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 .
Election/Restrictions
Applicant’s election without traverse of Group I, claims 1-6, 10-11, and 13-5, drawn to a lithium-containing oxide cathode material in the reply filed on February 9th, 2026 is acknowledged.
Claims 7-8 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected preparation method of the lithium-containing oxide cathode material, there being no allowable generic or linking claim.
Election was made without traverse in the reply filed on February 9th, 2026.
Claim Rejections - 35 USC § 112(b)
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.
Claim 1-6, 10-11, 13-15 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.
Regarding claim 1, the instant claim recites the Formula (3), Li[LiaNixMnyMj]O2@M’. It is unclear to the Examiner what is meant by an “@” symbol in a chemical formula, as no such notation is known in the art relating to lithium-containing oxide cathode materials. It is further unclear the structural features required of M’ to be considered a part of the composition, for example if M’ represents a component which is in complex with Li[LiaNixMnyMj]O2, or is a coating on Li[LiaNixMnyMj]O2. For the purposes of examination, @M’ is understood to refer to a compound M’ which is associated with the remainder of the chemical composition of the lithium-containing oxide cathode material.
Regarding claims 2-6, they are rejected based on their dependence on a previously rejected claim.
Regarding claim 10, the instant claim recites the Formula (3), Li[LiaNixMnyMj]O2@M’. It is unclear to the Examiner what is meant by an “@” symbol in a chemical formula, as no such notation is known in the art relating to lithium-containing oxide cathode materials. It is further unclear the structural features required of M’ to be considered a part of the composition, for example if M’ represents a component which is in complex with Li[LiaNixMnyMj]O2, or is a coating on Li[LiaNixMnyMj]O2. For the purposes of examination, @M’ is understood to refer to a compound M’ which is associated with the remainder of the chemical composition of the lithium-containing oxide cathode material.
Regarding claims 11, 13-15, they are rejected based on their dependence on a previously rejected claim.
Further regarding claim 1, the preamble of the instant claim recites “a lithium-containing oxide cathode material.” However, the instant claim recites “the cathode material” and “the lithium-containing oxide cathode material.” It is unclear if the cathode material refers to the same material as the lithium-containing oxide cathode material. For the purposes of examination, all recitations of “the cathode material” is presumed to refer to the lithium-containing oxide cathode material as recited in the preamble. The Examiner asks that the recitations of the cathode material be amended to incorporate consistent claim language with respect to the lithium-containing oxide cathode material.
Regarding claim 2, the preamble of the instant claim recites “the cathode material”. However, the independent claim recites “the lithium-containing oxide cathode material” in the preamble. It is unclear if the cathode material refers to the same material as the lithium-containing oxide cathode material. For the purposes of examination, all recitations of “the cathode material” is presumed to refer to the lithium-containing oxide cathode material of claim 1. The Examiner asks that the recitations of the cathode material be amended to incorporate consistent claim language with respect to the lithium-containing oxide cathode material.
Regarding claims 3-6, they are rejected based on their dependence on a previously rejected claim.
Regarding claim 10, the instant claim recites “a lithium-containing oxide cathode material.” However, the instant claim recites “the cathode material” and “the lithium-containing oxide cathode material.” It is unclear if the cathode material refers to the same material as the lithium-containing oxide cathode material. For the purposes of examination, all recitations of “the cathode material” is presumed to refer to the lithium-containing oxide cathode material. The Examiner asks that the recitations of the cathode material be amended to incorporate consistent claim language with respect to the lithium-containing oxide cathode material.
Regarding claim 13, the instant claim recites “the cathode material”. However, the independent claim recites “the lithium-containing oxide cathode material”. It is unclear if the cathode material refers to the same material as the lithium-containing oxide cathode material as the independent claim. For the purposes of examination, all recitations of “the cathode material” is presumed to refer to the lithium-containing oxide cathode material of claim 10. The Examiner asks that the recitations of the cathode material be amended to incorporate consistent claim language with respect to the lithium-containing oxide cathode material.
Regarding claims 11, 13-14, they are rejected based on their dependence on a previously rejected claim.
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.
Claims 1-4, 10-11, and 13-15 are rejected under 35 U.S.C. 103 as being unpatentable over Du (Chinese Patent Publication No. 111384371 A).
Regarding claim 1, Du teaches a lithium-containing oxide cathode material (Paragraph 10).
