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 .
Election/Restrictions
Claims 21-32 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected article, there being no allowable generic or linking claim. Applicant timely traversed the restriction (election) requirement in the reply filed on 3/11/2026.
Applicant's election with traverse of the restriction requirement in the above reply is acknowledged. The traversal is on the ground(s) that restriction is improper because a full and complete search of the claimed subject matter would include both groups of claims, such that a serious search burden does not exist between the groups. This is not found persuasive because, as set forth in MPEP 808.02, in order to demonstrate a serious search burden, the examiner must show by appropriate explanation one of the following, including separate classification thereof, a separate status in the art when they are classifiable together, OR a different field of search. The groups have been shown to be at least classified separately, as shown in the requirement for restriction.
Therefore, without a more detailed showing as to how a serious search burden does not exist between the two groups, or evidence the claims are not distinct from one another, the requirement is still deemed proper and is therefore made FINAL.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(d):
(d) REFERENCE IN DEPENDENT FORMS.—Subject to subsection (e), a claim in dependent form shall contain a reference to a claim previously set forth and then specify a further limitation of the subject matter claimed. A claim in dependent form shall be construed to incorporate by reference all the limitations of the claim to which it refers.
The following is a quotation of pre-AIA 35 U.S.C. 112, fourth paragraph:
Subject to the following paragraph [i.e., the fifth paragraph of pre-AIA 35 U.S.C. 112], a claim in dependent form shall contain a reference to a claim previously set forth and then specify a further limitation of the subject matter claimed. A claim in dependent form shall be construed to incorporate by reference all the limitations of the claim to which it refers.
Claims 4 -5, 10, and 14-15 are rejected under 35 U.S.C. 112(d) or pre-AIA 35 U.S.C. 112, 4th paragraph, as being of improper dependent form for failing to further limit the subject matter of the claim upon which it depends, or for failing to include all the limitations of the claim upon which it depends.
Claim 1 recites methyl silicate 51 has a total weight percent of greater than or equal to 10.7% and less than or equal to 24.1%, and the methyltrimethoxysilane has a total weight percent of greater than or equal to 2.3% and less than or equal to 4.5% while claim 4 recites the limitation that methyl silicate 51 at a weight percent of greater than or equal to 30.8% or less than or equal to 69.2% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5%. Claim 5 recites the limitation methyl silicate 51 at a weight percent of greater than or equal to 30.8% and less than or equal to 55.6% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5%. Claim 10 recites the limitation methyl silicate 51 at a weight percent of greater than or equal to 36.8% and less than or equal to 53.8% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5% Claims 14 and 15 recite the limitation methyl silicate 51 at a weight percent of greater than or equal to 36.8% and less than or equal to 49% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 13.2%, methyl silicate 51 at a weight percent of greater than or equal to 36.8% and less than or equal to 44.7% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 13.2%. The claims 4 -5, 10, and 14-15 range respecting methyl silicate and methyltrimethoxysilane do not fall within the claim 1 range. As such, claims 4 -5, 10, and 14-15 are directed to compositions that fall outside the scope of claim 1. Claims 4 -5, 10, and 14-15 therefore fails to further limit the subject matter of the claim upon which it depends, or for fails to include all the limitations of the claim upon which it depends.
Applicant may cancel the claim(s), amend the claim(s) to place the claim(s) in proper dependent form, rewrite the claim(s) in independent form, or present a sufficient showing that the dependent claim(s) complies with the statutory requirements.
Claim Rejections - 35 USC § 103
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious to 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.
Claim(s) 1-4, 16-18, and 20 is/are rejected under 35 U.S.C. 103 as being unpatentable over Yokogawa (US6740416B1) in view of Chen et al (US2024/0199835 A1).
Regarding claim 1, Yokogawa teaches a method of making a hydrophobic silica aerogel [abstract], comprising the steps of: preparing a first solution by mixing methyl silicate 51 and methanol (Example 1); preparing a second solution by mixing methanol, ammonium hydroxide and water (Example 1);
mixing the first solution and the second solution together to form a mixed solution (Example 1); allowing components in the mixed solution to react to form silica wet gel (Example 1);
Yokogawa discloses drying the hydrophobic silica wet gel to form hydrophobic silica aerogel (column 7 lines 27-30);
wherein the methyl silicate 51 has a total weight percent of greater than or equal to 10.7% and less than or equal to 24.1% (Col 24, lines 56-57: solution A and B are mixed in a mass ratio of 16:17 – this corresponds to a precursor solution having a mass composition of 17.80 wt% MS-51, 62.29 wt% methanol, 19.79 wt% water, and 0.109 wt% ammonium hydroxide, (also see attached table below)).
Yokogawa does not explicitly disclose preparing a third solution by mixing methyltrimethoxysilane and methanol and adding the third solution to the silica wet gel; allowing the third solution to react with the silica wet gel to form hydrophobic silica wet gel. However, analogous aerogel art, Chen et al, discloses mixing methylsiloxane and alcohol (methanol) since “the purpose of adding the methylsiloxane compound is to provide strong hydrophobic properties of the complex aerogel composites; the purpose of adding the siloxane compound is to control the internal microstructure of the aerogel system; and the purpose of adding aqueous solution containing alcohols is to provide the porosity content of the aerogel structure” [0059]. Therefore, it would have been obvious to one having ordinary skill in the art before the effective filing date of the claimed invention to have incorporated a third solution of methyltrimethoxysilane and methanol to the silica wet gel in order to control the internal microstructure and porosity structure of the aerogel while providing strong hydrophobic properties.
