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 Amendment
Examiner notes the following amendments made to the claims:
Claim 1 amended to include subject matter of previously presented claims 4 and 6
Claims 4 and 6 cancelled
New claim 11 added
Response to Arguments
Applicant's arguments filed 11/25/2025 regarding the rejection of claim 1 under 35 USC 103 have been fully considered but they are not persuasive. Specifically, examiner finds that the previously applied prior art still meets the limitations of previously presented claims 4 and 6, which have now been incorporated into claim 1. Examiner will respond to applicant arguments in order:
First, applicant argues that Lee does not teach the claimed range of previously presented claim 4 because it teaches the percentage of carbon in coating layer based on the total weight of silicon based carbon composite, rather than the total weight of negative electrode active material. Examiner notes this argument, but would like to point out example 1, paragraph [0259] of Lee, which teaches that the silicon-based-carbon composite is used as the negative electrode active material (“A negative electrode and a battery (coin cell) comprising the silicon-based-carbon composite (composite E1) of a core-shell structure as a negative electrode active material were fabricated.” Lee [0259]). Therefore, the amount of carbon in the silicon-based carbon composite is the same as the amount of carbon in the negative electrode active material, and thus the range taught by Lee anticipates the claimed range.
Second, applicant argues that Lee II (referred to as Lee ‘161 in rejection below) does not teach the claimed amount of single-walled carbon nanotubes, as Lee II teaches a weight percentage of SWCNTs in the context of a negative electrode active material slurry, rather than a total weight of the negative electrode active material. This argument is not persuasive, as the only additional material used in the slurry is water, (“97.45 wt % of artificial graphite, 1.5 wt % of styrene butadiene rubber, 0.05 wt % of an SWCNT conductive agent of Table 1, and 1 wt % of carboxymethyl cellulose were mixed in water to prepare negative active material slurry.” Lee II [0115]) and the method involves drying the slurry onto the electrode foil, which would remove the excess water anyhow, and the ratios of negative electrode active material contents would remain the same. The slurry is just a method of applying the active material, but the weight ratios taught for the slurry would also correspond to those of the active material itself. (“After disposing a Cu foil on a magnet having an intensity of a magnetic field of 3,000 Gauss, the negative active material slurry was coated on the Cu foil, exposed to the magnetic field for 9 seconds, while the Cu foil was being moved, and then, dried and compressed to manufacture a negative electrode having electrode plate density of 1.45 g/cc and a single surface loading level (L/L) of 6.2 mg/cm.sup.2.” Lee II [0116]).
Lastly, applicant argues that there would not be sufficient motivation to combine the teachings of Lee with Jo and Son as there is no mention of the specific two-layer configuration with an outer graphene layer and SWCNTs and the advantages therefrom. Examiner does not find this argument persuasive, as there are reasons provided in the prior art of the advantages of both an outer layer containing graphene and the usage of SWCNTs, both within the claimed weight ranges and both in regards to a negative electrode active material. Thus, examiner finds that there was proper motivation for one skilled in the art and the rejections are maintained.
Based on the above arguments, examiner does not find applicant arguments and the rejection of claim 1 remains in place, other than claim 1 now depending further on Lee II, to account for the amendment of the claim. Since there are no further arguments regarding the dependent claims, they remain in place and unchanged other than now depending on Lee II.
Regarding new claim 11, all of the ranges provided in the new claim are met by previously applied prior art, and therefore the claim is rejected in view of the same references as claim 1.
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claim(s) 1-3, 5, 7-11 is/are rejected under 35 U.S.C. 103 as being unpatentable over Lee (US 20230238514 A1) in view of Jo (US 20130248772 A1), further in view of Son (US 20150380728 A1) and further in view of Lee (US 20190334161 A1), hereinafter referred to as Lee ‘161 .