It is reasonable to presume that the lithium-containing oxide cathode material of Du:
has a compressive index Δλ(P100) satisfying Δλ(P100) ≥ 60%+(y/x)×5%,
has a compressive index Δλ(P300) satisfying Δλ(P300) ≥ 35%+(y/x)×5%,
where y/x is a molar ratio of Mn/Ni in the cathode material,
wherein the compressive index Δλ(P100) is calculated based on the following equation:
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106
473
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, where:
D50 refers to a value of particle cumulative distribution D5 of the material in a natural state without external mechanical pressure, i.e., P=0 Mpa;
D5p100 refers to a value of particle cumulative distribution D5 of the material under P=l00 Mpa;
D5 refers to a particle size value when a cumulative volume distribution of the particles is 5%;
Δλ(P100) represents the compressive index of the material when pressure P=l00Mpa;
Δλ(P200) represents the compressive index of the material when pressure P=200Mpa; and
Δλ(P300) represents the compressive index of the material when pressure P=300Mpa,
wherein the lithium-containing oxide cathode material has a chemical formula represented by Formula (3):
Li[LiaNixMnyMj]O2@M’, Formula (3), where:
0≤a≤0.3; 0.2<x<1; 0<y≤0.75; 0<j≤0.35; M is selected from at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B;
M' is an oxide, phosphide, sulfide, fluoride, or chloride containing at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B; and
a molar content of cations in M' is w, w satisfying 0<w/(a+x+y+j)≤0. l.
Support for said presumption is found in that Du teaches a method of making the lithium-containing oxide cathode material which overlaps the method described by the instant disclosure, particularly relating to the conditions of the process and the materials used.
The instant disclosure provides the following flows in the preparation method of a lithium-containing oxide cathode material (Paragraph 0073):
S1: uniformly mixing a precursor having a chemical formula represented by Formula (1), a lithium source, and an optional additive containing element M2, and performing a first sintering on the mixed material in an atmosphere furnace, to obtain a primary sintered material having a chemical formula represented by Formula (2); and
S2: uniformly mixing the primary sintered material with an additive containing element M′, and performing a second sintering on the mixed material in an atmosphere furnace, to obtain a lithium-containing metal oxide having a chemical formula represented by Formula (3)
NiuMnvM1γ(OH)2, Formula (1)
where: u+v+γ=1, 0.2<u<1, 0<v≤0.75, 0≤γ≤0.35, and M1 is selected from at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, Na, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B;
Li[LiaNixMnyMj]O2, Formula (2);
Li[LiaNixMnyMj]O2@M′, Formula (3);
wherein in Formula (2) and Formula (3), 0≤a≤0.3, 0.2<x<1, 0<y≤0.75, 0<j≤0.35; and M includes element M1 in the precursor and element M2 introduced during the first sintering, M1 and M2 being the same or different and being each selected from at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B;
and wherein in Formula (3), M' is oxide, phosphide, sulfide, fluoride, or chloride containing at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B, and a molar content of cations in M' is w, w satisfying 0 < w/(a+x+y+j) ≤ 0.1.
The following process steps to produce a lithium-containing oxide cathode material of Du are related to the process steps to produce a lithium-containing oxide cathode material of the instant disclosure.
Du discloses a method of preparing the cathode material of the instant disclosure including raw material of a ternary material precursor of nickel, cobalt, manganese and/or aluminum and a lithium source (Paragraph 68), which is equated with step S1 of the instant disclosure including mixing a chemical formula represented by Formula (1) and a lithium source. The instant disclosure provides the additive containing element M2 is optional (Paragraph 0008), and is thus not considered pertinent by the Examiner in obtaining the product of the instant disclosure.
The examples of suitable ternary material precursor of nickel, cobalt, manganese and/or aluminum taught by Du overlaps with the general Formula (1) of the instant claim. Du teaches the precursor may be represented by Ni1/3Co1/3Mn1/3(OH)2, Ni0.5Co0.2Mn0.3(OH)2, Ni0.5Co0.25Mn0.25(OH)2, Ni0.55Co0.15Mn0.3(OH)2, Ni0.55Co0.1Mn0.35(OH)2, Ni0.55Co0.05Mn0.4(OH)2, Ni0.6Co0.2Mn0.2(OH)2, Ni0.75Co0.1Mn0.15(OH)2, Ni0.8Co0.1Mn0.1(OH)2, Ni0.88Co0.05Mn0.07(OH)2 (Paragraph 68), which overlaps with Formula (1) of the instant claim, NiuMnvM1γ(OH)2, when M1 is Co, as the subscripts of the elements Ni, Mn, and M1 of Du lie within the ranges defined by the instant claim for u, v, and γ, respectively.
