material is made up of monoclinic gamma phase sulfur that is deposited on a substrate of carbon nanofibers which reads on the gamma sulfur-fibrous carbon-based material composite of claim 1 [0030, 0034, 0172]. Pai also teaches that there Li2S is present in the cathode active material as a product of the reduction of gamma sulfur during charge/discharge cycles [0126, 0130]. Since Li2S is a result of the reversible redox reaction of gamma sulfur it will necessarily be present in the cathode active material. When gamma phase sulfur is used in the cathode active material, a direct transition from gamma phase sulfur to lithium sulfide without the formation of undesirable polysulfides which result in decreased cycle life of the battery [0172].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the cathode active material taught by Liu with the teachings of Pai to use a monoclinic gamma phase sulfur on the fibrous carbon-based material to have a cathode active material layer with a cathode active material comprising Li2S and a gamma sulfur-fibrous carbon-based material composite. Including gamma phase sulfur deposited on carbon nanofibers as the cathode active material results in a cathode active material comprising Li2S. The motivation to use the gamma phase of sulfur is to have a sulfur phase that does not from polysulfides in side reactions that negatively impact the operation of the battery.
Regarding claim 2, Liu in view of Pai teaches all the limitations of claim 1 as described above. Liu also teaches that the positive electrode active material (cathode active material) is present in 40-90 parts by weight with respect to the positive electrode material (cathode active material layer) [0008]. Liu teaches that elemental sulfur has poor conductivity which results in low discharge specific capacity [0004]. Liu does not explicitly teach the weight percentage of the gamma sulfur-fibrous carbon-based material composite relative to the total cathode active material layer.
Pai teaches that both sulfur and Li2S have insulating properties which results in low material utilization [0003]. Pai teaches that the benefit of having carbon nanofibers (fibrous carbon-based material) deposited with gamma monoclinic phase sulfur, which corresponds to the claimed gamma sulfur-fibrous carbon-based material composite, is that conductive carbon channels are maintained for better electron pathways and excellent mechanical stability during cycling [0049]. Pai teaches a cathode containing the gamma sulfur deposited carbon nanofibers which retains is cycling capacity and displays complete utilization of the active material [0203]. The motivation to use a gamma sulfur-fibrous carbon-based material composite in a cathode active material layer it to have a cathode with high material utilization by using the carbon nanofibers to increase the conductivity of the insulating sulfur and Li2S in the active material.
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the cathode taught by Liu with the teaching of Pai to adjust the weight percent of the gamma sulfur-fibrous carbon-based material composite in the range of about 1 part by weight to about 30 parts by weight based on about 100 parts by weight of the cathode active material layer. The motivation to use this loading is to balance the loading of sulfur active material with the conductive fibrous carbon-based material for increasing utilization of the active material and ultimately improving battery function.
Regarding claim 4, Liu in view of Pai teaches all the limitations of claim 1 as described above. Since Liu teaches carbon nanotubes and/or carbon microspheres as the fibrous-carbon based material in the active material, the cross section of each these embodiments are a circle or a circular shape. It is well known in the art that a circular shaped cross section is a structural feature of a tube and sphere shape. Liu further teaches that the cathode active material which contains the gamma sulfur-fibrous carbon-based material composite can have a halogen inorganic salt added to it [0010]. This additive reads on the doping the gamma sulfur-fibrous carbon-based material composite with fluorine which is a halogen. Liu is silent on the specific surface area of the gamma sulfur-fibrous carbon-based material composite.
Pai teaches that with the deposition of sulfur onto the carbon nano fibers (fibrous carbon-based material) decreases the specific surface area (Brunauer-Emmett-Teller (BET) specific surface area) of the fibrous carbon-based material [0182]. After deposition the surface area of the fibrous carbon-based material is 31.78 m2/g [Table 1]. By decreasing the surface area with the addition of sulfur, more gamma sulfur is present in the active material which is desired for high battery performance [0130].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the cathode active material taught by Liu with the teachings of Pai to make the gamma sulfur-fibrous carbon-based material composite with a low specific surface area for the purpose of creating an electrode with high sulfur content to create a high energy density battery.
