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 .
Claim Interpretation
The phrase “less than 3% methanol remaining within the silica aerogel” is being interpreted to mean less than 3 wt% residual methanol relative to the total mass of the as-dried aerogel sample measured after drying. This interpretation is supported by [0087] of the publication of the instant application.
Claim Rejections - 35 USC § 102
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 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.
Claim(s) 1-3, 5-13 is/are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Tabata et al. (Large-area silica aerogel for use as Cherenkov radiators with high refractive index, developed by supercritical carbon dioxide drying, The Journal of Supercritical Fluids, 2016), hereinafter ‘Tabata’.
Regarding Claim 1, Tabata discloses a method of making a silica aerogel, comprising the steps of:
synthesizing a silica wet gel from methyl silicate 51 (2. Wet gel synthesis: wet gels are synthesized using methyl silicate 51 (hereinafter ‘MS51’);
aging the silica wet gel for an aging time period until structural changes of the silica wet gel no longer occur (2. Wet gel synthesis: the wet gel in the covered mold was transferred to a sealed tank and aged, typically for two weeks; this is considered a period of time long enough such that structural changes of the silica wet gel no longer occur, per [0048] of the instant published specification);
subjecting the silica wet gel to solvent extraction with methanol for an extraction time period (2. Wet gel synthesis: to obtain highly transparent aerogel tiles, a mixture of methanol and N,N-dimethylformamide (DMF) was used as the diluent solvent; after several minutes, the formed wet gel was covered with a small amount of methanol, and the mold was covered with an aluminum (or polystyrene) lid to prevent the gel from drying – this is considered to meet the claimed solvent extraction with methanol for an extraction time, wherein the extraction time takes place between the addition of the methanol and the addition of the covered wet gel to the aging tank);
drying the silica wet gel to form a silica aerogel (3. Supercritical carbon dioxide drying: The synthesized wet gel tiles were subjected to supercritical carbon dioxide (scCO2) drying)
having a linear shrinkage value of 3% or less (5.2.2. Dependence of refractive index on room temperature: the side length of the aerogel manufactured in summer had an edge length that was 97.6% of the mold size, implying a degree of linear shrinkage of 2.4%).
Further regarding Claim 1, Tabata is silent regarding less than 3% methanol remaining within the silica aerogel.
However, in the process disclosed by Tabata, the amount of methanol utilized per 100 mL of wet gel volume ranged between 4.40 and 7.09 g, which represents a small amount of methanol per volume of the catalyst considering the loadings of the remaining components shown in Table 1. Further, after removing the wet gels from the aging tank, the gels are subjected to solvent replacement with 2-propanol for 1-3 hours, removed from the tank and added to a stainless-steel punched tray, and again immersed in 2-propanol for 1-3 days. Following this treatment, the gel is subjected to hydrophobic treatment by immersing the gels in hexamethyldisilazane for 2-3 days, followed by another immersion in 2-propanol for 2-3 days. This washing process is disclosed as being performed three times, and it is disclosed that such washing “removed impurities such as ammonia generated in the hydrophobic reaction and unreacted chemicals” (2. Wet gel synthesis). From this, it is clear that after exposure to methanol, the wet gels are subjected to extensive subsequent treatment involving immersion in several solvents, which would necessarily displace solvent contained within the gel, including methanol, from the pores thereof.
Furthermore, after being subjected to the treatment described above, the gels are further subjected to supercritical carbon dioxide drying, in which supercritical carbon dioxide acts as a solvent to dissolve remaining solvents within the gel and remove them from the pores thereof. Tabata discloses that the gels are subjected to several stages of drying, and that drying is not halted until the 2-propanol concentration in the extracted fluid is below 100 ppm (3. Supercritical carbon dioxide drying). As discussed above, these gels are immersed for long periods of time and washed repeatedly in 2-propanol, providing a reasonable expectation that there would be relatively more 2-propanol within the pores of the gels than methanol, which is only added to the gel once in the first stages of wet gel formation.
Given that methanol is soluble in supercritical CO2 as well as 2-propanol, that drying is performed until the 2-propanol concentration in the extracted fluid is below 100 ppm, and that there is a reasonable expectation that there would be relatively more 2-propanol within the pores of the gels than methanol, there is a reasonable prima facie basis to conclude that the amount of methanol in the dried aerogels would be almost or entirely negligible, or at least no more than 3% as claimed.
Regarding Claim 2, Tabata discloses the step of drying the silica wet gel forms the silica aerogel having a linear shrinkage value of 2.7% or less (5.2.2. Dependence of refractive index on room temperature: the side length of the aerogel manufactured in summer had an edge length that was 97.6% of the mold size, implying a degree of linear shrinkage of 2.4%).
Regarding Claim 3, Tabata is silent regarding the haze value of the produced silica aerogels.
