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 .
Specification
The disclosure is objected to because of the following informalities: In [0038] “a molar ratio of iron and manganese to (Fe + Mn)/P of the is 1.45-1.465” contains a typo. Appropriate correction is required.
Claim Objections
Claim 6 is objected to because of the following informalities: line 1 “The method for preparing carbon-encapsulated lithium iron manganese phosphate material according to claim 2” should read “The method for preparing the carbon-encapsulated lithium iron manganese phosphate material according to claim 2”. Appropriate correction is required.
Claims 9-10 are objected to under 37 CFR 1.75(c) as being in improper form because a multiple dependent claim should refer to other claims in the alternative only. See MPEP § 608.01(n). Accordingly, the claims have not been further treated on the merits.
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 nonobviousness.
Claim 1 is rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al. (US 20190088922 A1, “Zhamu”) in view of Ruan et al. (CN 114512649 A, “Ruan”). The machine translation is used herein for citation purposes.
Regarding claim 1, Zhamu discloses a carbon-encapsulated lithium manganese iron phosphate material (see [0098] “lithium manganese-iron phosphate” & “material”; see [0040] “encapsulating device that encapsulates the prelithiated particles”; see [0066] “coating of carbon”). Regarding the limitation having a composition of: LiFe1-x-yMnxMyPO4@C, wherein M comprises at least one of Mg, V, Zr, Nb, In, Al, Co and Ni, 0.5 ≤ x ≤ 0.8, 0 < y ≤ 0.02, and C is encapsulated carbon, Zhamu discloses lithium manganese-iron phosphate in [0098] & discloses in [0065] “Al” & “In”, but does not explicitly disclose a composition of LiFe1-x-yMnxMyPO4@C nor 0.5 ≤ x ≤ 0.8, 0 < y ≤ 0.02.
Ruan teaches composition in [0013] “composite lithium iron phosphate positive electrode material includes a doping element M, M is Mg, Al, Ti, Zr, Zn, V, Co, W, and Nb, and its chemical composition is LiMnαFeβMγPO4/C, 0.55 ≤α <1, 0 <β ≤0.4, 0 ≤γ ≤0.05 & in [0021] “the additive is the oxide containing Mg, Al, Ti, Zr, Zn, V, Co, W and Nb”. Ruan teaches in abstract “composite lithium manganese iron phosphate positive electrode material by the invention has higher capacity and multiplying power performance, has better electrochemical performance, and the electrochemical performance is not reduced, the material particles can be large, realizing higher compaction density”.
Zhamu and Ruan are analogous to the current invention because they are related to the same field of endeavor, namely lithium-ion batteries (see [0003]).
Therefore, 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 incorporate composition “LiMnαFeβMγPO4/C, 0.55 ≤α <1, 0 <β ≤0.4, 0 ≤γ ≤0.05”, as suggested by Ruan into the carbon-encapsulated lithium manganese iron phosphate material of Zhamu because doing so improves electrochemical performance, as suggested by Ruan (see abstract).
Claims 2, 6-8 are rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al. (US 20190088922 A1, “Zhamu”) in view of Ruan et al. (CN 114512649 A, “Ruan”) as applied to claim 1 above, and further in view of Ren et al. (CN 106129409 B, “Ren”) and Dai et al. (CN 104425820 B, “Dai”). The machine translations are used herein for citation purposes.
Regarding claim 2, Zhamu discloses a method for preparing a carbon-encapsulated lithium manganese iron phosphate material (see [0058] “method” & see [0056] “method may further comprise a step of coating a surface of the fine particles with a thin layer of carbon”; see [0098] “lithium manganese-iron phosphate” & “material”; see [0040] “encapsulating device that encapsulates the prelithiated particles”). Regarding the limitation S10. Mixing and dissolving an iron source, a manganese source, phosphoric acid and deionized water according to a certain proportion, Zhamu does not explicitly disclose.
