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 .
Claims 1-15 are pending
Double Patenting
The nonstatutory double patenting rejection is based on a judicially created doctrine grounded in public policy (a policy reflected in the statute) so as to prevent the unjustified or improper timewise extension of the “right to exclude” granted by a patent and to prevent possible harassment by multiple assignees. A nonstatutory double patenting rejection is appropriate where the conflicting claims are not identical, but at least one examined application claim is not patentably distinct from the reference claim(s) because the examined application claim is either anticipated by, or would have been obvious over, the reference claim(s). See, e.g., In re Berg, 140 F.3d 1428, 46 USPQ2d 1226 (Fed. Cir. 1998); In re Goodman, 11 F.3d 1046, 29 USPQ2d 2010 (Fed. Cir. 1993); In re Longi, 759 F.2d 887, 225 USPQ 645 (Fed. Cir. 1985); In re Van Ornum, 686 F.2d 937, 214 USPQ 761 (CCPA 1982); In re Vogel, 422 F.2d 438, 164 USPQ 619 (CCPA 1970); In re Thorington, 418 F.2d 528, 163 USPQ 644 (CCPA 1969).
A timely filed terminal disclaimer in compliance with 37 CFR 1.321(c) or 1.321(d) may be used to overcome an actual or provisional rejection based on nonstatutory double patenting provided the reference application or patent either is shown to be commonly owned with the examined application, or claims an invention made as a result of activities undertaken within the scope of a joint research agreement. See MPEP § 717.02 for applications subject to examination under the first inventor to file provisions of the AIA as explained in MPEP § 2159. See MPEP § 2146 et seq. for applications not subject to examination under the first inventor to file provisions of the AIA . A terminal disclaimer must be signed in compliance with 37 CFR 1.321(b).
The filing of a terminal disclaimer by itself is not a complete reply to a nonstatutory double patenting (NSDP) rejection. A complete reply requires that the terminal disclaimer be accompanied by a reply requesting reconsideration of the prior Office action. Even where the NSDP rejection is provisional the reply must be complete. See MPEP § 804, subsection I.B.1. For a reply to a non-final Office action, see 37 CFR 1.111(a). For a reply to final Office action, see 37 CFR 1.113(c). A request for reconsideration while not provided for in 37 CFR 1.113(c) may be filed after final for consideration. See MPEP §§ 706.07(e) and 714.13.
The USPTO Internet website contains terminal disclaimer forms which may be used. Please visit www.uspto.gov/patent/patents-forms. The actual filing date of the application in which the form is filed determines what form (e.g., PTO/SB/25, PTO/SB/26, PTO/AIA /25, or PTO/AIA /26) should be used. A web-based eTerminal Disclaimer may be filled out completely online using web-screens. An eTerminal Disclaimer that meets all requirements is auto-processed and approved immediately upon submission. For more information about eTerminal Disclaimers, refer to www.uspto.gov/patents/apply/applying-online/eterminal-disclaimer.
Claims 1-9 and 11-15 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1, 4-9, and 11-15 of copending Application No. 18/989,948. Although the claims at issue are not identical, they are not patentably distinct from each other because of the following.
Regarding instant claims 1-4, reference claim 5 recites silica particles having an average pore volume of nanoscale pores of 5.4 nm³ or less and, through its dependence from reference claim 1, an average pore volume of atomic-scale pores of 0.35 nm³ or more. Instant claim 1 recites an average pore volume of nanoscale pores of 5.3 nm³ or less, which overlaps and is slightly narrower than the nanoscale-pore range of reference claim 5. Instant claim 2 further limits the average pore volume of nanoscale pores to 4.0 nm³ or less, and instant claim 3 further requires the average pore volume of nanoscale pores to be 1.5 nm³ or more, thereby defining narrower ranges within the nanoscale-pore range encompassed by reference claim 5. Instant claim 4 further requires an average pore volume of atomic-scale pores of 0.33 nm³ or more, which overlaps the atomic-scale-pore limitation of 0.35 nm³ or more recited through reference claim 5. The respective claimed ranges therefore overlap or define narrower selections within the subject matter of the reference claims, and selection of such overlapping or narrower ranges would have been obvious absent evidence of criticality or unexpected results. See MPEP § 2144.05.
