Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Continued Examination Under 37 CFR 1.114
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on 12/30/2025 has been entered.
DETAILED ACTION
This Office Action is responsive to the amendment filed on 12/30/2025. Claims 1-17 are pending. Applicant’s arguments have been considered. Claims 1-17 are non-finally rejected for reasons stated herein below.
Claim Rejections - 35 USC § 103
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
Claim(s) 1-17 are rejected under 35 U.S.C. 103 as being unpatentable over Lee (US 2022/0140327) in view of Kim (US 2012/0037858).
Regarding claim 1, Lee discloses a negative electrode material for a secondary battery in a particle form, comprising: a matrix including a silicon oxide, a composite oxide of silicon and one or more doping elements selected from the group consisting of alkali metals, alkaline earth metals, and post transition metals, or a mixture thereof; and silicon nanoparticles dispersed and embedded in the matrix [0008],
wherein a compressive strength of the particles is 100 MPa or more [0081]. See Table 1.
Regarding claim 6, the FWHM of the Raman peak of nanoparticulate silicon included in the negative electrode material is 4 to 20 cm⁻¹ [0068].
Regarding claim 7, the following Equation 1 is satisfied based on a silicon Raman signal:
Equation 1
1 < WN(Si)/WN(ref)
wherein WN(ref) is a central wave number of a Raman peak of bulk monocrystalline silicon, and WN(Si) is a central wave number of a Raman peak of nanoparticulate silicon included in the negative electrode material [0061].
Regarding claim 8, in a two-dimensional mapping analysis based on the silicon Raman signal a difference between a maximum value and a minimum value of shift as defined by the following Equation 2
Shift = WN'(Si)-WN(ref)
wherein WN(ref) is as defined in Equation 1, and WN'(Si) is a central wave number of a Raman peak of nanoparticulate silicon included in the negative electrode material in one pixel which is a unit analysis area in a mapping analysis, and wherein the mapping conditions is 5 cm⁻¹ or less [0070, 0074].
Regarding claim 11, the negative electrode material includes a plurality of negative electrode materials, and has composition uniformity between particles according to the following Equation 3:
1.3 ≤ UF(D)
wherein UF(D) is a value obtained by dividing an average doping element
composition between negative electrode material particles by a standard deviation of a doping element composition, based on wt% composition [0083, 0084].
Regarding claim 12, the silicon nanoparticles have an average diameter of 2 to 30 nm [0115].
Regarding claim 14, the one or more doping elements is selected from lithium (Li), sodium (Na), potassium (K), rubidium (Rb), cesium (Cs), beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), aluminum (Al), gallium (Ga), indium (In), tin (Sn), and bismuth (Bi) [0116].
Regarding claim 15, the particles of the negative electrode material have an average diameter in an order of 10° µm to 10¹ µm [0034].
Regarding claim 16, further comprising: a coating layer containing carbon [0121].
Regarding claim 17, a secondary battery comprising the negative electrode material for the secondary battery claim 1.
Regarding the limitations of claims 2-5, 9-10, 13, the instant Specification states:
Example 1
[0134] Si, SiO2, and MgO raw materials were put into a powder mixer at a mole ratio of 6 (Si):4.5 (SiO2):1.5 (MgO), respectively, and then homogeneously mixed to prepare a mixed raw material, and the mixed raw material was pelletized using a mold.
[0135] 26 kg of the pelletized mixed raw material was added to a crucible in a vacuum chamber at 0.1 torr or less, heated to 1,400°C to be vaporized, and then condensed in a collecting plate at 400°C to obtain a magnesium-doped silicon oxide.
[0136] The obtained magnesium-doped silicon oxide was heat-treated in an Ar atmosphere at 830°C for 20 hours to prepare a negative electrode material for a secondary battery in a balk form.
[0137] The thus-prepared bulk-type negative electrode material for a secondary battery was mechanically crushed to an average particle diameter of 3 um to prepare a particulate negative electrode material, and a hydrocarbon gas was used to coat the particulate negative electrode material with 5 wt% of carbon by a CVD process at 850°C to prepare carbon-coated negative electrode material powder.
Lee discloses an almost identical process of:
EXAMPLE
[0125] Each of Si, SiO.sub.2, and MgO raw material was added to the powder mixer at a molar ratio of 6(Si):4.5(SiO.sub.2):1.5(MgO) and homogeneously mixed to prepare a raw material.
