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 .
Response to Election/Restriction
Applicant’s election without traverse of Invention I, Claims 1-6 and 8, in the reply filed on July 1, 2026 is acknowledged.
Claims 7 and 9-13 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected invention, there being no allowable generic or linking claim.
Claim Rejections - 35 USC § 102
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
(a)(2) the claimed invention was described in a patent issued under section 151, or in an application for patent published or deemed published under section 122(b), in which the patent or application, as the case may be, names another inventor and was effectively filed before the effective filing date of the claimed invention.
Claims 1-8 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Chung et al. (“Carbon-Doped TiNb2O7 Suppresses Amorphization-Induced Capacity Fading”).
With regard to Claim 1, Chung teaches a method for preparing an anode active material comprising providing the first transition metal oxide source and the second transition metal oxide source for a secondary alcohol to prepare a base source, providing a hydrolysis catalyst for the base source and inducing a sol-gel reaction to prepare a transition metal oxide precursor (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; 40 mL of ethylene glycol (99.5%, Daejung Chemical & Metal Co., Ltd.) was poured into a 300 mL roundbottom flask in a nitrogen-filled glove box. Titanium butoxide (97%) and niobium ethoxide (99.999%) purchased from Merck with a molar ratio of 1:2 were added to the flask under stirring. The solution was mixed for 30 min, and an aliquot of acetone (99.95%, Daejung Chemical & Metal Co., Ltd.) in deionized water (1 mL of acetone in 99 mL of deionized water) was then rapidly injected into the solution to initiate the sol−gel reaction).
Chung teaches subjecting the transition metal oxide precursor to heat treatment in a nitrogen environment to prepare an anode-active material containing a transition metal oxide (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; this dried precursor was weighed out into an alumina crucible and placed in a muffle furnace with a temperature elevated to a target temperature (550, 600, 700, 800, and 900 °C) at a ramping rate of 10 °C min−1. Calcination in air at each target temperature was carried out for 2 h).
With regard to Claim 2, Chung teaches the method wherein the transition metal oxide precursor is subjected to heat treatment at a temperature higher than 550 °C (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; this dried precursor was weighed out into an alumina crucible and placed in a muffle furnace with a temperature elevated to a target temperature (550, 600, 700, 800, and 900 °C) at a ramping rate of 10 °C min−1. Calcination in air at each target temperature was carried out for 2 h).
With regard to Claim 3, Chung teaches the method wherein surface roughness (Page 19368, depending on the temperature, surface roughness became more prominent, presumably due to the complete decomposition of the organic part and the rapid grain growth), crystallinity (Page 19367, Figure 2A; As suggested by the appearance of more sharpened, intense diffraction peaks, as temperatures rose, the crystalline nature was enhanced when the calcination temperature increased), carbon atom content (Page 19367, Table 1), and pore size (Page 19360, Figure 2C) of particles of the anode active material being generated are controlled by a temperature at which the transition metal oxide precursor is subjected to heat treatment.
With regard to Claim 4, Chung teaches the method wherein the hydrolysis catalyst is acetone, in which distilled water is further provided to the acetone and thus a sol-gel reaction of the base source is induced by the distilled water (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; The solution was mixed for 30 min, and an aliquot of acetone (99.95%, Daejung Chemical & Metal Co., Ltd.) in deionized water (1 mL of acetone in 99 mL of deionized water) was then rapidly injected into the solution to initiate the sol−gel reaction).
With regard to Claim 5, Chung teaches the method wherein the secondary alcohol is any one of ethylene glycol, diethylene glycol, or triethylene glycol (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; 40 mL of ethylene glycol (99.5%, Daejung Chemical & Metal Co., Ltd.) was poured into a 300 mL roundbottom flask in a nitrogen-filled glove box. Titanium butoxide (97%) and niobium ethoxide (99.999%) purchased from Merck with a molar ratio of 1:2 were added to the flask under stirring), wherein a size of particles of the anode active material is controlled to a nano-size by the secondary alcohol (Page 19367, 3. Results and Discussion; The sol−gel reaction has proven useful in the preparation of this kind of precursor because the structural integrity of the organic moiety that dictates the formation of nanostructures can be sustained without being decomposed).