Ruan teaches composition & in [0018] “manganese source, iron source and phosphorous source are introduced into the reaction vessel, and the pH is adjusted to obtain Mn3(PO4)2/MnFe(PO4)(2a+3b)/3 precursor precipitate”; see [0065] “deionized water”.
Therefore, 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 incorporate “manganese source, iron source and phosphorous source are introduced into the reaction vessel” which reads on mixing and dissolving & “pH is adjusted” to obtain the precursor precipitate as suggested by Ruan into a method for preparing carbon-encapsulated lithium manganese iron phosphate material of Zhamu because doing so improves electrochemical performance, as suggested by Ruan (see abstract).
Regarding the limitation preparing a ferromanganese phosphate precursor by a liquid phase coprecipitation method, respectively placing the ferromanganese phosphate precursor in an inert atmosphere, Zhamu discloses in [0099] “co-precipitation” & “heat processes at high temperatures” & see [0115] “heat-treated at 400 °C for 2 h under Ar atmosphere” which reads on an inert atmosphere. Zhamu does not explicitly disclose first sintering, and removing crystallization water to obtain an anhydrous ferromanganese phosphate precursor.
Ruan teaches in [0020] “dried” & “sintering to obtain a lithium-containing composite cathode material LiMnFeMPO/C”.
Therefore, 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 incorporate sintering as suggested by Ruan (see [0020]) into a method for preparing carbon-encapsulated lithium manganese iron phosphate material of Zhamu because doing so improves electrochemical performance, as suggested by Ruan (see abstract).
Regarding the limitation S20. Taking and mixing two groups of the anhydrous ferromanganese phosphate precursors, lithium phosphate, a carbon source, a dopant and deionized water according to a certain proportion, stirring and dispersing, Zhamu does not explicitly disclose.
Ruan teaches in [0020] “precursor precipitate 3” & “dried” & “mixed with a lithium source, a carbon source, and additives”.
Therefore, 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 incorporate drying and mixing “with a lithium source, a carbon source, and additives” as suggested by Ruan (see [0020]) into the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of Zhamu because doing so improves electrochemical performance, as suggested by Ruan (see abstract).
Regarding the limitation and subjecting to wet grinding, spray drying and second sintering to obtain two groups of carbon-encapsulated lithium manganese iron phosphate intermediates, wherein the first group is sintered at a first temperature and the second group is sintered at a second temperature different from the first temperature, Zhamu discloses “spray drying” in [0034] & in [0120] “grinding the solids in a mortar”, & in [0099] “heat processes at high temperatures,” but does not explicitly disclose second sintering nor wet grinding.
Ren teaches sintering (see [0027] “pre-calcination and sintering” & describes “ball milling” which reads on grinding & in [0028] “after sintering and carbonization, the carbon layer on the surface of the cathode material is uniform and complete”). Ren teaches two sintering steps in Example 2 in [0055] “sintered under an argon atmosphere. It was pre-fired at 300 °C for 4 hours, then cooled to room temperature with the furnace. Then it was ground and crushed, and then added back into the tube furnace for sintering under an argon atmosphere. The sintering process was 600 °C for 8 hours” which describes a first temperature and a second temperature different from the first temperature. Ren teaches “for sintering manganese lithium iron manganese phosphate positive electrode material to obtain carbon-coated. The positive electrode material of the invention surface carbon film thickness small so as to obviously improve the electrochemical performance of the material” (see abstract).
Therefore, 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 incorporate sintering as suggested by Ren (see [0027], [0055]) into the method of Zhamu because doing so improves the electrochemical performance as suggested by Ren (see abstract).
Dai teaches wet grinding (see [0069] “wet-mixing sand mill during the preparation process greatly enhances the uniformity of the mixture, and allows the primary particles to be nano-sized, with a particle size of 200 to 300 nm” & primary particles has a shorter ion migration path, which increases the conductivity of the material”).