The instant disclosure provides that the lithium source in step S1 of the disclosure is at least one of lithium hydroxide, lithium carbonate, and lithium nitrate (Paragraph 0075). Du teaches the lithium-containing raw material may be LiOH (lithium hydroxide) and Li2CO3 (lithium carbonate) (Paragraph 68).
The instant disclosure provides a molar ratio Li/(Ni+Mn+M1+M2) of the lithium source to a sum of the precursor and the additive containing the element M2 ranges from 1 to 1.85, and preferably from 1 to 1.5 (Paragraph 0079). In the examples provided, Du teaches the nickel-cobalt-manganese ternary material precursor and lithium-containing compound are mixed at a molar ratio of 1:1.05 (Paragraph 86). Therefore, Du teaches a molar ratio Li/(Ni+Mn+M1+M2) of the lithium source to a sum of the precursor and the additive containing the element M2 (1:05:1) that lies within the instant range disclosed by the specification.
Additionally in step S1, Du teaches performing a first sintering on the mixed material in an atmosphere furnace, to obtain a primary sintered material having a chemical formula represented by Formula (2).
In Example 1 of the disclosure, Du teaches sintering the mixture of the precursor and the Li-containing compound followed by sintering in an atmosphere furnace at 800°C (Paragraph 86). Du teaches the oxygen concentration during sintering may be greater than or equal to 20 percent (Paragraph 68). The precursor material of Du of Example 1 is represented by Ni0.8Co0.1Mn0.1(OH)2, and thus the molar ratio of Ni/Mn, x/y, is 0.8/0.1, or 8.
The instant disclosure provides in step S1 of the method:
[0083]According to the present disclosure, when a molar ratio of Ni/Mn is greater than 1, that is, x/y>1, a relationship between a sintering temperature T1 of the first sintering and a content of Ni satisfies 550×(2-x)℃≤T1≤400×(3-x)℃, and a sintering duration of the first sintering ranges from 6 hours to 20 hours, and preferably, from 8 hours to 15 hours. The molar ratio of Ni/Mn of Example 1 taught by Du is smaller than 1
According to the teachings of the instant disclosure, the ratio x/y taught by Du is greater than 1, thus the sintering temperature should fall within the range of 550×(2-0.8)℃ ≤ T1 ≤ 400×(3-0.8)℃, or 660℃ ≤ T1 ≤ 880 ℃. Thus, the temperature for sintering taught by Du for Example 1 of the disclosure lies within the range of suitable temperatures for sintering taught by the instant disclosure according to the molar ratio of Ni/Mn in order to obtain the claimed lithium-containing oxide cathode material according to the instant disclosure.
The instant disclosure provides in step S1 of the method:
[0084]According to the present disclosure…when x≥0.6, the first sintering and the second sintering are performed in an oxygen atmosphere or a mixture atmosphere of oxygen and air.
As mentioned above, Du teaches sintering in at atmospheric furnace wherein the oxygen concentration during sintering may be greater than or equal to 20 percent. Thus, according to the subscript of nickel of the precursor material of Du of Example 1, x=0.8, Du teaches the appropriate atmospheric conditions for sintering in order to obtain the claimed lithium-containing oxide cathode material according to the instant disclosure.
Therefore, the overlap between the first step of Du and step S1 of the instant disclosure results in a primary sintered material having a chemical formula represented by Formula (2), or it would have been obvious to the ordinary artisan that the steps of Du discussed above would result in a primary sintered material having a chemical formula represented by Formula (2). Additionally, Du teaches in Table 2, the positive active material represented by the formula LiNi0.8Co0.1Mn0.1O2 overlaps with the general Formula (2) of the instant disclosure, when M1 is Co, as the subscripts of the elements Ni, Mn, and M1 of Du lie within the ranges defined by the instant claim for u, v, and γ, respectively.
Thus, Du teaches the method step S1 in the process of forming lithium-containing oxide cathode material which shares process steps, conditions, and raw materials as the instant disclosure.
Du discloses a method of preparing the cathode material of the instant disclosure including a second step of mixing and sintering the positive electrode active material matrix, formed by sintering the nickel-cobalt-manganese ternary material precursor and the Li-containing precursor described above, with an additive Al2O3 (Paragraph 86), which is equated with step S2 of the instant disclosure.