However, Tabata discloses the use of MS51 as the silica precursor as discussed above. It is disclosed in the instant published speciation that “by using methyl silicate 51 as the silicon alkoxide, the resulting silica aerogel has less haze and less optical distortion than with other silicon alkoxides” ([0037]).
Further, Tabata discloses the use of a methanol solvent as discussed above. The instant specification discloses that “by using methanol as the solvent, the resulting silica aerogel has less haze and less optical distortion than with other solvents” ([0039]).
Further, Tabata discloses the use of ammonia water, also known as ammonium hydroxide, as the gelation catalyst (2. Wet gel synthesis). The instant specification discloses that “by using ammonium hydroxide as the catalyst, the resulting silica aerogel has less haze and less optical distortion than with other catalysts” ([0040]).
Furthermore, Tabata discloses an identical ratio of MS51:water as the claimed invention (see Table 1 of Tabata and Claim 13 of the instant application), an identically long aging time compared to the claimed invention (2. Wet gel synthesis of Tabata and Claim 8 of the instant application), and aging of the wet gel of both Tabata and the claimed invention occurs at room temperature (5.2.2. Dependence of refractive index on room temperature of Tabata and Claim 10 of the instant application).
In light of the above, it is clear that the resulting haze of an aerogel is influenced by the process of making, and in particular, critical elements for attaining the claimed haze are mutual to both the instant claimed process and that of Tabata.
Given the similarities of the process of making between the prior art and the claimed invention, the instant fact pattern resembles that of In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977), wherein the court held that “…where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established.”
Furthermore, it is noted that the Patent Office is not equipped to manufacture products by the myriad of processes put before it and then obtain prior art products and make physical comparisons therewith, as held by the court in In re Brown, 459 F.2d 531, 535, 173 USPQ 685, 688 (CCPA 1972) – as such, determinations of properties not disclosed by the prior art are made based on a preponderance of the evidence provided in both the prior art and the instant disclosure.
Therefore, based on the preponderance of evidence found in the disclosure of Tabata and the instant specification discussed above, there is a reasonable prima facie basis to conclude that the aerogel of Tabata would exhibit the same or nearly the same properties as claimed, including having a haze value of 1.5% or less, absent evidence to the contrary. The burden of proof now shifts to the Applicant to show that the prior art products do not necessarily or inherently possess the characteristics of the claimed product - see MPEP 2112(V).
Regarding Claim 5, Tabata is silent regarding less than 2% methanol remaining within the silica aerogel.
However, in the process disclosed by Tabata, the amount of methanol utilized per 100 mL of wet gel volume ranged between 4.40 and 7.09 g, which represents a small amount of methanol per volume of the catalyst considering the loadings of the remaining components shown in Table 1. Further, after removing the wet gels from the aging tank, the gels are subjected to solvent replacement with 2-propanol for 1-3 hours, removed from the tank and added to a stainless-steel punched tray, and again immersed in 2-propanol for 1-3 days. Following this treatment, the gel is subjected to hydrophobic treatment by immersing the gels in hexamethyldisilazane for 2-3 days, followed by another immersion in 2-propanol for 2-3 days. This washing process is disclosed as being performed three times, and it is disclosed that such washing “removed impurities such as ammonia generated in the hydrophobic reaction and unreacted chemicals” (2. Wet gel synthesis). From this, it is clear that after exposure to methanol, the wet gels are subjected to extensive subsequent treatment involving immersion in several solvents, which would necessarily displace solvent contained within the gel, including methanol, from the pores thereof.
Furthermore, after being subjected to the treatment described above, the gels are further subjected to supercritical carbon dioxide drying, in which supercritical carbon dioxide acts as a solvent to dissolve remaining solvents within the gel and remove them from the pores thereof. Tabata discloses that the gels are subjected to several stages of drying, and that drying is not halted until the 2-propanol concentration in the extracted fluid is below 100 ppm (3. Supercritical carbon dioxide drying). As discussed above, these gels are immersed for long periods of time and washed repeatedly in 2-propanol, providing a reasonable expectation that there would be relatively more 2-propanol within the pores of the gels than methanol, which is only added to the gel once in the first stages of wet gel formation.
Given that methanol is soluble in supercritical CO2 as well as 2-propanol, that drying is performed until the 2-propanol concentration in the extracted fluid is below 100 ppm, and that there is a reasonable expectation that there would be relatively more 2-propanol within the pores of the gels than methanol, there is a reasonable prima facie basis to conclude that the amount of methanol in the dried aerogels would be almost or entirely negligible, or at least no more than 2% as claimed.
Regarding Claims 6-7, Tabata is silent regarding the maximum resilience at complete breaking point of the produced silica aerogels.
However, Tabata discloses the use of a methanol solvent as discussed above. The instant specification discloses that “silica aerogel sample obtained using methanol had better resilience than samples obtained using ethanol or IPA” ([0137]).