Regarding instant claim 5, reference claim 4 recites an average pore volume of atomic-scale pores of 0.80 nm³ or less, while reference claim 5 recites an average pore volume of nanoscale pores of 5.4 nm³ or less. It would have been obvious to apply both pore-volume characteristics to the same silica particles because the reference claims recite each characteristic for the same silica-particle subject matter, and the slight difference between the instant nanoscale upper limit of 5.3 nm³ and the reference upper limit of 5.4 nm³ constitutes an overlapping range.
Regarding instant claims 6-9, reference claims 6-9 respectively recite the same additional limitations concerning a nitrogen-gas-adsorption pore volume of 0.0070 cm³/g or less, a refractive index of 1.390 or more, a metal impurity content of 5 ppm or less, and a tetraalkoxysilane condensate as a main component. It would have been obvious to apply the nanoscale pore-volume characteristic of reference claim 5 to the silica particles having the respective characteristics of reference claims 6-9 because the reference claims concern characteristics of the same silica-particle subject matter.
Regarding instant claims 11-15, reference claims 11-15 respectively recite the same silica sol, polishing composition, polishing method, method for producing a semiconductor wafer, and method for producing a semiconductor device. It would have been obvious to use silica particles having the nanoscale pore-volume characteristic of reference claim 5 in the silica-particle subject matter in those compositions and methods.
This is a provisional nonstatutory double patenting rejection because the patentably indistinct claims have not in fact been patented.
Claim 10 is provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 5 and 10 of copending Application No. 18/989,948 in view of Sumiya et al. (JP 2021-116225 A).
Reference claim 10 recites a method for producing silica particles by carrying out a hydrolysis reaction and a condensation reaction of an alkoxysilane for 600 minutes or less. Reference claim 5 further recites silica particles having an average pore volume of nanoscale pores of 5.4 nm³ or less. Instant claim 10 requires producing silica particles having an average nanoscale pore volume of 5.3 nm³ or less by carrying out a hydrolysis reaction and a condensation reaction of an alkoxysilane at 40°C or higher. The 5.3 nm³-or-less range lies within and overlaps the 5.4 nm³-or-less range of reference claim 5, and selection of the overlapping range would have been obvious. See MPEP § 2144.05.
Sumiya teaches producing silica particles by hydrolyzing and condensing tetraalkoxysilane and further teaches carrying out the hydrolysis reaction and condensation reaction at a reaction temperature of 40°C or higher.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to perform the hydrolysis and condensation reactions of the method of reference claims 5 and 10 at 40°C or higher because Sumiya teaches the claimed temperature condition for the same type of alkoxysilane hydrolysis and condensation reaction used to produce silica particles. One of ordinary skill in the art would have had a reasonable expectation of successfully applying the known reaction-temperature condition to the reference method. See MPEP § 2143(G). The additional 600-minute-or-less limitation of reference claim 10 does not patentably distinguish instant claim 10 because instant claim 10 is broader in that respect and encompasses performance of the reference method within that time period.
This is a provisional nonstatutory double patenting rejection because the patentably indistinct claims have not in fact been patented.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
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 1-5, 8-9, and 11-15 are rejected under 35 U.S.C. 103 as being unpatentable over Kyotani et al. (WO 2020/171140 A1) in view of Kajcsos et al., On the peculiarities of positron annihilation features in silicalite-1 and Y-zeolites, Radiation Physics and Chemistry, Vol. 58, pages 709-714 (2000).
Regarding claim 1, Kyotani teaches silica particles (teaching that colloidal silica is widely used as abrasive particles in polishing compositions and may be produced by hydrolysis and condensation of alkoxysilane; paragraph [0003]).
Kyotani does not expressly teach wherein an average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 5.3 nm³ or less.
Kajcsos teaches positron annihilation spectroscopy for characterizing internal voids and channels of a siliceous framework (teaching silicalite-1 having an MFI structure with 96 SiO₂ per unit cell and studying the material as a micro-crystalline powder; page 710, Section 2, Experimental). Kajcsos further teaches that the positron lifetime spectra include a 10-90 ns component attributed to o-Ps decaying in internal channels of the zeolite and reports for defected silicalite-1 sample B a corresponding lifetime τ3 of 20.8 ns; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1.