[0126] 26 kg of the raw material was placed in a crucible in a vacuum chamber of 0.1 torr or less, heated to 1,400° C. to evaporate, and then condensed in a collecting plate at 400° C. to obtain a magnesium-doped silicon oxide.
[0127] The obtained magnesium-doped silicon oxide was subjected to heat treatment at 900° C. for 15 hours in an Ar atmosphere to prepare a bulk-type negative electrode material for a secondary battery.
[0128] The prepared bulk-type negative electrode material for a secondary battery was mechanically pulverized to have an average particle diameter of 5 μm to prepare a particulate negative electrode material, and 5% by weight of carbon was coated on the resulting particulate negative electrode material through a CVD process at 850° C. using a hydrocarbon gas to prepare a carbon-coated negative electrode material powder.
Hence, the limitations of claims 2-5, 9-10, 13 are met by Lee. MPEP 2112 V states that "once a reference teaching product appearing to be substantially identical is made the basis of a rejection, and the Examiner presents evidence or reasoning tending to show inherency, the burden shifts to the Applicant to show an unobvious difference."
Regarding claim 1, Lee does not disclose a ratio (A₁/A₂) between an area of a first peak (A₁) and an area of a second peak (A₂) is 0.8 to 6, a diffraction angle 2Θ being positioned in a range of 10° to 27.4° in the first peak and being positioned in a range of 28±0.5° in the second peak, in an X-ray diffraction pattern using a CuKa ray. The instant Specification states:
[0064] In another specific example, an intensity ratio (I1/I2) between a maximum intensity of the first peak (I1) and a maximum intensity of the second peak (I2) may be 0.05 to 1.25, specifically 0.05 to 1.05, and more specifically 0.08 to 0.75. Here, the first peak may be derived from an amorphous silicon oxide, and the second peak may be derived from crystalline silicon. Since the negative electrode material of a secondary battery including the amorphous silicon oxide may act as a buffer against volume expansion during secondary battery charging, its capacity retention rate may be excellent.
[0148] FIG. 2 is a drawing illustrating XRD patterns of Examples 1 to 3 and Comparative Example 3, and as seen in the drawing, it was confirmed that the peak of crystalline silicon (111) was observed at about 28Q in all of Examples 1 to 3 and Comparative Example 3, and the peaks in which a diffraction angle 2 Q of Examples 1 to 3 was positioned in a range of 10° to 27.4° appeared broadly, but there was no peak in which the diffraction angle 2 Q of Comparative Example 3 was positioned in a range of 100 to 27.4°. It was found therefrom that Examples 1 to 3 included an amorphous silicon oxide, Comparative Example 3 did not include an amorphous silicon oxide, and thus, since Examples 1 to 3 including the amorphous silicon oxide may act as a buffer against volume expansion during charging of a secondary battery, it may be advantageous in terms of the capacity retention rate of a secondary battery. (emphasis added)
Kim teaches a negative active material comprising silicon and silicon alloy having crystalline phase and an amorphous phase. Si and the Si-metal alloy are present both in the crystalline phase and the amorphous phase, and the ratio of the two phases is controlled to minimize volume expansion and maximize cycle characteristics [0027]. the amount of the amorphous phase may be 30 wt % or more based on the crystalline phase and the amorphous phase combined. The higher the content of the amorphous phase, the better [0028]. As the ratio of the amorphous phase increased, the electric capacity was decreased, but maintenance of capacity was improved and volume expansion was decreased after 50 cycles [0065]. It can be seen that as the ratio of the amorphous phase increases, the cycle characteristics become satisfactory and the volume expansion becomes controllable [0067]. Table 1 discloses the ratio of amorphous phase of 46.6%, 75%, 81%, 89%, and 90%.
It would have been obvious to one of ordinary skilled in the art at the time the invention was made to form the silicon active material of Lee in a mixture of amorphous phase and crystalline phase, as taught by Kim, for the benefit of controlling the maintenance capacity and volume expansion of Lee.
Claim 1 is met by Lee modified by Kim.
Response to Arguments
Applicant’s arguments dated 12/30/2025 are moot in view of the new grounds of rejections.
Pertinent Art
Shin (US 2021/0074995) – [0084-0086]
Oh (US 2018/0090750) – [0073-0074]
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to CYNTHIA KYUNG SOO WALLS whose telephone number is (571)272-8699. The examiner can normally be reached on M-F until 5pm.
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/CYNTHIA K WALLS/ Primary Examiner, Art Unit 1751
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