Regarding claim 5, Liu in view of Pai teaches all the limitations of claim 1 as described above. Pai further teaches what the X-ray diffraction (XRD) pattern of the gamma sulfur-fibrous carbon-based material composite is in Figure 9A [0074]. Figure 9 shows a first peak at diffraction angle (2θ) of 13° corresponding to the (111) crystal plane, a second peak at 25° corresponding to the (122) crystal plane, and a third peak at 28° corresponding to the (222) crystal plane.
Regarding claim 6, Liu in view of Pai teaches all the limitations of claim 1 as described above.
Liu teaches that the cathode active material layer contains a positive electrode active material (cathode active material), a halogen inorganic salt, a conductive material, and a lithium-ion conductive material or sodium ion conductive material [0008]. The cathode active material may include lithium sulfide (Li2S), elemental sulfur, a carbon/sulfur complex, or a carbon/Li2S complex [0009], the halogen inorganic salt is AB1-3, where A may be Li and B = F, Cl, Br, I, or At [0010], the conductive material (carbon-based material) can be carbon nanotubes or carbon nanofibers [0011], and the lithium-ion conductive material (solid electrolyte) can include a polymer or sulfide type material (sulfide-based solid electrolyte) [0012]. The combination of Li2S, halogen inorganic salt, conductive material, and lithium-ion or sodium-ion conductive material in the positive active material can correspond to the claimed composite of Li2S and a carbon-based material; composite of Li2S, a carbon-based material, and a solid electrolyte; composite of Li2S and a solid electrolyte; or composite of Li2S and a lithium salt.
Regarding claim 7, Liu in view of Pai teaches all the limitations of claim 6 as described above. Liu further teaches that the carbon-based material can be graphene, carbon nano fibers, or carbon nanotubes [0011].
Regarding claim 8, Liu in view of Pai teaches all the limitations of claim 1 as described above. Liu further teaches that the Li salt in the Li2S composite can be LiX where X is I, Br, Cl, F, or At [0010].
Regarding claim 9, Liu in view of Pai teaches all the limitations of claim 8 as described above. Liu further teaches that carbon nanofibers or carbon nanotubes are present in the cathode which are referred to as a conductive material [0011]. The conductive material (carbon-based material) is present in 0.01-20 parts by weight based on 100 parts by weight of the positive electrode material [0008]. The amount of carbon-based material is about 0.01 – 20 wt. % which overlaps the claimed range. In the case where the claimed ranges overlap or lie inside similar ranges disclosed by the prior art, a prima facie case of obviousness exists. See MPEP 2144.05(I).
Regarding claim 12, Liu in view of Pai teaches all the limitations of claim 1 as described above. Pai further teaches that the gamma sulfur-fibrous carbon-based material composite is formed by vapor deposition of gamma sulfur on carbon nano fibers [0020, 0028, 0030]. This monoclinic sulfur is stable at temperatures below 80 °C [0020].
The limitation “wherein the gamma sulfur-fibrous carbon-based material composite is a product formed by vapor deposition of gamma sulfur on carbon nanofibers” is a method limitation and does not determine the patentability of the product, unless the method produces a structural feature of the product. The method of forming the product is not germane to the issue of patentability of the product itself, unless Applicant presents evidence from which the Examiner could reasonably conclude that the claimed product differs in kind from those of the prior art. See MPEP 2113. Furthermore, there does not appear to be a nonobvious difference between the prior art structure and the structure resulting from the claimed method because the prior art by Pai discloses an identical method.
Regarding claim 13, Liu in view of Pai teaches all the limitations of claim 8 as described above. Liu teaches that the Li salt in cathode active material is LiI, LiBr, LiCl, or LiF, which is a binary compound [0010].
Regarding claim 14, Liu in view of Pai teaches all the limitations of claim 1 as described above. Liu further teaches a secondary lithium battery [0002, 0004]. The lithium battery has a cathode, negative electrode (anode), and solid electrolyte membrane (electrolyte layer) [0007]. The cathode, electrolyte layer, and anode are sequentially stacked which reads on the electrolyte layer being between the cathode and the anode [0044]. Liu describes the anode as a sheet made of metallic lithium, a lithium-containing alloy, metallic sodium, or a sodium-containing alloy which reads on the first anode active material [0044, 0021]. The presence of an anode active layer inherently requires an anode current collector on a side of the active material because there must be a current collector present to conduct ions from the anode active material.