The instant disclosure provides, the additive containing the element M' is selected from at least one of oxide, hydroxide, oxyhydroxide, phosphate, fluoride, boride, nitride, carbonate, and oxalate containing the element M', which as described above is Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B.
As described above, Du teaches the additive is Al2O3, which is considered at additive is an oxide containing the element M’ when M’=Al.
The instant disclosure provides a molar ratio M'/(Ni+Mn+M1+M2) of the additive containing the element M' to the primary sintered material ranges from 0 to 0.1, and preferably, from 0.001 to 0.02 (Paragraph 0081).
Du teaches an additive Al2O3 is added to the positive electrode active material matrix formed in step 1 (primary sintered material) in a ratio of 100:0.3 (Paragraph 86). Thus, Du teaches the molar ratio M'/(Ni+Mn+M1+M2) of the additive containing the element M' to the primary sintered material, Ni0.8Co0.1Mn0.1(OH)2, to be 0.006 (0.6/(80+10+10)). Thus, the molar ratio at which the element M’ in the additive is added to the primary sintered material in step 2 of Du overlaps with the range of the instant claim.
The instant disclosure provides in step S1 of the method:
[0084]According to the present disclosure…when x≥0.6, the first sintering and the second sintering are performed in an oxygen atmosphere or a mixture atmosphere of oxygen and air.
Du teaches the second sintering in at atmospheric furnace (Paragraph 86). As an atmospheric atmosphere comprises oxygen, the furnace of Du is considered a mixture atmosphere of oxygen and air. Thus, according to the subscript of nickel of the precursor material of Du of Example 1, x=0.8, Du teaches the appropriate atmospheric conditions for sintering in order to obtain the claimed lithium-containing oxide cathode material according to the instant disclosure.
Thus, Du teaches the method step S2 in the process of forming lithium-containing oxide cathode material which shares process steps, conditions, and raw materials as the instant disclosure.
Therefore, the overlap between the second step of Du and step S2 of the instant disclosure results in a lithium-containing metal oxide having a chemical formula represented by Formula (3), or it would have been obvious to the ordinary artisan that the steps of Du discussed above would result in a lithium-containing metal oxide having a chemical formula represented by Formula (3).
In summary, as detailed above, the method of producing a lithium-containing oxide cathode material disclosed by Du aligns with the method steps to produce the lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials, their proportions, and the process conditions. Therefore, a lithium-containing oxide cathode material whose compressive index, particle size distribution, and chemical formula meeting instant claimed limitations would result from the method taught by Du, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material possessing the properties of the instant claim.
Regarding claim 2, Du teaches the cathode material according to claim 1.
As described above in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material wherein:
the cathode material has a compressive index Δλ(P200) satisfying Δλ(P200) ≥ 45%+(y/x)×5%.
Regarding claim 3, Du teaches the lithium-containing oxide cathode material according to claim 1.
As described above in the rejection of claim 1, the method taught by Du and embodied in Example 1 of the disclosure, the precursor material of Du comprising M1, and thus M in the final product (the disclosure provides the source of the element M in the cathode material includes the element M1 in the precursor and the optional additive containing the element M2 introduced during the first sintering process), is Co. Thus it would be obvious the ordinary artisan that if the precursor materials comprise M as cobalt, then the resulting lithium-containing oxide cathode material represented by formula (3) would comprise cobalt, meeting the instant claimed limitations when M is selected from at least one element including Co.
Further, as described above, the additive of Du included in the second step of the method was represented by Al2O3. However, Du teaches generally that the coating element of the outer coating layer is at least selected from two or more of Al, Ba, Zn, Ti, Co, W, Y, Si, Sn, B, and P and the outer coating layer on the surface of the positive electrode active material contains at least two or more oxides formed by the above elements (Paragraph 51). Thus according to the teachings of Du described in the embodiment above the ordinary artisan may include oxide additives, in addition to Al2O3, such as titanium oxide, cobalt oxide, tungsten oxide, yttrium oxide, and or boron oxide in the method of making the lithium-containing oxide cathode material according to the teachings of Du.
Thus, in the second step of mixing and sintering the positive electrode active material matrix, with an additive Al2O3 (Paragraph 86) and additionally titanium oxide, cobalt oxide, tungsten oxide, yttrium oxide, and or boron oxide, is equated with step S2 of the instant disclosure, when M’ is an oxide containing at least one element of Ti, Y, Co, W, and B.