The instant specification explains that the average pore volume of nanoscale pores is determined from the positron lifetime measured by positron annihilation spectroscopy and provides the equations for determining average nanoscale-pore radius R and average pore volume V; paragraphs [0019]-[0023]. Applying Kajcsos’s τ3 value of 20.8 ns to those equations gives a calculated average nanoscale-pore radius of approximately 0.954 nm and a calculated average nanoscale-pore volume of approximately 3.63 nm³, which is less than the claimed 5.3 nm³.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the silica particles of Kyotani to evaluate their internal nanoscale pore structure using the positron annihilation spectroscopy technique taught by Kajcsos because Kyotani teaches that the internal structure of silica particles affects mechanical strength and polishing characteristics and that the internal structure may be controlled by adjusting the hydrolysis and condensation reaction conditions and subsequent treatment; paragraphs [0006], [0013]-[0017], and one of ordinary skill in the art would know to control the d value to be as much or as little as necessary to achieve the desired result and it is not inventive to discover the optimum or workable ranges by routine experimentation, see MPEP 2144.05. Further, Kyotani further explains that its d value represents spacing between aligned planes across a gap in amorphous silica; paragraph [0014]. Kajcsos teaches positron annihilation spectroscopy as a known technique for characterizing internal voids and channels in siliceous materials. Accordingly, one of ordinary skill in the art seeking to improve the mechanical strength and polishing characteristics of Kyotani’s silica particles would have had reason to optimize the internal silica structure through Kyotani’s disclosed reaction and treatment conditions while using Kajcsos’s positron annihilation spectroscopy technique as an additional means of evaluating internal void dimensions. Such characterization would have provided a predictable means of comparing the internal void structures of silica particles obtained under different processing conditions. See MPEP §§ 2143(G) and 2144.05(II).
Regarding claim 2, modified Kyotani teaches the limitations of claim 1 as discussed above.
Regarding the limitation “wherein the average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 4.0 nm³ or less,” Kajcsos reports for defected silicalite-1 sample B a positron lifetime τ3 of 20.8 ns for the component attributed to o-Ps decaying in internal channels of the zeolite; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1. Applying Kajcsos’s τ3 value of 20.8 ns to the nanoscale-pore equations set forth in paragraphs [0019]-[0023] of the instant specification gives a calculated average nanoscale-pore volume of approximately 3.63 nm³, thereby satisfying the claimed 4.0 nm³-or-less limitation.
Regarding claim 3, modified Kyotani teaches the limitations of claim 1 as discussed above.
Regarding the limitation “wherein the average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 1.5 nm³ or more,” Kajcsos reports for defected silicalite-1 sample B a positron lifetime τ3 of 20.8 ns for the component attributed to o-Ps decaying in internal channels of the zeolite; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1. Applying Kajcsos’s τ3 value of 20.8 ns to the nanoscale-pore equations set forth in paragraphs [0019]-[0023] of the instant specification gives a calculated average nanoscale-pore volume of approximately 3.63 nm³, thereby satisfying the claimed 1.5 nm³-or-more limitation and the 5.3 nm³-or-less limitation of claim 1.
Regarding claim 4, modified Kyotani teaches the limitations of claim 1 as discussed above.
Regarding the limitation “wherein an average pore volume of atomic-scale pores as measured by positron annihilation spectroscopy is 0.33 nm³ or more,” Kajcsos reports for defected silicalite-1 sample B a positron lifetime τ2 of 4.66 ns and explains that the corresponding lifetime represents a void having a radius of approximately 0.46 nm; page 711, Table 1; page 711, Section 3, Results and discussion, right column, first paragraph. Applying the atomic-scale-pore-volume relationship set forth in paragraphs [0026]-[0030] of the instant specification to Kajcsos’s approximately 0.46 nm radius gives a calculated average atomic-scale-pore volume of approximately 0.41 nm³, thereby satisfying the claimed 0.33 nm³-or-more limitation.
Regarding claim 5, modified Kyotani teaches the limitations of claim 1 as discussed above.
Regarding the limitation “wherein the average pore volume of atomic-scale pores as measured by positron annihilation spectroscopy is 0.80 nm³ or less,” Kajcsos reports for defected silicalite-1 sample B a positron lifetime τ2 of 4.66 ns and explains that the corresponding lifetime represents a void having a radius of approximately 0.46 nm; page 711, Table 1; page 711, Section 3, Results and discussion, right column, first paragraph. Applying the atomic-scale-pore-volume relationship set forth in paragraphs [0026]-[0030] of the instant specification to Kajcsos’s approximately 0.46 nm radius gives a calculated average atomic-scale-pore volume of approximately 0.41 nm³, thereby satisfying the claimed 0.80 nm³-or-less limitation.