Furthermore, Tabata discloses an identical ratio of MS51:water as the claimed invention (see Table 1 of Tabata and Claim 13 of the instant application), an identically long aging time compared to the claimed invention (2. Wet gel synthesis of Tabata and Claim 8 of the instant application), and aging of the wet gel of both Tabata and the claimed invention occurs at room temperature (5.2.2. Dependence of refractive index on room temperature of Tabata and Claim 10 of the instant application).
In light of the above, it is clear that the resulting maximum resilience at complete breaking point of an aerogel is influenced by the process of making, and in particular, critical elements for attaining the claimed haze are mutual to both the instant claimed process and that of Tabata.
Given the similarities of the process of making between the prior art and the claimed invention, the instant fact pattern resembles that of In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977), wherein the court held that “…where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established.”
Furthermore, it is noted that the Patent Office is not equipped to manufacture products by the myriad of processes put before it and then obtain prior art products and make physical comparisons therewith, as held by the court in In re Brown, 459 F.2d 531, 535, 173 USPQ 685, 688 (CCPA 1972) – as such, determinations of properties not disclosed by the prior art are made based on a preponderance of the evidence provided in both the prior art and the instant disclosure.
Therefore, based on the preponderance of evidence found in the disclosure of Tabata and the instant specification discussed above, there is a reasonable prima facie basis to conclude that the aerogel of Tabata would exhibit the same or nearly the same properties as claimed, including having a maximum resilience at complete breaking point within the ranges instantly claimed, absent evidence to the contrary. The burden of proof now shifts to the Applicant to show that the prior art products do not necessarily or inherently possess the characteristics of the claimed product - see MPEP 2112(V).
Regarding Claim 8, Tabata discloses aging the gel for a period of about two weeks as discussed above.
Regarding Claim 9, Tabata discloses the extraction time period is less than 24 hours (2. Wet gel synthesis: to obtain highly transparent aerogel tiles, a mixture of methanol and N,N-dimethylformamide (DMF) was used as the diluent solvent; after several minutes, the formed wet gel was covered with a small amount of methanol, and the mold was covered with an aluminum (or polystyrene) lid to prevent the gel from drying – this is considered to meet the claimed solvent extraction with methanol for an extraction time, wherein the extraction time takes place between the addition of the methanol and the addition of the covered wet gel to the aging tank. This extraction time is considered to take place on a scale of minutes or hours, and absent disclosure to the contrary, not longer than 24 hours).
Regarding Claim 10, Tabata discloses aging the silica wet gels at room temperature (5.2.2. Dependence of refractive index on room temperature).
Regarding Claim 11, Tabata discloses the step of synthesizing the silica aerogel from methyl silicate 51 comprises the steps of:
preparing a first solution by mixing methyl silicate 51 and methanol (2. Wet gel synthesis: Solution A was first prepared by adding methanol and DMF to polymethoxy siloxane in a beaker);
preparing a second solution by mixing ammonium hydroxide and water (2. Wet gel synthesis: next, water was mixed with aqueous ammonia in another beaker to yield Solution B.);
mixing the first solution and the second solution together to form a precursor material (2. Wet gel synthesis: Immediately after adding solution B to solution A, the mixed solution was stirred for 20 s); and
allowing components in the precursor material to react to form silica wet gel (2. Wet gel synthesis: after several minutes, the formed wet gel…).
Regarding Claims 12 and 13, Tabata discloses a ratio of MS51 to water of approximately 1:1 – see Table 1.
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 1-3, 5-11 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1-3, 4, 7-8, 10-13 of copending Application No. 18636591 (reference application). Although the claims at issue are not identical, they are not patentably distinct from each other because:
The reference application claims a method of making a silica aerogel, comprising the steps of synthesizing a silica wet gel from methyl silicate 51; aging the silica wet gel for an aging time period until structural changes of the silica wet gel no longer occur; subjecting the silica wet gel to solvent extraction with methanol for an extraction time period; and drying the silica wet gel to form a silica aerogel having a linear shrinkage value of 3% or less and less than 3% methanol remaining within the silica aerogel (Claims 1, 4, 7, 10-11).
The reference application claims the silica aerogel has a haze value of 1.5% or less (Claim 12).
The reference application claims the aging time period is at least 7 days (Claim 2).
The reference application claims the extraction time period is less than 24 hours (Claim 8).
The reference application claims the step of aging comprises aging the silica wet gel at room temperature (Claim 3).
The reference application claims the step of synthesizing the silica aerogel from methyl silicate 51 comprises the steps of: preparing a first solution by mixing methyl silicate 51 and methanol; preparing a second solution by mixing ammonium hydroxide and water; mixing the first solution and the second solution together to form a precursor material; and allowing components in the precursor material to react to form silica wet gel (Claim 13).
This is a provisional nonstatutory double patenting rejection because the patentably indistinct claims have not in fact been patented.
Conclusion
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LOGAN LACLAIR
Examiner
Art Unit 1736
/L.E.L./Examiner, Art Unit 1736
/DANIEL C. MCCRACKEN/Primary Examiner, Art Unit 1736
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