Thus as described above and in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations of Formula (3), or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material meeting the instant claimed limitations;
in Formula (3):
0.02≤a≤0.2;
0.3<x<0.9;
0.05<y≤0.68;
0<j≤0.30;
0.001<w/(a+x+y+j)≤0.02;
Regarding claim 4, Du teaches the lithium-containing oxide cathode material according to claim 1.
As described above in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material wherein:
the lithium-containing oxide cathode material has a pellet density of ≥ 2.8 g/cm3, preferably ≥ 3 g/cm3; and/or
the lithium-containing oxide cathode material has a tap density of ≥ 1.7 g/cm3, preferably ≥ 2 g/cm3; and/or
a content of surface soluble alkali of the lithium-containing oxide cathode material satisfies the following conditions: Li2CO3≤l wt%, LiOH≤0.5 wt%;
a full width at half maximum FWHM(003) of (003) crystal plane and a full width at half maximum FWHM(104) of (104) crystal plane of the lithium-containing oxide cathode material obtained by X-Ray Diffraction, XRD, satisfy the following conditions: 0.10≤FWHM(003)≤0.25; and 0.20≤FWHM(104)≤0.50; and/or
a peak area S(003) of the (003) crystal plane and a peak area S(104) of the (104) crystal plane of the lithium-containing oxide cathode material obtained by XRD satisfy the following conditions: 1.1≤S(003)/S(104)≤1.8
Regarding claim 10, Du teaches a positive electrode sheet (plate) including a positive electrode material layer on the positive electrode current collector, the positive electrode material layer includes the positive electrode active material of the disclosed invention. Du teaches the positive electrode active material may be mixed with a binder and a conductive agent to form a slurry prior to coating on the current collector (Paragraph 75). In an embodiment of the disclosure, Du teaches the prepared positive electrode material (lithium-containing oxide cathode material) mixed with a binder and a conductive agent at a mass ratio of 98:1:1 (Paragraph 88). Thus, Du teaches the positive electrode plate comprising 98% of a lithium-containing oxide cathode material based on a total weight of the positive electrode plate, which lies within the suitable range of the instant claim, meeting the claimed limitations.
As discussed above in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material wherein:
the cathode material has a compressive index Δλ(P100) satisfying Δλ(P100)≥60%+(y/x)×5%,
the cathode material has a compressive index Δλ(P300) satisfying Δλ(P300)≥35%+(y/x)×5%, where y/x is a molar ratio of Mn/Ni in the cathode material,
wherein the compressive index Δλ(P100) is calculated based on the following equation:
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, where:
D50 refers to a value of particle cumulative distribution D5 of the material in a natural state without external mechanical pressure, i.e., P=0 Mpa;
D5p100 refers to a value of particle cumulative distribution D5 of the material under P=l00 Mpa;
D5 refers to a particle size value when a cumulative volume distribution of the particles is 5%;
Δλ(P100) represents the compressive index of the material when pressure P=l00Mpa;
Δλ(P200) represents the compressive index of the material when pressure P=200Mpa; and
Δλ(P300) represents the compressive index of the material when pressure P=300Mpa,
wherein the lithium-containing oxide cathode material has a chemical formula represented by Formula (3):
Li[LiaNixMnyMj]O2@M’, Formula (3), where:
0≤a≤0.3; 0.2<x<1; 0<y≤0.75; 0<j≤0.35; M is selected from at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B;
M' is an oxide, phosphide, sulfide, fluoride, or chloride containing at least one element of Al, Zr, Nb, Ti, Y, Sc, Cr, Co, W, Mg, La, Os, Pr, Re, Ru, Sr, Sm, Ta, and B; and
a molar content of cations in M' is w, w satisfying 0<w/(a+x+y+j)≤0. l.
Regarding claim 11, Du teaches the positive electrode plate according to claim 10.
It is reasonable to presume that the positive electrode plate of Du has an electrode density of ≥ 2.8 g/cm3.
Support for said presumption is found in that, as described above, Du teaches a positive electrode plate comprising a suitable proportion of lithium-containing oxide cathode material, the lithium-containing oxide cathode material produced by a method whose precursor materials, their proportions, and process conditions overlap with those of the instant claim.
Therefore, a positive electrode plate whose who density meets the instant claimed limitations would result from the method taught by Du, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a positive electrode plate possessing the properties of the instant claim.