Chung teaches the method wherein a carbon atom is provided on a surface and an inside of the particles of the anode active material (Page 19367, Table 1; Page 19369, FT-IR analysis revealed that the weight gain from ∼350 °C was associated with the formation of oxygen-functionalized residual carbon. Based on the carbon content of TNO-600, it appeared that the decomposition of the TNO precursor at approximately 300 °C cannot completely burn ethylene glycolate units out of the TNO precursor. Some of it may have turned into oxygen-functionalized carbon).
With regard to Claim 6, Chung teaches the method wherein the first transition metal oxide source is titanium butoxide, and the second transition metal oxide source is niobium ethoxide (Page 19366, 2.1. Synthesis of TiNb2O7 Nanospheres; Titanium butoxide (97%) and niobium ethoxide (99.999%) purchased from Merck with a molar ratio of 1:2 were added to the flask under stirring).
With regard to Claim 8, Chung teaches a method for preparing an anode electrode comprising preparing an anode active material according to the method for preparing the anode active material according to Claim 1, stirring the anode active material and a polymer binder to prepare a slurry, and coating the slurry on a current collector to prepare an anode electrode (Page 19367, 2.3. Electrochemical Analysis; A slurry containing an active material (each TNO sample), carbon black (Super P), and polyvinylidene difluoride binder dissolved in N-methyl-2-pyrrolidone… the slurry was applied and spread evenly onto copper foil, and the resulting film was dried for 12 h in a vacuum oven at 120 °C.).
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.
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.
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 1-3, 6, and 8 are rejected under 35 U.S.C. 103 as being obvious over Lee (“TiNbO4 as a Novel Electrode Material for Lithium Ion Battery”).
With regard to Claim 1, Lee teaches a method for preparing an anode active material (Pages 10-11, Chapter 2. Experimental) comprising preparing a first transition metal oxide source and a second transition metal oxide source (Page 10, 2.1. Chemicals; Titanium (IV) butoxide (97 %)) was purchased from Sigma Aldrich Corp. Niobium (V) ethoxide (99.999 %, metal basis) was purchased from Alfa Aesar).
Lee teaches providing the first transition metal oxide source and the second transition metal oxide source for a secondary alcohol to prepare a base source, providing a hydrolysis catalyst for the base source and inducing a sol-gel reaction to prepare a transition metal oxide precursor (Page 10, 2.2. Synthesis of Titanium Niobium Solid Gel Precursors; The precursors for the synthesis of TiNbO4 were made with a simple sol-gel reaction… 0.4 mL of Titanium butoxide and 0.288 mL of Niobium ethoxide were taken by syringes and dissolved in 25 mL ethanol with 8 mL acetic acid and stirring for 2 hours. Until the ethanol was gradually evaporated, this solution was placed in manipulated air whose humidity is around 50%. The homogeneous gel was finally obtained. The obtained solid gel was then pulverized to fine powder by ball milling). Ethanol is interpreted as the secondary alcohol, and acetic acid is interpreted as the hydrolysis catalyst.
While ethanol and acetic acid are added together in the process, as set forth in MPEP 2144.04.IV.C., the selection of any order of mixing ingredients is prima facie obvious. See In re Burhans, 154 F.2d 690, 69 USPQ 330 (CCPA 1946) (selection of any order of performing process steps is prima facie obvious in the absence of new or unexpected results); In re Gibson, 39 F.2d 975, 5 USPQ 230 (CCPA 1930) (Selection of any order of mixing ingredients is prima facie obvious.)
Lee teaches subjecting the transition metal oxide precursor to heat treatment in a nitrogen environment to prepare an anode-active material containing a transition metal oxide (Page 10, 2.3. Calcination for the Pure TiNbO4; To obtain pure TiNbO4, 0.1 g of titanium niobium precursors was put in ceramic crucible. The powder was calcined at 600 ~ 900 °C for 2 h using a tube furnace in thorough high purity N2 atmosphere (10 °C/min of ramping time)).
With regard to Claim 2, Lee teaches the method wherein the transition metal oxide precursor is subjected to heat treatment at a temperature higher than 550 °C (Page 10, 2.3. Calcination for the Pure TiNbO4; The powder was calcined at 600 ~ 900 °C for 2 h using a tube furnace).