Regarding claim 1, Lee teaches the following elements:
A negative electrode, comprising: a current collector; and a negative electrode active material layer on at least one surface of the current collector, wherein the negative electrode active material layer comprises: (“The negative electrode may be composed of a negative electrode composition only or may be composed of a negative electrode current collector and a negative electrode composition layer (negative electrode active material layer) supported thereon.” Lee [0235])
1) a negative electrode active material comprising a Mg- containing silicon oxide, a carbon coating layer surrounding the surface of the Mg- containing silicon oxide and a graphene coating layer surrounding the surface of the carbon coating layer, (“an embodiment of the present invention provides a silicon-based-carbon composite having a core-shell structure, wherein the core comprises silicon, a silicon oxide compound, and magnesium silicate, and the shell comprises at least two carbon layers comprising a first carbon layer and a second carbon layer, wherein the second carbon layer is reduced graphene oxide.” Lee [0014])
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3) a binder, (“In addition, the negative electrode composition and the positive electrode composition may each further comprise a conductive agent and a binder.” Lee [0235])
wherein an amount of the graphene coating layer is 0.5 wt% to 10 wt % based on a total weight of the negative electrode active material. (“The content of carbon (C) in the second carbon layer may preferably be 3% by weight to 20% by weight, more preferably, 3% by weight to 15% by weight, even more preferably, 3% by weight to 10% by weight, based on the total weight of the silicon-based-carbon composite.” Lee [0097] and “The second carbon layer according to an embodiment of the present invention may be reduced graphene oxide having particularly high electrical conductivity.” Lee [0116] and “A negative electrode and a battery (coin cell) comprising the silicon-based-carbon composite (composite E1) of a core-shell structure as a negative electrode active material were fabricated.” Lee [0259])
The examiner takes note of the fact that the prior art range of 3-20 wt % for the amount of graphene based on the total weight of the negative electrode active material layer overlaps the claimed range of 0.5-10 wt % for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Lee is silent on the following elements of claim 1:
wherein the graphene present in the graphene coating layer has a D/G band intensity ratio of 0.8 to 1.5, and the D/G band intensity ratio of the graphene is defined as an average value of a ratio of a maximum peak intensity of D band at 1360 ± 50 cm' based on a maximum peak intensity of G band at 1580 ± 50 cm1, as determined by Raman spectroscopy of graphene.
2) a conductive material comprising single-walled carbon nanotubes (SWCNTs),
The negative electrode according to claim 1, wherein an amount of the single-walled carbon nanotubes is 0.01 wt % to 0.06 wt% based on a total weight of the negative electrode active material layer.
Jo teaches the following elements of claim 1 that are not explicitly taught by Lee:
2) a conductive material comprising single-walled carbon nanotubes (SWCNTs), electrode (“The first and second carbon nano conductive agents may include single-walled carbon nanotubes (SWNTs), multi-walled carbon nanotubes (MTWNTs), cup-stack type MTWNTs or mixtures thereof. “ Jo [0016])
Jo and Lee are considered to be analogous because they are both within the same field of electrode materials containing carbonaceous materials. Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to modify the carbon nanotubes taught by Lee (“The carbon-based negative electrode material may comprise, for example, at least one selected from the group consisting of natural graphite, synthetic graphite, soft carbon, hard carbon, mesocarbon, carbon fibers, carbon nanotubes,” Lee [0230]) to be specifically SWCNTs, as taught by Jo. This would be obvious as it would only require a simple substitution of one known material with another, and the simple substitution of one known element for another is likely to be obvious when predictable results are achieved. (see MPEP § 2143, B.).
Lee and Jo are both silent on the following elements of claim 1:
wherein the graphene present in the graphene coating layer has a D/G band intensity ratio of 0.8 to 1.5, and the D/G band intensity ratio of the graphene is defined as an average value of a ratio of a maximum peak intensity of D band at 1360 ± 50 cm' based on a maximum peak intensity of G band at 1580 ± 50 cm1, as determined by Raman spectroscopy of graphene.
The negative electrode according to claim 1, wherein an amount of the single-walled carbon nanotubes is 0.01 wt % to 0.06 wt% based on a total weight of the negative electrode active material layer.
Son teaches the following elements of claim 1 that are not found in Lee or Jo:
wherein the graphene contained in the graphene coating layer has a D/G band intensity ratio of 0.8-1.5, and the D/G band intensity ratio of the graphene is defined as an average value of the ratio of the maximum peak intensity of D band at 1360 ± 50 cm' based on the maximum peak intensity of G band at 1580 ± 50 cm1, as determined by Raman spectroscopy of graphene. (“The coating of graphene on the silicon oxide (SiOx) by vapor deposition may form a coating layer having high crystallinity on the composite.” Son [0148]) and “The graphene may have a degree of crystallinity of about 0.5 to about 1.5, for example, about 1.055 to about 1.146, or about 1.06 to about 1.14. The degree of crystallinity (or degree of disordering of graphene crystals) of the graphene may be obtained by measuring an intensity ratio of D peak to G peak (D/G) in a Raman spectra of the composite.” Son [0086-0087])
The examiner takes note of the fact that the prior art range of ------0.5-1.5 for the D/G ratio in the graphene coating encompasses the claimed range of 0.8-1.5 for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Son and Lee are considered to be analogous because they are both within the same field of graphene-coated silicon oxide materials to be used in anodes of secondary batteries. Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to modify the graphene coating of Lee to have the specific D/G ratio of Son in order to improve conductivity without requiring structural change (“The coating of graphene on the silicon oxide (SiOx) by vapor deposition may form a coating layer having high crystallinity on the composite. When the composite having such a highly-crystalline coating layer is used as an anode active material, the anode active material may have improved conductivity without structural change.” Son [0148]). Additionally, both inventions use a graphene coating, and therefore it would only require a simple substitution to replace that of Lee with that of Son, and the simple substitution of one known element for another is likely to be obvious when predictable results are achieved. (see MPEP § 2143, B.).