Regarding claim 15, Liu in view of Pai teaches all the limitations of claim 14 as described above. Liu further teaches that the electrolyte comprises a solid electrolyte membrane (solid electrolyte) [0013]. The solid electrolyte membrane includes a lithium-ion or sodium-ion conductive material, where the lithium-ion or sodium-ion conductive material can comprise organic polymers and inorganic salts [0013, 0014]. The inorganic salts can include sulfide [0013]. Liu therefore teaches a solid electrolyte comprising a sulfide-based solid electrolyte, a polymer solid electrolyte, or a combination thereof.
Regarding claim 17, Liu in view of Pai teaches all the limitations of claim 14 as described above. Liu teaches that the first anode active material layer is in the form of a sheet which can be made of metallic lithium, a lithium-containing alloy, metallic sodium, or a sodium-containing alloy [0021, 0044]. This description reads on the first anode active material being a metal layer where the metal layer comprises lithium or a lithium alloy.
Regarding claim 18, Liu in view of Pai teaches all the limitations of claim 17 as described above. Since “the anode active material” is not positively recited in claim 18, all the limitations of claim 18 are satisfied by meeting the limitations of claim 17. Claim 17 requires that “the first anode active material layer is a metal layer” OR “the first anode active material layer comprises an anode active material and a binder”. The limitation of “the first anode active material layer is a metal layer” has been met in claim 17 as described above and the presence of “the anode active material” in claim 18 is not required.
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Liu et. al (CN 109509872, machine translation attached) and Pai et. al (US 20200313188) as applied to claim 1 above, and further in view of Yan et. al (US 20160172667).
Regarding claim 3, Liu in view of Pai teaches all the limitations of claim 1 as described above. Liu further teaches that the fibrous carbon-based material in the cathode is carbon nanotubes or carbon nanofibers [pg. 5]. Liu is silent on the specific length or diameter of the fibrous carbon-based material. Pai teaches that the fibrous carbon-based material has a diameter of 150 nm but is silent on the length of the fibrous carbon-based material [0181].
Yan teaches secondary lithium sulfur battery with a cathode active material that contains sulfur and carbon nanotubes (fibrous carbon-based material) [0006, 0007]. Yan teaches that the fibrous carbon-based material has a length of 5-9 µm, and a diameter of 110-170 nm [0075]. Given these dimensions the aspect ratio of the fibrous carbon-based material will be more than 2. In the case where the claimed ranges overlap or lie inside similar ranges disclosed by the prior art, a prima facie case of obviousness exists. See MPEP 2144.05(I). The motivation to use this high aspect ratio in the fibrous carbon-based material is to have a cathode with robust and abundant interconnected channels that will effectively transport Li ions [0065].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the cathode taught by Liu and Pan with the teaching of Yan by using a high aspect ratio fibrous carbon-based material for the purpose of improving the Li ion conductivity through the cathode.
Claims 10 and 11 are rejected under 35 U.S.C. 103 as being unpatentable over Liu et. al (CN 109509872, machine translation attached) and Pai et. al (US 20200313188) as applied to claim 1 above, and further in view of Cui (US 20110200883).
Regarding claims 10 and 11, Liu in view of Pai teaches all the limitations of claim 1 as described above. Liu teaches that the cathode comprises a cathode active material and a halogen salt [0008]. The cathode active material can be Li2S [0009], and the halogen salt can be a lithium-halogen salt [0010]. One embodiment of the lithium-halogen salt is LiI [0010]. Liu also teaches that the battery is an all-solid-state battery, therefore, the Li2S and lithium-halogen salt must be in a solid solution [0007]. Liu is silent on the particle size of the Li2S crystallites.
Cui teaches a lithium sulfide cathode for a rechargeable battery [0012]. The cathode is made with Li2S, and Cui teaches that the Li2S nanoparticles are contained withing the pores of the carbon structure which are between 2 and 50 nm [0041]. For the Li2S particles to be in the pores they must be less than 50 nm in size. The motivation to have Li2S particles of this size is to improve the conductivity of lithium through the cathode [0064].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the cathode taught by Liu and Pai with the teachings of Cui to have Li2S crystals less than about 20 nm and less than about 9.9 nm for the purpose of improving lithium conductivity.