Regarding claim 8, modified Kyotani teaches the limitations of claim 1 as discussed above.
Kyotani further teaches wherein a content of metal impurities is 5 ppm or less (teaching that the metal impurity content of the silica particles is preferably 5 ppm or less and more preferably 2 ppm or less; paragraph [0037]; further teaching that a metal impurity content of 5 ppm or less may be obtained by producing the silica particles through hydrolysis and condensation reactions using alkoxysilane as the main raw material; paragraph [0040]).
Regarding claim 9, modified Kyotani teaches the limitations of claim 1 as discussed above.
Kyotani further teaches wherein a tetraalkoxysilane condensate is a main component (teaching that the silica particles preferably contain an alkoxysilane condensate as the main component and more preferably contain a tetraalkoxysilane condensate as the main component, wherein “main component” means that the component accounts for 50 mass% or more of all components constituting the silica particles; paragraph [0043]). Kyotani further teaches examples of tetraalkoxysilane condensates including tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, and tetraisopropoxysilane condensates; paragraph [0044].
Regarding claim 11, modified Kyotani teaches the limitations of claim 1 as discussed above.
Kyotani further teaches a silica sol comprising the silica particles (teaching a silica sol containing the disclosed silica particles; paragraph [0010]; further teaching that the silica sol of the embodiment preferably contains the silica particles of the embodiment and a solvent or dispersion medium; paragraph [0058]).
Regarding claim 12, modified Kyotani teaches the limitations of claim 11 as discussed above.
Kyotani further teaches a polishing composition comprising the silica sol (teaching that the polishing composition of the embodiment contains the disclosed silica sol and preferably further contains a water-soluble polymer; paragraph [0069]).
Regarding claim 13, modified Kyotani teaches the limitations of claim 12 as discussed above.
Kyotani further teaches a polishing method comprising polishing using the polishing composition (teaching a polishing method using the disclosed polishing composition, including pressing the surface of a silicon wafer against a polishing pad, supplying the polishing composition to the polishing pad, and polishing the surface of the silicon wafer; paragraph [0083]).
Regarding claim 14, modified Kyotani teaches the limitations of claim 12 as discussed above.
Kyotani further teaches a method for producing a semiconductor wafer comprising polishing by using the polishing composition (teaching that the method for manufacturing a semiconductor wafer includes a step of polishing using the disclosed polishing composition, and identifying silicon wafers and compound semiconductor wafers as examples of the semiconductor wafer; paragraph [0084]).
Regarding claim 15, modified Kyotani teaches the limitations of claim 12 as discussed above.
Kyotani further teaches a method for producing a semiconductor device comprising polishing by using the polishing composition (teaching that the method for manufacturing a semiconductor device includes a polishing step using the disclosed polishing composition; paragraph [0085]).
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Kyotani et al. in view of Kajcsos et al., as applied to claim 1 above, and further in view of Motl et al. (WO 2022/171507 A1).
Regarding claim 6, modified Kyotani teaches the limitations of claim 1 as discussed above.
Modified Kyotani does not expressly teach wherein a volume of pores having a diameter of 2 nm or less as measured by a nitrogen gas adsorption method is 0.0070 cm³/g or less.
Motl teaches wherein a volume of pores as measured by a nitrogen gas adsorption method is within the claimed range (teaching amorphous non-porous silica particles having a nitrogen-adsorption pore volume of less than 0.03 cm³/g and, in further embodiments, less than 0.005 cm³/g for non-spherical silica particles and less than 0.002 cm³/g for spherical silica particles; paragraph [0025]). Motl further teaches determining the pore volume using a BET nitrogen-adsorption method; paragraph [0025]. Because Motl’s disclosed total nitrogen-adsorption pore volume is less than 0.005 cm³/g or less than 0.002 cm³/g, the portion of that total attributable to pores having a diameter of 2 nm or less necessarily is no greater than the total pore volume and therefore is less than the claimed 0.0070 cm³/g.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the silica particles of modified Kyotani to have the low nitrogen-adsorption pore volume taught by Motl because Kyotani expressly teaches that the silica particles preferably have no pores in order to provide excellent mechanical strength and storage stability and confirms the presence or absence of pores using BET multipoint nitrogen adsorption; paragraph [0042]. Motl provides a quantitative teaching of non-porous silica particles having nitrogen-adsorption pore volumes below the claimed upper limit. Accordingly, selecting the low nitrogen-adsorption pore volume taught by Motl would have predictably implemented the low-porosity silica structure expressly preferred by Kyotani, with a reasonable expectation of obtaining the mechanical-strength and storage-stability benefits sought by Kyotani. See MPEP § 2143(G).