By using the graphene coating layer of Son in place of that of Lee, the additional limitations of claims 2-3, 5, 8-10 would all be met without requiring any further modification or motivation.
Lee, Son, and Jo are silent on the following elements of claim 1:
The negative electrode according to claim 1, wherein an amount of the single-walled carbon nanotubes is 0.01 wt % to 0.06 wt% based on a total weight of the negative electrode active material layer.
However, Lee ‘161 teaches all of the elements of claim 6 that are not found in modified Lee:
The negative electrode according to claim 1, wherein an amount of the single-walled carbon nanotubes is 0.01 wt % to 0.06 wt% based on a total weight of the negative electrode active material layer. (“97.45 wt % of artificial graphite, 1.5 wt % of styrene butadiene rubber, 0.05 wt % of an SWCNT conductive agent of Table 1, and 1 wt % of carboxymethyl cellulose were mixed in water to prepare negative active material slurry.” Lee [0115])
Lee ‘161 is considered to be analogous to Lee because they are both within the same field of negative electrode active materials. Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to modify the conductive agent of Lee to be the specific ratio of Lee ‘161 (0.05 wt % of the total) as this proportion is known in the art and was shown in Lee ‘161 to have a higher capacity retention and lower are specific resistance than comparative examples (Lee ‘161 figures 6 and 7).
Regarding claim 2, modified Lee teaches all of the elements of claim 1, as shown above. Lee is silent on the following elements of claim 2:
The negative electrode according to claim 1, wherein the D/G band intensity ratio of the graphene present in the graphene coating layer ranges from 0.8 to 1.4.
However, Son teaches all of the elements of claim 2 that are not found in Lee:
The negative electrode according to claim 1, wherein the D/G band intensity ratio of the graphene present in the graphene coating layer ranges from 0.8 to 1.4. (“The coating of graphene on the silicon oxide (SiOx) by vapor deposition may form a coating layer having high crystallinity on the composite.” Son [0148]) and “The graphene may have a degree of crystallinity of about 0.5 to about 1.5, for example, about 1.055 to about 1.146, or about 1.06 to about 1.14. The degree of crystallinity (or degree of disordering of graphene crystals) of the graphene may be obtained by measuring an intensity ratio of D peak to G peak (D/G) in a Raman spectra of the composite.” Son [0086-0087])
The examiner takes note of the fact that the prior art range of ------0.5-1.5 for the D/G ratio in the graphene coating encompasses the claimed range of 0.8-1.4 for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Regarding claim 3, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches all of the additional elements of claim 3:
The negative electrode according to claim 1, wherein the Mg-containing silicon oxide comprises 4 wt % to 15 wt % of Mg. (“Meanwhile, the content of magnesium (Mg) in the silicon-based-carbon composite may be 0.2% by weight to 15% by weight, 0.2% by weight to 10% by weight, or 0.2% by weight to 8% by weight, based on the total weight of the silicon-based-carbon composite.” Lee [0034])
The examiner takes note of the fact that the prior art range of 0.2-15 wt% for Mg present in the silicon oxide containing composite material encompasses the claimed range of 4-15 wt% for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Regarding claim 5, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches all of the additional elements of claim 5:
The negative electrode according to claim 1, wherein an amount of the carbon coating layer is 0.5 wt % to 10 wt % based on a total weight of the negative electrode active material. (“Meanwhile, the total content of carbon (C) in the first carbon layer and the second carbon layer may be 5% by weight to 50% by weight based on the total weight of the silicon-based-carbon composite.” Lee [0095])
The examiner takes note of the fact that the prior art range of 5-50 wt % for the amount of carbon based on the total weight of the negative electrode active material layer overlaps the claimed range of 0.5-10 wt % for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Regarding claim 7, modified Lee teaches all of the elements of claim 1, as shown above. Lee and Son are silent on the following elements of claim 7:
The negative electrode according to claim 1, wherein the conductive material further comprises at least one of carbon black, acetylene black, ketjen black, carbon nanofibers, channel black, furnace black, lamp black, thermal black, carbon fibers, metal fibers, fluorocarbon, metal powder, conductive whisker, conductive metal oxide, or polyphenylene derivative.