Regarding claim 13, Du teaches the positive electrode plate according to claim 10,
As described above in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material wherein:
Δλ(P200) satisfying Δλ(P200) ≥ 45%+(y/x)×5%.
Regarding claim 14, Du teaches the positive electrode plate according to claim 10.
As described above in the rejection of claim 1, the method taught by Du and embodied in Example 1 of the disclosure, the precursor material of Du comprising M1, and thus M in the final product (the disclosure provides the source of the element M in the cathode material includes the element M1 in the precursor and the optional additive containing the element M2 introduced during the first sintering process), is Co. Thus it would be obvious the ordinary artisan that if the precursor materials comprise M as cobalt, then the resulting lithium-containing oxide cathode material represented by formula (3) would comprise cobalt, meeting the instant claimed limitations when M is selected from at least one element include Co.
Further, as described above, the additive of Du included in the second step of the method was represented by Al2O3. However, Du teaches generally that the coating element of the outer coating layer is at least selected from two or more of Al, Ba, Zn, Ti, Co, W, Y, Si, Sn, B, and P and the outer coating layer on the surface of the positive electrode active material contains at least two or more oxides formed by the above elements (Paragraph 51). Thus according to the teachings of Du described in the embodiment above the ordinary artisan may include oxide additives, in addition to Al2O3, such as titanium oxide, cobalt oxide, tungsten oxide, yttrium oxide, and or boron oxide in the method of making the lithium-containing oxide cathode material according to the teachings of Du.
Thus, in the second step of mixing and sintering the positive electrode active material matrix, with an additive Al2O3 (Paragraph 86) and additionally titanium oxide, cobalt oxide, tungsten oxide, yttrium oxide, and or boron oxide, is equated with step S2 of the instant disclosure, when M’ is an oxide containing at least one element of Ti, Y, Co, W, and B.
Thus as described above and in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material meeting the instant claimed limitations of Formula (3): 0.02≤a≤0.2; 0.3<x<0.9; 0.05<y≤0.68; 0<j≤0.30; 0.001<w/(a+x+y+j)≤0.02.
Regarding claim 15, Du teaches the positive electrode plate according to claim 10.
As described above in the rejection of claim 1, the method of producing a lithium-containing oxide cathode material by Du aligns with the method steps to produce a lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the precursor materials and their quantities in each step as well as the process conditions.
Therefore, it is reasonable to presume that the positive electrode active oxide material produced by the method taught by Du meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a lithium-containing oxide cathode material wherein:
the lithium-containing oxide cathode material has a pellet density of ≥ 2.8 g/cm3; and/or
the lithium-containing oxide cathode material has a tap density of ≥ 1.7 g/cm3; and/or
a content of surface soluble alkali of the lithium-containing oxide cathode material satisfies the following conditions: Li2CO3≤l wt%, LiOH≤0.5 wt%;
a full width at half maximum FWHM(003) of (003) crystal plane and a full width at half maximum FWHM(104) of (104) crystal plane of the lithium-containing oxide cathode material obtained by X-Ray Diffraction, XRD, satisfy the following conditions: 0.10≤FWHM(003)≤0.25; and 0.20≤FWHM(104)≤0.50; and/or
a peak area S(003) of the (003) crystal plane and a peak area S(104) of the (104) crystal plane of the lithium-containing oxide cathode material obtained by XRD satisfy the following conditions: 1.1≤S(003)/S(104)≤1.8
Claims 5-6 are rejected under 35 U.S.C. 103 as being unpatentable over Du as applied to claims 1-4, 10-11, and 13-15 above, and further in view of Shang (Chinese Patent Publication No. 103794778 A).
Regarding claim 5, Du teaches a lithium-containing oxide cathode material according to claim 1.
Du is silent to:
a precursor of the lithium-containing oxide cathode material has a compressive index Δλ’(P50) satisfying Δλ’(P50) ≥ 35%+(v/u)×8%, where v/u is a molar ratio of Mn/Ni in the precursor,
wherein the compressive index Δλ’(P50) of the precursor is calculated based on the following equation:
PNG
media_image2.png
93
530
media_image2.png
Greyscale
where:
D’50 to refers to a value of particle cumulative distribution D5 of the precursor in a natural state without external mechanical pressure, i.e. P=0 Mpa;
D’5P50 to a value of particle cumulative distribution D5 of the precursor under P=50 Mpa;
Δλ’(P50) represents the compressive index of the precursor when pressure P=50 MPa; and
Δλ’(P100) represents the compressive index of the precursor when pressure P=100 MPa.