With regard to Claim 3, Lee teaches the method wherein crystallinity (Page 15, 3.2.1. Structure Analysis Using X-Ray Diffraction, the increase in the peak sharpness shows that TiNbO4 which was calcined at higher temperature has more enhanced crystallinity), carbon atom content (Page 23, Table 3), and pore size (Page 20, Figure 9b) of particles of the anode active material being generated are controlled by a temperature at which the transition metal oxide precursor is subjected to heat treatment.
While Lee does not explicitly disclose the method wherein surface roughness of particles are controlled by a temperature at which the transition metal oxide precursor is subjected to heat treatment, the anode active material and disclosed temperature parameters of Lee and of the claimed invention are considered to be substantially identical and thus are expected to have the same properties. See MPEP 2112.01.
The instant specification discloses a preferred embodiment of TiNbO4 formation (Page 37, lines 3-7; when the transition metal oxide precursor is subjected to heat treatment at a temperature of more than 550°C, it can be seen that the chemical composition of the anode active material being generated is TiNbO4).
Lee teaches the formation of TiNbO4 (Page 10, 2.3. Calcination for the Pure TiNbO4; To obtain pure TiNbO4, 0.1 g of titanium niobium precursors was put in ceramic crucible. The powder was calcined at 600 ~ 900 °C for 2 h using a tube furnace in thorough high purity N2 atmosphere (10 °C/min of ramping time)).
Once a reference teaching a 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. "[T]he PTO can require an applicant to prove that the prior art products do not necessarily or inherently possess the characteristics of his [or her] claimed product. Whether the rejection is based on ‘inherency’ under 35 U.S.C. 102, on ‘prima facie obviousness’ under 35 U.S.C. 103, jointly or alternatively, the burden of proof is the same, and its fairness is evidenced by the PTO’s inability to manufacture products or to obtain and compare prior art products." In re Best, 562 F.2d 1252, 1255, 195 USPQ 4380, 483-34 (CCPA 1977)), see MPEP 2112. Applicant has not clearly shown an unobvious difference between the instant invention and the prior art’s product.
With regard to Claim 6, Lee teaches the method wherein the first transition metal oxide source is titanium butoxide, and the second transition metal oxide source is niobium ethoxide (Page 10, 2.1. Chemicals; Titanium (IV) butoxide (97 %)) was purchased from Sigma Aldrich Corp. Niobium (V) ethoxide (99.999 %, metal basis) was purchased from Alfa Aesar).
With regard to Claim 8, Lee teaches a method for preparing an anode electrode comprising preparing an anode active material according to the method for preparing the anode active material according to Claim 1, stirring the anode active material and a polymer binder to prepare a slurry, and coating the slurry on a current collector to prepare an anode electrode (Page 12, 2.5. Electrochemical Measurements; To make the electrode, the bulk TiNbO4 (active material). the conductive agent {Super P), and the polymer binder (polyvinylidene fluoride, PVDF) were well mixed at a weight ratio 7:2:1… The slurry prepared with N-methyl-2-pyrrolidone (NMP) as a solvent was coated evenly on the current collector (Cu foil) using a doctor-blade method to obtain a 6 μm-thick film).
Claim 4 is rejected under 35 U.S.C. 103 as being unpatentable over Lee (“TiNbO4 as a Novel Electrode Material for Lithium Ion Battery”) in view of Chen et al. (“A modified sol–gel method using acetone–ethanol mixed solvent for fast constructing nanometric TiO2 shells”).
With regard to Claim 4, Lee is silent to the method wherein the hydrolysis catalyst is acetone, in which distilled water is further provided to the acetone and thus a sol-gel reaction of the base source is induced by the distilled water, instead teaching the method wherein the hydrolysis catalyst is acetic acid, in which the sol-gel reaction is induced by evaporation of ethanol (Page 10, 2.2. Synthesis of Titanium Niobium Solid Gel Precursors; The precursors for the synthesis of TiNbO4 were made with a simple sol-gel reaction… 0.4 mL of Titanium butoxide and 0.288 mL of Niobium ethoxide were taken by syringes and dissolved in 25 mL ethanol with 8 mL acetic acid and stirring for 2 hours. Until the ethanol was gradually evaporated, this solution was placed in manipulated air whose humidity is around 50%. The homogeneous gel was finally obtained).