Zhamu and Dai are analogous to the current invention because they are related to the same field of endeavor, namely lithium ion batteries (see title).
Therefore, 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 incorporate wet grinding as suggested by Dai (see [0069]) into the method of Zhamu because doing so improves the mixing uniformity, allows for the particles to be nanosized and doing so further increase the conductivity, as suggested by Dai (see [0069]).
Regarding the limitation S30. mixing the two groups of carbon-encapsulated lithium manganese iron phosphate intermediates, a carbon source, a dopant and deionized water according to a certain proportion, stirring and dispersing, and subjecting to wet grinding, spray drying and third sintering to obtain the carbon-encapsulated lithium manganese iron phosphate material, Zhamu discloses in [0034] “spray drying” & in [0120] “grinding the solids in a mortar”, but does not explicitly disclose third sintering.
Ren teaches sintering in Example 1 see [0045] “sintering process is 650 °C for 6 hours”. Ren teaches “for sintering manganese lithium iron manganese phosphate positive electrode material to obtain carbon-coated. The positive electrode material of the invention surface carbon film thickness small so as to obviously improve the electrochemical performance of the material” (see abstract).
Therefore, 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 incorporate sintering steps as suggested by Ren (see Example 1 [0045] & see Example 2 [0055]) into the method of Zhamu because doing so improves the electrochemical performance of the material, as suggested by Ren (see abstract).
Regarding claim 6, Zhamu discloses the method for preparing the carbon-encapsulated lithium iron manganese phosphate material of claim 2 and further discloses wherein the carbon source comprises “surface-modified graphite” (see [0019]). Zhamu discloses the dopant comprises a compound of In, Al (see [0065] “dopants” & “Al” & “In”).
Regarding claim 7, Zhamu discloses the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of claim 2, and further discloses in [0067] “this solution can then be used to encapsulate solid particles via several of the micro-encapsulation methods” & “spray-drying”. Zhamu does not explicitly disclose wherein a mixing ratio of the two groups of carbon-encapsulated lithium manganese iron phosphate intermediates is (1-9):(9-1).
Ruan teaches in [0095] “solutions S1 and S3 were simultaneously added to the reaction vessel at a flow rate of 50 mL/h for S1 and 50 mL/h for S3” which reads on a ratio 1:1. Ruan teaches “the composite lithium manganese iron phosphate positive electrode material by the invention has higher capacity and multiplying power performance, has better electrochemical performance, and the electrochemical performance is not reduced, the material particles can be large, realizing higher compaction density” (see abstract).
Therefore, 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 incorporate ratio 1:1, as suggested by Ruan (see [0095]) into the method of Zhamu because doing so improves the electrochemical performance of the battery, as suggested by Ruan (see abstract).
Regarding claim 8, Zhamu discloses the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of claim 2 and further discloses grinding (see [0120] “grinding the solids in a mortar” & in [0102] “ball milling”). Zhamu does not explicitly disclose wherein in the wet grinding, a particle size D50 is controlled to be 0.3 µm-0.6 µm.
Dai teaches wet grinding (see [0069] “wet-mixing sand mill during the preparation process greatly enhances the uniformity of the mixture, and allows the primary particles to be nano-sized, with a particle size of 200 to 300 nm” & primary particles has a shorter ion migration path, which increases the conductivity of the material”). Dai teaches controlling particle size (see [0063]) “D50 is controlled”.
Dai teaches a range of 200 to 300 nm (equivalent to 0.2 µm to 0.3 µm), which overlaps with the claimed range of 0.3 µm to 0.6 µm. MPEP 2144.05 I states that 'In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990)'.
Therefore, 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 incorporate wet grinding and controlling particle size to smaller nanosized particle grain diameter between 200 and 300 nm, as suggested by Dai (see [0069]) because doing so increases the electric conductivity, as suggested by Dai (see [0069]).