However, Jo teaches all of the elements of claim 7 that are not found in Lee:
The negative electrode according to claim 1, wherein the conductive material further comprises at least one of carbon black, acetylene black, ketjen black, carbon nanofibers, channel black, furnace black, lamp black, thermal black, carbon fibers, metal fibers, fluorocarbon, metal powder, conductive whisker, conductive metal oxide, or polyphenylene derivative. (“The first and second carbon nano conductive agents may include single -walled carbon nanotubes (SWNTs), multi-walled carbon nanotubes (MTWNTs), cup-stack type MTWNTs or mixtures thereof. The secondary battery may further include an additional conductive agent selected from the group consisting of natural graphite, artificial graphite, carbon black, acetylene black, ketjen black, carbon fiber, copper, nickel, aluminum, silver, polyphenylene derivatives and combinations thereof, and a mixing ratio of the first and second carbon nano conductive agents and the additional conductive agent may range from 1:1 to 1:10” Jo [0016-0017])
Jo is analogous to Lee because they are both within the same field of negative electrode active materials, as shown above for claim 1. Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to modify the conductive material of Lee to comprise both SWCNTs and a second conductive agent, as taught in Jo, in order to reduce the electrical resistance and improve the binding strength of the active material (“the conductive agent for an electrode of a secondary battery may include a first carbon nano conductive agent which has a first diameter and is dispersed on a surface of an active material and a second carbon nano conductive agent which has a second diameter and is positioned between molecules of active material and forms a micro network of electrical conduction. Such conductive agent reduces the electrical resistance of the active material and improves the binding strength of the active material.” Jo [0027]). Additionally, the combination of conductive agents taught by Jo can improve discharge characteristics (“In addition, the conductive agent for the electrode of a secondary battery constructed with an embodiment of the present invention serves to perform a conducting function like the contemporary conductive agent and improves the binding strength between active materials and between an active material and a current collector, thereby improving the high-rate discharge characteristic and the cycle life characteristics.” Jo [0028]).
Regarding claim 8, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches all of the additional elements of claim 8:
The negative electrode according to claim 1, wherein the negative electrode active material layer further comprises a carbonaceous active material. (“The negative electrode active material according to an embodiment may comprise the silicon-based-carbon composite. Specifically, the silicon-based-carbon composite employed in the negative electrode active material has a core-shell structure, wherein the core comprises silicon, a silicon oxide compound, and magnesium silicate, and the shell comprises at least two carbon layers comprising a first carbon layer and a second carbon layer, wherein the second carbon layer may be reduced graphene oxide… In addition, the negative electrode active material may further comprise a carbon-based negative electrode material.” Lee [0228-0229])
Regarding claim 9, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches all of the additional elements of claim 9:
The negative electrode according to claim 8, wherein the carbonaceous active material comprises at least one of artificial graphite, natural graphite, graphitizable carbon fibers, graphitizable mesocarbon microbeads, petroleum cokes, baked resin, carbon fibers, or pyrolyzed carbon. (“The negative electrode active material may be used as a mixture of the silicon-based-carbon composite and the carbon-based negative electrode material. In such an event, the electrical resistance of the negative electrode active material can be reduced, while the expansion stress involved in charging can be relieved at the same time. The carbon-based negative electrode material may comprise, for example, at least one selected from the group consisting of natural graphite, synthetic graphite, soft carbon, hard carbon, mesocarbon, carbon fibers, carbon nanotubes, pyrolytic carbon, coke, glass carbon fibers, sintered organic high molecular compounds, and carbon black.” Lee [0230])
Regarding claim 10, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches all of the additional elements of claim 10:
A lithium secondary battery comprising the negative electrode as defined in claim 1. (“The present invention may provide a negative electrode comprising the negative electrode active material and a secondary battery comprising the same.” Lee [0233])
Regarding claim 11, modified Lee teaches all of the elements of claim 1, as shown above. Lee teaches the following elements of claim 11:
an amount of the graphene coating layer is 1.0 wt% to 9.7 wt% based on a total weight of the negative electrode active material, (“The content of carbon (C) in the second carbon layer may preferably be 3% by weight to 20% by weight, more preferably, 3% by weight to 15% by weight, even more preferably, 3% by weight to 10% by weight, based on the total weight of the silicon-based-carbon composite.” Lee [0097] and “The second carbon layer according to an embodiment of the present invention may be reduced graphene oxide having particularly high electrical conductivity.” Lee [0116] and “A negative electrode and a battery (coin cell) comprising the silicon-based-carbon composite (composite E1) of a core-shell structure as a negative electrode active material were fabricated.” Lee [0259])
The examiner takes note of the fact that the prior art range of 3-20 wt % for the amount of graphene based on the total weight of the negative electrode active material layer overlaps the claimed range of 1-9.7 wt % for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Lee is silent on the following elements of claim 11:
The negative electrode according to claim 1, wherein the graphene present in the graphene coating layer has a D/G band intensity ratio of 0.8 to 1.32,
and an amount of the single-walled carbon nanotubes is 0.04 wt% to 0.06 wt% based on a total weight of the negative electrode active material layer.