Chen teaches the method wherein the hydrolysis catalyst is acetone, in which distilled water is further provided to the acetone and thus a sol-gel reaction of the base source is induced by the distilled water (Page 560, 1. Introduction; we introduce a modified sol–gel method to fast constructing uniform TiO2 shells and fabricate core@TiO2 particles with high dispersibility. The key point of this method is adding acetone, which is known as a cheap and commonly used chemical, into the conventional reaction solution of ethanol/NH3/water/TBOT and controlling it in an appropriate fraction; 2.3. Fabrication of STcsps, Reaction solution for the fabrication STcsps contained ethanol, acetone, NH3, water, TBOT, and SiO2 cores).
Chen notes that the use of acetone improves the reactivity of titanium oxides through decreased agglomeration (Abstract, When acetone was controlled at an optimum fraction in solvent (acetone:ethanol=1.2:1 v/v), it not only increased the hydrolysis rate of precursor (i.e., titanium (IV) tetrabutoxide) and the condensation of titanium oligomers, but also regulated these two sub-reactions of TiO2 formation to be in balance – and thus suppressed the occurrence of agglomeration during TiO2 coating).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the invention for Lee to disclose the method wherein the hydrolysis catalyst is acetone, in which distilled water is further provided to the acetone and thus a sol-gel reaction of the base source is induced by the distilled water, as taught in Chen, as the use of acetone improves the reactivity of titanium oxides through decreased agglomeration.
Claim 5 is rejected under 35 U.S.C. 103 as being unpatentable over Lee (“TiNbO4 as a Novel Electrode Material for Lithium Ion Battery”) in view of Liu et al. (CN109859957A).
With regard to Claim 5, Lee teaches the method wherein a size of particles of the anode active material is controlled to a nano-size by the secondary alcohol and a carbon atom is provided on a surface and an inside of the particles of the anode active material (Page 20, Figure 9, Table 1, Mean pore diameter (nm); Page 23, Table 3; Page 25, This carbon component was from the sol-gel reaction reagent and it was formed by the carbonization process… There is a relationship between the amount of carbon and oxygen vacancy contents: that is the carbon can make oxygen vacancy survive by making Ti-O-C bonding).
Lee is silent to the method wherein the secondary alcohol is any one of ethylene glycol, diethylene glycol, or triethylene glycol, instead teaching the method wherein the secondary alcohol is ethanol (Page 10, 2.2. Synthesis of Titanium Niobium Solid Gel Precursors; The precursors for the synthesis of TiNbO4 were made with a simple sol-gel reaction… 0.4 mL of Titanium butoxide and 0.288 mL of Niobium ethoxide were taken by syringes and dissolved in 25 mL ethanol with 8 mL acetic acid and stirring for 2 hours. Until the ethanol was gradually evaporated, this solution was placed in manipulated air whose humidity is around 50%. The homogeneous gel was finally obtained).
Liu teaches the method wherein the secondary alcohol is ethylene glycol (Claim 5, Paragraph 0018, The organic solvent is one or more of methanol, ethanol, isopropanol, and ethylene glycol).
It would have been obvious to one of ordinary skill in the art to substitute ethanol for ethylene glycol, because these two compounds are disclosed in the reference (Paragraph 0018) as being suitable for use as an organic solvent. One of ordinary skill in the art could have substituted one compound for the other with a predictable result of producing an anode active material. See MPEP 2143.I.B.
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure:
Watanabe (US 2006/0216638 A1) discloses the preparation of a planographic printing plate precursor material prepared with a sol-gel reaction, wherein acetone and ethylene glycol are disclosed as chemicals used for the sol-gel reaction.
Wang (“Titanium Niobium Oxides”) discloses a titanium niobium mixed-phase system prepared via the sol-gel method and characterized as a function of heat treatment temperature.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to ABDUL-RAHMAN YUSUF WALEED SMARI whose telephone number is (571)270-7302. The examiner can normally be reached M-Th 7:30-5, F 7:30-4.
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/ABDUL-RAHMAN YUSUF WALEED SMARI/Examiner, Art Unit 1736
/DANIEL C. MCCRACKEN/Primary Examiner, Art Unit 1736
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