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al. (US 20190088922 A1, “Zhamu”), Ruan et al. (CN 114512649 A, “Ruan”), Ren et al. (CN 106129409 B, “Ren”) and Dai et al. (CN 104425820 B, “Dai”) as applied to claim 2 above, and further in view of Jang (US 20200280055 A1, “Jang”). The machine translations are used herein for citation purposes.
Regarding claim 3, Zhamu discloses the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of claim 2 and further discloses wherein the first temperature is 400 °C (see [0099] “co-precipitation” & “heat processes at high temperatures” & see [0115] “heat-treated at 400 °C for 2 hours under Ar atmosphere”). Zhamu does not explicitly disclose the second temperature is 670 °C - 760 °C, and sintering time is 4h-6h.
Ren teaches “sintering process is 650 °C for 6 h” (see [0045]).
Ren teaches a range of 6h, which overlaps with the claimed range of 4h-6h. MPEP 2144.05 I states that 'In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990)'.
Jang teaches “carbon-encapsulated” (see title) & see [0100] teaches heat treatment temperature “between 300 and 1,500 °C”. Jang teaches in [0029] “that exhibit long and stable charge-discharge cycle life”.
Jang teaches a range of 300 and 1500°C, which overlaps with the claimed range of 670 °C – 760 °C. MPEP 2144.05 I states that 'In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990)'.
Claims 4-5 are rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al. (US 20190088922 A1, “Zhamu”), Ruan et al. (CN 114512649 A, “Ruan”), Ren et al. (CN 106129409 B, “Ren”) and Dai et al. (CN 104425820 B, “Dai”) as applied to claim 2 above, and further in view of Qi et al. (CN 106340639 A, “Qi”). The machine translations are used herein for citation purposes.
Regarding claim 4, Zhamu discloses the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of claim 2, but does not explicitly disclose wherein the iron source comprises at least one of ferrous sulfate, ferrous chloride, ferrous oxalate, and ferrous acetate.
Qi teaches in [0021] “preferably, the iron source is any one or a combination of two of ferrous oxalate” & “ferrous sulfate”. Qi teaches (see abstract) “the circulation performance of the battery is greatly improved.”
Zhamu and Qi are analogous to the current invention because they are related to the same field of endeavor, namely lithium ion batteries (see [0007]).
Therefore, 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 incorporate iron source is “ferrous oxalate”, “ferrous sulfate”, as suggested by Qi (see [0021]) into the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of Zhamu because doing so is preferable, as suggested by Qi (see [0021]).
Regarding claim 5, Zhamu discloses the method for preparing a carbon-encapsulated lithium manganese iron phosphate material of claim 2, but does not explicitly disclose wherein a molar ratio of iron and manganese to phosphorous (Fe + Mn)/P of the ferromanganese phosphate precursor is 1.45-1.465, and a molar ratio of lithium to iron and manganese Li(Fe+Mn) is 1.02-1.05.
Qi teaches molar ratio of iron and manganese to phosphorous and a molar ratio of lithium to iron and manganese is 1 (see [0019] “the stoichiometric ratio of the above substances are determined according to the formula LiMnxFe1-x PO4/LiMnyFe1-yPO4/LiFePO4/C, wherein 0.8 ≤ x ≤ 0.9 0.2 ≤ y ≤ 0.4”).
The amount of Fe, Mn, P and Li taught by reference Qi is close to the claimed range and similar properties are expected. It is the Office’s position that the values are close enough that one of ordinary skill in the art would have expected similar properties. A prima facie case of obviousness exists where the claimed ranges and prior art ranges do not overlap but are close enough that one skilled in the art would have expected them to have the same properties. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 227 USPQ 773 (Fed. Cir. 1985). See MPEP 2144.05.
Conclusion
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/S.A.A./Examiner, Art Unit 1725
/NICOLE M. BUIE-HATCHER/Supervisory Patent Examiner, Art Unit 1725
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