Claims 16, 19, and 20 are rejected under 35 U.S.C. 103 as being unpatentable over Liu et. al (CN 109509872, machine translation attached) and Pai et. al (US 20200313188) as applied to claim 1 above, and further in view of Lee et. al (US 20220140312).
Regarding claim 16, Liu in view of Pai teaches all the limitations of claim 15 as described above. Liu does not explicitly teach that the sulfide-based solid electrolyte is an argyrodite type solid electrolyte of the form Li6PS5Cl, Li6PS5Br, and Li6PS5I.
Lee teaches a lithium secondary battery [0070, 0007]. The battery comprises a cathode, anode, and electrolyte where the electrolyte layer is between the cathode and the anode [0113]. Lee also teaches that the cathode active material may include Li2S and carbon fiber (fibrous carbon-based material) [0070, 0080]. The anode comprises an anode current collector and an anode active material layer (first anode active material layer) on a side of the anode current collector [0091]. Lee further teaches that the solid electrolyte is a sulfide-based solid electrolyte [0085]. The sulfide-based solid electrolyte comprises an argyrodite kind (argyrodite-type) solid electrolyte comprising at least one selected from Li6PS5Cl, Li6PS5Br, and Li6PS5I [0087]. The motivation to use an argyrodite-type solid electrolyte is to reduce the internal resistance of the battery [0088].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the lithium secondary battery taught by Liu and Pai with the teachings of Lee to have an argyrodite-type sulfide-based solid electrolyte to reduce the internal resistance in the battery.
Regarding claim 19, Liu in view of Pai teaches all the limitations of claim 14 as described above. Liu teaches an anode current collector but does not explicitly teach a second anode active material layer or its position relative to the other battery elements.
Lee teaches a lithium secondary battery [0070, 0007]. The battery comprises a cathode, anode, and electrolyte where the electrolyte layer is between the cathode and the anode [0113]. Lee also teaches that the cathode active material may include Li2S and carbon fiber (fibrous carbon-based material) [0070, 0080]. The anode comprises an anode current collector and an anode active material layer (first anode active material layer) on a side of the anode current collector [0091]. Lee further teaches a second anode activate material layer which is disposed between the current collector (anode current collector) and the anode active material layer (first anode active material layer) [0105]. The second anode active material layer is a metal layer which comprises lithium and/or a lithium alloy [0105]. The purpose of including a second anode active material is to improve the cycle characteristics of the secondary battery with the second anode acting as a lithium reservoir [0107-0178].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the lithium secondary battery taught by Liu and Pai with the teachings of Lee to have a second anode active material layer made of lithium between the anode current collector and the first anode active material for the purpose of improving the battery’s cycle characteristics.
Regarding claim 20, Liu in view of Pai teaches all the limitations of claim 14 as described above. Liu teaches an aluminum, lithium, sodium, or alloy metal layer for the current collectors [0021, 0023] but is silent on the presence or composition of a base film layer in the current collector.
Lee teaches a lithium secondary battery [0070, 0007]. The battery comprises a cathode, anode, and electrolyte where the electrolyte layer is between the cathode and the anode [0113]. Lee also teaches that the cathode active material may include Li2S and carbon fiber (fibrous carbon-based material) [0070, 0080]. The anode comprises an anode current collector and an anode active material layer (first anode active material layer) on a side of the anode current collector [0091] Lee further teaches that the cathode and anode contain a current collector in the form of a plate or foil (metal layer) which may include copper, stainless steel, titanium, iron, cobalt, nickel, aluminum, or a combination [0056]. The cathode and anode each include a binder (base film) which may contain polyethylene [0079, 0099]. Since the electrode (anode or cathode) inherently contains a current collector, the structure of the electrode and electrode current collector are considered together. Therefore, the binder in the cathode and anode reads on the base film of the cathode current collector or the anode current collector. The purpose of including a binder is to stably disperse the active material [0100].
It would have been prima facie obvious to one of ordinary skill in the art, before the effective filing date of the claimed invention, to modify the lithium secondary battery taught by Liu and Pai with the teachings of Lee to have an anode or cathode current collector that comprises a base film and a metal layer on the side of the base film to stabilize the active material.
Conclusion
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/N.R.A./Examiner, Art Unit 1785
/MARK RUTHKOSKY/Supervisory Patent Examiner, Art Unit 1785
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