However, Shang discloses a method for preparing a lithium nickel cobalt manganate cathode material (Paragraph 10), including the preparation of a nickel-cobalt-manganese oxyhydroxide precursor (Paragraph 11). Shang teaches the advantages of the method to form the precursor by the disclosed method is that the compacted density of the prepared nickel cobalt lithium manganate material is large, the specific capacity is high, the rate property and consistency are good, the preparation method is simple, and the preparation process is easy to control and operate (Paragraphs 21-25).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified Du to incorporate the teachings of Shang in which the precursor of the lithium-containing oxide cathode material of Du is prepared according to the method of Shang. Doing so would advantageously result in a large compacted density, specific capacity, and rate property of the resulting cathode material and the preparation method of the method is simple, easy to control, and operate, as recognized by Shang,
It is reasonable to presume the precursor material of Du in view of Shang:
has a compressive index Δλ’(P50) satisfying Δλ’(P50) ≥ 35%+(v/u)×8%, where v/u is a molar ratio of Mn/Ni in the precursor,
wherein the compressive index Δλ’(P50) of the precursor is calculated based on the following equation:
PNG
media_image2.png
93
530
media_image2.png
Greyscale
where:
D’50 to refers to a value of particle cumulative distribution D5 of the precursor in a natural state without external mechanical pressure, i.e. P=0 Mpa;
D’5P50 to a value of particle cumulative distribution D5 of the precursor under P=50 Mpa;
Δλ’(P50) represents the compressive index of the precursor when pressure P=50 MPa; and
Δλ’(P100) represents the compressive index of the precursor when pressure P=100 MPa.
Support for said presumption is found in that Shang teaches a method of making the precursor of a lithium-containing oxide cathode material which overlaps the method described by the instant disclosure, particularly relating to the conditions of the process and the materials used.
The instant disclosure provides the following flows in the preparation method for the precursor of a lithium-containing oxide cathode material (Paragraph 0061)
(1) mixing, by contacting, a solution or suspension of a nickel salt, a manganese salt, and a compound containing M, to obtain a mixed salt solution; and
(2) feeding the parallel flows of the mixed salt solution, a precipitant solution, and a complexing agent solution l into a reactor for crystallization reaction, and performing solid-liquid separation, washing, heat treatment, and sieving treatment on the obtained slurry, to obtain the precursor of the lithium-containing oxide cathode material.
The following process steps to produce a lithium-containing oxide cathode material of Shang are related to the process steps to produce a lithium-containing oxide cathode material of the instant disclosure.
Shang teaches in the method a nickel salt, a cobalt salt, and a manganese salt solution are uniformly mixed in a first step to form a mixed solution (Paragraph 32).
The instant disclosure provides in step (1), the nickel salt is one or more of nickel sulfate, nickel chloride, nickel nitrate, and nickel acetate (Paragraph 0067); the manganese salt is one or more of manganese sulfate, manganese chloride, manganese nitrate, and manganese acetate (Paragraph 0068); and the compound containing M is one or more of sulfate, chloride, nitrate, acetate, citrate, carbonate, phosphate, oxalate, and fluoride containing the element M (Paragraph 0069).
In Example 1 of Shang, Shang teaches the nickel-cobalt-manganese solution was prepared using nickel sulfate, cobalt sulfate, and manganese sulfate (Paragraph 32), which overlaps with the materials used to form the precursor oxyhydroxide material of Formula (1) of the instant disclosure, when M is cobalt.
The instant disclosure provides the nickel salt, the manganese salt, or the additive containing M element are dissolved according to a molar ratio of u : v : γ (Paragraph 0063), where in the precursor material, u+v+γ=1, 0.2<u<1, 0<v≤0.75, 0≤γ≤0.35 (Paragraph 0073).
According to the teachings of Shang in Example 1, the mixed solution was prepared according to mixing nickel, cobalt, and manganese in a ratio of 0.5:0.2:0.3. Thus, Shang teaches the nickel salt, the manganese salt, or the additive containing M element are dissolved according to a molar ratio u=0.5 : v = 0.3 : γ = 0.2, which aligns with the instant disclosure’s teachings that u+v+γ=1, and the values of u, v, and γ of Shang lie within the suitable ranges for these variables disclosed by the instant specification.
The instant disclosure provides in step (2), the mixed salt solution is fed to a reactor with a precipitant solution and a complexing agent solution for crystallization reaction (Paragraph 0061).