Son teaches the following elements of claim 11:
The negative electrode according to claim 1, wherein the graphene present in the graphene coating layer has a D/G band intensity ratio of 0.8 to 1.32, (“The coating of graphene on the silicon oxide (SiOx) by vapor deposition may form a coating layer having high crystallinity on the composite.” Son [0148]) and “The graphene may have a degree of crystallinity of about 0.5 to about 1.5, for example, about 1.055 to about 1.146, or about 1.06 to about 1.14. The degree of crystallinity (or degree of disordering of graphene crystals) of the graphene may be obtained by measuring an intensity ratio of D peak to G peak (D/G) in a Raman spectra of the composite.” Son [0086-0087])
The examiner takes note of the fact that the prior art range of ------0.5-1.5 for the D/G ratio in the graphene coating encompasses the claimed range of 0.8-1.32 for the same parameter. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315 F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Lee and Son are silent on the following elements of claim 11:
and an amount of the single-walled carbon nanotubes is 0.04 wt% to 0.06 wt% based on a total weight of the negative electrode active material layer.
However, Lee II teaches all of the elements of claim 11 not found in Lee or Son:
and an amount of the single-walled carbon nanotubes is 0.04 wt% to 0.06 wt% based on a total weight of the negative electrode active material layer. (“97.45 wt % of artificial graphite, 1.5 wt % of styrene butadiene rubber, 0.05 wt % of an SWCNT conductive agent of Table 1, and 1 wt % of carboxymethyl cellulose were mixed in water to prepare negative active material slurry.” Lee [0115]. The 0.05% by weight of SWCNT anticipates the claimed range, see above arguments for why the composition of the slurry is considered analogous to the composition of the negative electrode active material.)
Conclusion
The following references were found in an updated search and considered relevant, but not included in rejection as the limitations were already met by the previously applied prior art:
Ikenuma (US 20150349345 A1) –teaches a graphene coating for a negative electrode active material that meets the claimed weight ratio (“Here, the amount of graphene oxide is set to higher than or equal to 0.1 wt % and lower than or equal to 10 wt %, preferably higher than or equal to 0.1 wt % and lower than or equal to 5 wt %, further preferably higher than or equal to 0.2 wt % and lower than or equal to 2 wt %, still further preferably higher than or equal to 0.2 wt % and lower than or equal to 1 wt % with respect to the total weight of the mixture of the graphene oxide, the active material, the conductive additive, and the binder.” Ikenuma [0104] and “The graphene flakes 104 are schematically shown by heavy lines in FIG. 1C but are actually thin films each having a thickness corresponding to the thickness of a single layer or a multiple layer of carbon molecules. The plurality of graphene flakes 104 are formed in such a way as to wrap, coat, or be adhered to a plurality of the active material particles 103, so that the graphene flakes 104 make surface contact with the active material particles 103. “ Ikenuma [0063])
THIS ACTION IS MADE FINAL. Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to BENJAMIN ELI KASS-MULLET whose telephone number is (571)272-0156. The examiner can normally be reached Monday-Friday 8:30am-6pm except for the first Friday of bi-week.
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/BENJAMIN ELI KASS-MULLET/Examiner, Art Unit 1752
/NICHOLAS A SMITH/Supervisory Primary Examiner, Art Unit 1752