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over Kyotani et al. in view of Kajcsos et al., as applied to claim 1 above, and further in view of Yoshitake et al. (US 2017/0001870 A1).
Regarding claim 7, modified Kyotani teaches the limitations of claim 1 as discussed above.
Modified Kyotani does not expressly teach wherein a refractive index of the silica particles is 1.390 or more.
Yoshitake teaches wherein a refractive index of the silica particles is 1.390 or more (teaching silica particles formed from an alkoxysilane and having a refractive index, as determined by a liquid immersion method, of 1.450 to 1.460; claim 1; further teaching that refractive index is indicative of the density of the silica particles and that silica particles within the disclosed refractive-index range have high density and excellent moisture resistance; paragraphs [0034]-[0036]). Yoshitake further teaches determining the refractive index by immersing dry silica powder in organic solvents and measuring the refractive index using an Abbe refractometer; paragraph [0037]. Yoshitake’s disclosed range of 1.450 to 1.460 is entirely above the claimed minimum of 1.390.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the silica particles of modified Kyotani to have the refractive index taught by Yoshitake because Kyotani teaches silica particles formed from alkoxysilane condensates and seeks silica particles having improved mechanical strength and storage stability, while Yoshitake teaches alkoxysilane-derived silica particles having a refractive index of 1.450 to 1.460 and explains that refractive index is indicative of silica-particle density. Accordingly, selecting Yoshitake’s known dense alkoxysilane-derived silica-particle structure for use in Kyotani would have predictably provided silica particles having a refractive index within the claimed range. See MPEP § 2141, rationale III(C).
Claim 10 is rejected under 35 U.S.C. 103 as being unpatentable over Kyotani et al. in view of Kajcsos et al., as applied to claim 1 above, and further in view of Sumiya et al. (JP 2021-116225 A).
Regarding claim 10, modified Kyotani teaches the silica particles described in claim 1 as discussed above.
Kyotani further teaches a method for producing the silica particles comprising carrying out a hydrolysis reaction and a condensation reaction of an alkoxysilane (teaching that a preferred method for producing the silica particles is based on hydrolysis and condensation reactions of an alkoxysilane, more preferably a tetraalkoxysilane; paragraph [0046]). Kyotani further teaches that reaction temperature is one of the conditions that may be adjusted during the hydrolysis and condensation reactions; paragraph [0022].
Modified Kyotani does not expressly teach carrying out the hydrolysis reaction and condensation reaction of the alkoxysilane at 40°C or higher.
Sumiya teaches carrying out the hydrolysis reaction and condensation reaction of an alkoxysilane at 40°C or higher (teaching that the reaction temperature for the hydrolysis and condensation reactions is preferably 50°C to 80°C and more preferably 55°C to 75°C; paragraph [0037]). Sumiya further teaches in Example 3 adding a tetramethoxysilane-containing solution while maintaining the reaction solution at 50°C and, after completion of the addition, continuing stirring for another 30 minutes at 50°C; paragraph [0098].
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the method of modified Kyotani to carry out the hydrolysis reaction and condensation reaction at 40°C or higher because Sumiya teaches a known method for producing silica particles by hydrolysis and condensation of tetraalkoxysilane at temperatures of 50°C to 80°C, while Kyotani likewise produces silica particles by hydrolysis and condensation of alkoxysilane and expressly identifies reaction temperature as a controllable reaction condition. Accordingly, applying Sumiya’s known reaction-temperature conditions to Kyotani’s corresponding alkoxysilane hydrolysis-and-condensation process would have been use of a known technique in a similar process to obtain the predictable result of producing silica particles under the claimed reaction-temperature condition. See MPEP § 2141, rationale III(C).
Claims 1-5 and 8-15 are rejected under 35 U.S.C. 103 as being unpatentable over Sumitani et al. (WO 2021/153502 A1) in view of Kajcsos et al., On the peculiarities of positron annihilation features in silicalite-1 and Y-zeolites, Radiation Physics and Chemistry, Vol. 58, pages 709-714 (2000).