Shang teaches in the method the metal salt solution described above is co-currently added to a reaction kettle with a precipitating agent solution and a complexing agent solution in order to perform a precipitation reaction in an alkaline environment (Paragraph 11).
The instant disclosure teaches the precipitant is an alkaline substance, and the alkali is one or more of sodium hydroxide, potassium hydroxide, and lithium hydroxide (Paragraph 0070), the alkali solution with a concentration ranging from 2 mol/L to 10 mol/L is obtained by dissolving alkali (Paragraph 0063).
Shang teaches in the method, the precipitating agent solution is a 2-5 mol/L solution of sodium hydroxide, potassium hydroxide, or barium hydroxide (Paragraph 16). Thus, Shang teaches precipitating agents in the method which are shared by the instant disclosure, with a concentration that overlaps the suitable concentrations disclosed by the instant specification.
The instant disclosure teaches the complexing agent is one or more of salicylic acid, ammonium sulfate, ammonium chloride, ammonium hydroxide, sulfosalicylic acid, and ethylenediaminetetraacetic acid (Paragraph 0071), the complexing agent solution with a concentration ranging from 2 mol/L to 13 mol/L is obtained by dissolving a complexing agent (Paragraph 0063).
Shang teaches in the method, the complexing agent solution is a 1-4 mol/L solution of ammonia or ammonium, the ammonium salt solution is preferably chlorinated, ammonium nitrate, or ammonium sulfate (Paragraph 15). Thus, Shang teaches complexing agents in the method which are shared by the instant disclosure, with a concentration that overlaps the suitable concentrations disclosed by the instant specification.
The instant disclosure provides that the reaction conditions include: a reaction temperature ranging from 40℃ to 70°C, reaction pH ranging from 10.6 to 12.5, and a reaction duration ranging from 5 hours to 100 hours (Paragraph 0066).
Shang teaches in the method of forming the precursor, the reaction conditions are controlled, specifically the pH of the reaction system of the precipitation reaction is controlled to be 8.5 to 11.5, the reaction temperature is 50 to 70 ° C, ranges which overlap the reaction conditions of the instant disclosure as suitable pH and reaction temperatures to perform the precipitation reaction.
The instant disclosure teaches in step 2, after the precipitation reaction, performing solid-liquid separation, washing, heat treatment, and sieving treatment on the obtained slurry, to obtain the precursor of the lithium-containing oxide cathode material (Paragraph 0061). Shang teaches after the precipitation reaction is sufficiently carried out, the slurry is subjected to solid-liquid separation, washed and dried to obtain the precursor, overlapping with the steps of step (2) of the method of the instant disclosure.
The instant disclosure provides the slurry has a solid content ranging from 200 g/L to 1000 g/L, and preferably, from 300 g/L to 800 g/L (Paragraph 0064). Shang teaches the solid content of the reaction system is controlled by a solid content regulating valve (Paragraph 18), and an embodiment of preparing the precursor material of Example 3 in which the solid content regulating valve is controlled at 500 g/L, which overlaps with the suitable solid content of the slurry of the instant disclosure.
In summary, as detailed above, the method of producing a precursor of the lithium-containing oxide cathode material disclosed by Shang aligns with the method steps to produce the precursor of the lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the reactants, their proportions, and the process conditions.
Therefore, a precursor of the lithium-containing oxide cathode material whose compressive index and particle size distribution meeting instant claimed limitations would result from the method taught by Du in view of Shang, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a precursor of the lithium-containing oxide cathode material possessing the properties of the instant claim.
Regarding claim 6, the lithium-containing oxide cathode material according to claim 5.
As described above in the rejection of claim 5, the method of producing a precursor of the lithium-containing oxide cathode material disclosed by Du in view of Shang aligns with the method steps to produce a precursor of the lithium-containing oxide cathode material described in the instant disclosure, particularly relating to the reactants materials and their proportions as well as the process conditions.
Therefore, it is reasonable to presume that the precursor of the positive electrode active oxide material produced by the method taught by Du in view of Shang meets the instant claimed limitations, or it would have been obvious to the ordinary artisan to tune the conditions of the process described above to obtain a precursor of the lithium-containing oxide cathode material wherein:
a compressive index Δλ’(P100) satisfying Δλ’(P100)≥25%+(v/u)×8%.
Conclusion
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/O.A.J./Examiner, Art Unit 1789
/MARLA D MCCONNELL/Supervisory Patent Examiner, Art Unit 1789