Regarding claim 1, Sumitani teaches silica particles (teaching silica particles for use in a silica sol and polishing composition, including semiconductor-wafer and semiconductor-device polishing applications; paragraphs [0014]-[0015]).
Sumitani does not expressly teach wherein an average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 5.3 nm³ or less.
Kajcsos teaches positron annihilation spectroscopy for characterizing internal voids and channels of a siliceous framework (teaching silicalite-1 having an MFI structure with 96 SiO₂ per unit cell and studying the material as a micro-crystalline powder; page 710, Section 2, Experimental). Kajcsos further teaches that the positron lifetime spectra include a 10-90 ns component attributed to o-Ps decaying in internal channels of the zeolite and reports for defected silicalite-1 sample B a corresponding lifetime τ3 of 20.8 ns; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1.
The instant specification explains that the average pore volume of nanoscale pores is determined from the positron lifetime measured by positron annihilation spectroscopy and provides the equations for determining average nanoscale-pore radius R and average pore volume V; paragraphs [0019]-[0023]. Applying Kajcsos’ τ3 value of 20.8 ns to those equations gives a calculated average nanoscale-pore radius of approximately 0.954 nm and a calculated average nanoscale-pore volume of approximately 3.63 nm³, which is less than the claimed 5.3 nm³.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the silica particles of Sumitani to evaluate and select the internal pore structure using the positron annihilation spectroscopy technique taught by Kajcsos because Sumitani identifies pore structure as relevant to the mechanical strength and storage stability of silica particles and prefers silica particles having no pores as evaluated by nitrogen adsorption; paragraph [0037]. Kajcsos teaches positron annihilation spectroscopy as a technique for characterizing internal voids and channels in siliceous materials and provides an internal-channel positron lifetime that, when calculated according to the equations of the instant specification, corresponds to an average nanoscale-pore volume within the claimed range. Accordingly, one of ordinary skill in the art would have had reason to supplement Sumitani’s pore evaluation with Kajcsos’ characterization of internal pore structure and to select silica-particle structures having low internal pore volume, with a reasonable expectation of obtaining the mechanical-strength and storage-stability benefits sought by Sumitani. See MPEP § 2143(G).
Regarding claim 2, modified Sumitani teaches the limitations of claim 1 as discussed above.
Kajcsos further teaches wherein the average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 4.0 nm³ or less (reporting for defected silicalite-1 sample B a positron lifetime τ3 of 20.8 ns for the component attributed to o-Ps decaying in internal channels of the zeolite; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1). Applying Kajcsos’ τ3 value of 20.8 ns to the nanoscale-pore equations set forth in paragraphs [0019]-[0023] of the instant specification gives a calculated average nanoscale-pore volume of approximately 3.63 nm³, which is less than the claimed 4.0 nm³.
Regarding claim 3, modified Sumitani teaches the limitations of claim 1 as discussed above.
Kajcsos further teaches wherein the average pore volume of nanoscale pores as measured by positron annihilation spectroscopy is 1.5 nm³ or more (reporting for defected silicalite-1 sample B a positron lifetime τ3 of 20.8 ns for the component attributed to o-Ps decaying in internal channels of the zeolite; page 711, Section 3, Results and discussion, first paragraph; page 711, Table 1). Applying Kajcsos’ τ3 value of 20.8 ns to the nanoscale-pore equations set forth in paragraphs [0019]-[0023] of the instant specification gives a calculated average nanoscale-pore volume of approximately 3.63 nm³, which is greater than the claimed 1.5 nm³ and also satisfies the 5.3 nm³-or-less limitation of claim 1.
Regarding claim 4, modified Sumitani teaches the limitations of claim 1 as discussed above.
Kajcsos further teaches wherein an average pore volume of atomic-scale pores as measured by positron annihilation spectroscopy is 0.33 nm³ or more (reporting for defected silicalite-1 sample B a positron lifetime τ2 of 4.66 ns and explaining that the corresponding lifetime represents a void having a radius of approximately 0.46 nm; page 711, Table 1; page 711, Section 3, Results and discussion, right column, first paragraph). Applying the atomic-scale-pore-volume relationship set forth in paragraphs [0026]-[0030] of the instant specification to Kajcsos’ approximately 0.46 nm radius gives a calculated average atomic-scale-pore volume of approximately 0.41 nm³, which is greater than the claimed 0.33 nm³.
Regarding claim 5, modified Sumitani teaches the limitations of claim 1 as discussed above.
Kajcsos further teaches Kajcsos further satisfies wherein the average pore volume of atomic-scale pores as measured by positron annihilation spectroscopy is 0.80 nm³ or less (reporting for defected silicalite-1 sample B a positron lifetime τ2 of 4.66 ns and explaining that the corresponding lifetime represents a void having a radius of approximately 0.46 nm; page 711, Table 1; page 711, Section 3, Results and discussion, right column, first paragraph). Applying the atomic-scale-pore-volume relationship set forth in paragraphs [0026]-[0030] of the instant specification to Kajcsos’ approximately 0.46 nm radius gives a calculated average atomic-scale-pore volume of approximately 0.41 nm³, which is less than the claimed 0.80 nm³.
Regarding claim 8, modified Sumitani teaches the limitations of claim 1 as discussed above.
Modified Sumitani further teaches wherein a metal impurity content is 5 ppm or less (teaching that the metal impurity content of the silica particles is preferably 5 ppm or less and more preferably 2 ppm or less; paragraph [0032]). Sumitani further teaches that a metal impurity content of 5 ppm or less may be obtained by producing the silica particles through hydrolysis and condensation reactions using alkoxysilane as the main raw material; paragraph [0036].
Regarding claim 9, modified Sumitani teaches the limitations of claim 1 as discussed above.
Modified Sumitani further teaches wherein a tetraalkoxysilane condensate is a main component (teaching that the silica particles preferably are mainly composed of alkoxysilane condensates and more preferably tetraalkoxysilane condensates, wherein “main component” means 50 mass % or more of the total components constituting the silica particles; paragraph [0038]). Sumitani further teaches using tetraalkoxysilane as the main raw material to obtain silica particles mainly composed of tetraalkoxysilane condensates; paragraph [0039].
Regarding claim 10, modified Sumitani teaches the silica particles described in claim 1 for the reasons discussed regarding claim 1 above.
Modified Sumitani further teaches a method for producing the silica particles comprising carrying out a hydrolysis reaction and a condensation reaction of an alkoxysilane (teaching producing silica particles by adding a solution containing tetraalkoxysilane and a solution containing an alkaline catalyst to a solution containing water and causing the tetraalkoxysilane to undergo hydrolysis and condensation reactions; paragraph [0040]).
Modified Sumitani also teaches carrying out the hydrolysis reaction and condensation reaction of the alkoxysilane at 40°C or higher (teaching that the reaction temperature for the hydrolysis and condensation reactions is preferably 50°C to 80°C and more preferably 55°C to 75°C; paragraph [0063]).
Regarding claim 11, modified Sumitani teaches the limitations of claim 1 as discussed above.
Modified Sumitani further teaches a silica sol comprising the silica particles described in claim 1 (teaching that the silica sol contains the disclosed silica particles and may be produced using the silica-particle dispersion; paragraphs [0075]-[0076]).
Regarding claim 12, modified Sumitani teaches the limitations of claim 11 as discussed above.
Modified Sumitani further teaches a polishing composition comprising the silica sol (teaching that the abrasive composition contains the disclosed silica sol and that the polishing composition preferably contains the silica sol and a water-soluble polymer; paragraph [0084]).
Modified Sumitani further teaches that the polishing composition may be obtained by mixing the disclosed silica sol with a water-soluble polymer and other optional components; paragraph [0099].
Regarding claim 13, modified Sumitani teaches the limitations of claim 12 as discussed above.
Modified Sumitani further teaches a polishing method comprising polishing using the polishing composition (teaching a polishing method including the step of polishing using a polishing composition containing the disclosed silica sol; paragraph [0100]).
Modified Sumitani also teaches a specific polishing method comprising pressing the surface of a silicon wafer against a polishing pad, supplying the polishing composition to the polishing pad, and polishing the surface of the silicon wafer; paragraph [0101].
Regarding claim 14, modified Sumitani teaches the limitations of claim 12 as discussed above.
Modified Sumitani further teaches a method for producing a semiconductor wafer comprising polishing by using the polishing composition described in claim 12 (teaching that the method for manufacturing semiconductor wafers includes the disclosed polishing method, wherein the polishing method includes pressing a silicon wafer against a polishing pad, supplying the polishing composition to the polishing pad, and polishing the silicon-wafer surface; paragraphs [0101]-[0102]). Sumitani further identifies silicon wafers and compound semiconductor wafers as examples of semiconductor wafers; paragraph [0102].
Regarding claim 15, modified Sumitani teaches the limitations of claim 12 as discussed above.
Modified Sumitani further teaches a method for producing a semiconductor device comprising polishing by using the polishing composition described in claim 12 (teaching that the method for manufacturing semiconductor devices includes the disclosed polishing method; paragraph [0103], wherein the disclosed polishing method includes pressing the surface of a silicon wafer against a polishing pad, supplying the polishing composition to the polishing pad, and polishing the surface of the silicon wafer; paragraph [0101]).
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Sumitani et al. in view of Kajcsos et al., as applied to claim 1 above, and further in view of Motl et al. (WO 2022/171507 A1).
Regarding claim 6, modified Sumitani teaches the limitations of claim 1 as discussed above.
Modified Sumitani does not expressly teach wherein a volume of pores having a diameter of 2 nm or less as measured by a nitrogen gas adsorption method is 0.0070 cm³/g or less.
Motl teaches silica particles having a nitrogen-adsorption pore volume within the claimed range (teaching amorphous non-porous silica particles having a nitrogen adsorption pore volume of less than 0.03 cm³/g, preferably less than 0.02 cm³/g, more preferably less than 0.01 cm³/g, and in further embodiments less than 0.005 cm³/g or less than 0.002 cm³/g; paragraph [0025]). Motl further teaches determining the nitrogen-adsorption pore volume using a BET nitrogen adsorption method; paragraph [0025]. Because Motl’s disclosed total nitrogen-adsorption pore volume is less than 0.005 cm³/g or less than 0.002 cm³/g, the portion of that total attributable to pores having a diameter of 2 nm or less necessarily is no greater than the total pore volume and therefore is less than the claimed 0.0070 cm³/g.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the silica particles of modified Sumitani to have the low nitrogen-adsorption pore volume taught by Motl because modified Sumitani expressly teaches that silica particles preferably have no pores in order to provide excellent mechanical strength and storage stability and confirms the presence or absence of pores using nitrogen adsorption; paragraph [0037]. Motl provides a quantitative teaching of non-porous silica particles having nitrogen-adsorption pore volumes below the claimed upper limit. Accordingly, selecting the low nitrogen-adsorption pore volume taught by Motl would have predictably implemented the low-porosity silica structure expressly preferred by Sumitani, with a reasonable expectation of obtaining the mechanical-strength and storage-stability benefits sought by modified Sumitani. See MPEP § 2143(G).
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over Sumitani et al. in view of Kajcsos et al., as applied to claim 1 above, and further in view of Yoshitake et al. (US 2017/0001870 A1).
Regarding claim 7, modified Sumitani teaches the limitations of claim 1 as discussed above.
Modified Sumitani does not expressly teach wherein a refractive index of the silica particles is 1.390 or more.
Yoshitake teaches wherein a refractive index of the silica particles is 1.390 or more (teaching silica particles formed from an alkoxysilane and having a refractive index, as determined by a liquid immersion method, of 1.450 to 1.460; claim 1; further teaching that the refractive index provides an indication of silica-particle density and that silica particles within the disclosed refractive-index range have high density and excellent moisture absorption resistance; paragraphs [0034]-[0036]). Yoshitake further teaches determining the refractive index by immersing dry silica powder in organic solvents and measuring the refractive index of the liquid using an Abbe refractometer; paragraph [0037]. Yoshitake’s disclosed 1.450-1.460 range is entirely above the claimed minimum of 1.390.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the silica particles of modified Sumitani to have the refractive index taught by Yoshitake because modified Sumitani seeks low-porosity silica particles having improved mechanical strength and storage stability, while Yoshitake teaches refractive index as an indicator of silica-particle density and teaches alkoxysilane-derived silica particles having refractive indices of 1.450 to 1.460 corresponding to high-density particles. Modified Sumitani itself prefers silica particles having no pores and teaches silica particles based on alkoxysilane condensates, making Yoshitake’s high-density alkoxysilane-derived silica particles technically compatible with modified Sumitani’s silica-particle system. Accordingly, one of ordinary skill in the art would have had reason to select a known dense silica-particle structure having a refractive index of 1.390 or more, with a reasonable expectation of obtaining the known density characteristics taught by Yoshitake. See MPEP § 2143(G).
Conclusion
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/JONATHAN L CARTER/Examiner, Art Unit 1713
/ERIN F BERGNER/Primary Examiner, Art Unit 1713
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