Analogous aerogel art, Chen et al, further discloses the methyltrimethoxysilane has a total weight percent of greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]), wherein total weight percent represents a total weight percent of a component in the first, second and third solutions. Thus, Chen et al’s range overlaps with Applicant’s claimed range.
MPEP 2144.05 states overlapping ranges is a prima facie evidence of obviousness. Further, In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Regarding claim 2, Yokogawa teaches Col 24, lines 56-57: solution A and B are mixed in a mass ratio of 16:17 – this corresponds to a precursor solution having a mass composition of 17.80 wt% MS-51, 62.29 wt% methanol, 19.79 wt% water, and 0.109 wt% ammonium hydroxide (also see attached table below). As for the methyltrimethoxysilane, Chen et al disclose the methyltrimethoxysilane has a total weight percent of greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]), wherein total weight percent represents a total weight percent of a component in the first, second and third solutions. This falls within Applicant’s range of the total weight percent of the methyl silicate 51 is greater than or equal to 10.7% and less than or equal to 24.1%; the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5%; the methanol has a total weight percent of greater than or equal to 59.8% and less than or equal to 75.1%; the water has a total weight percent of greater than or equal to 10.4% and less than or equal to 13.5%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.125%. MPEP 2144.05 states overlapping ranges is a prima facie evidence of obviousness. Further, In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
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Regarding claim 3, Yokogawa teaches the total weight percent of the methyl silicate 51 is greater than or equal to 10.7% and less than or equal to 22.3% (col 24, lines 56-57: 17.80 wt% MS-51); the methanol has a total weight percent of greater than or equal to 62.5% and less than or equal to 75.1% ( 62.29 wt% methanol; col 24 lines 56-57)
Chen teaches the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]).
Yokokawa further teaches 19.79 wt% water, and 0.109 wt% ammonium hydroxide which is close to Applicant’s range of the water has a total weight percent of greater than or equal to 10.8% and less than or equal to 11.7%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.016%. MPEP 2144.05 states Titanium Metals Corp. of America v. Banner, 778 F.2d 775,227 USPQ 773 (Fed. Cir. 1985) a prima facie case of obviousness exists where the claimed ranges and prior art ranges do not overlap but are close enough that one skilled in the art would have expected them to have the same properties. Therefore, it would have been obvious to one having ordinary skill in the art to of the claimed invention to have incorporated a range of the water has a total weight percent of greater than or equal to 10.8% and less than or equal to 11.7%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.016% since the claimed ranges and the prior art ranges are close enough that one skilled in the art would have expected them to have the same properties
Regarding claim 4, Yokogawa and Chen does not explicitly disclose wherein the first solution comprises methyl silicate 51 at a weight percent of greater than or equal to 30.8% and less than or equal to 55.6% and methanol at a weight percent of greater than or equal to 44.4% and less than or equal to 69.2%, the second solution comprises methanol at a weight percent of greater than or equal to 58.6% and less than or equal to 67.6%, water at a weight percent of greater than or equal to 32.1% and less than or equal to 41.1%, and ammonium hydroxide at a weight percent of greater than or equal to 0.03% and less than or equal to 0.39%, and the third solution comprises methanol at a weight percent of greater than or equal to 86.8% and less than or equal to 91.7% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5%.
However, Chen discloses mixing methylsiloxane and alcohol (methanol) since “the purpose of adding the methylsiloxane compound is to provide strong hydrophobic properties of the complex aerogel composites; the purpose of adding the siloxane compound is to control the internal microstructure of the aerogel system; and the purpose of adding aqueous solution containing alcohols is to provide the porosity content of the aerogel structure” [0059]. Therefore, the amounts of methyl silicate, methanol, ammonium hydroxide an methyltrimethoxysilane are result effective variables. MPEP 2144.05 discloses In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Regarding claim 16, Yokogawa does not explicitly disclose a step of aging the hydrophobic silica wet gel for a time period of at least 7 days (168 hour). However, since the time it requires to age the aerogels influences the final material’s structure, porosity, and mechanical stability, one would recognize it as a result effective variable. MPEP 2144.05 states It is well settled that determination of optimum values of cause effective variables such as these process parameters is within the skill of one practicing in the art. In re Boesch, 205 USPQ 215 (CCPA 1980). Further, MPEP 2144.05 discloses In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Regarding claim 17, Yokogawa does not explicitly disclose a step of subjecting the hydrophobic silica wet gel to solvent extraction with methanol for an extraction time period of less than 24 hours. However, Yokogawa discloses drying the gel to increase the porosity while maintaining the structure (column 11 lines 38-41). Therefore, one ordinary skill in the art would understand extraction time is a result effective variable. MPEP 2144.05 states It is well settled that determination of optimum values of cause effective variables such as these process parameters is within the skill of one practicing in the art. In re Boesch, 205 USPQ 215 (CCPA 1980). Further, MPEP 2144.05 discloses In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Regarding claim 18, Yokogawa does not explicitly disclose wherein the step of drying the hydrophobic silica wet gel to form hydrophobic silica aerogel comprises subjecting the hydrophobic silica wet gel to drying to form the hydrophobic silica aerogel with a shrinkage value of 4% or less. However, since Yokogawa and Chen’s method is similar to Applicant’s method, it would thus, have similar properties. Therefore, the claimed physical
properties implicitly would have been achieved by the composite structure as claimed and
rendered obvious (MPEP 2112.01(I,II)). If it is the applicant’s position that this would not be the
case: (1) evidence would need to be presented to support the applicant’s position; and (2) it
would be the Office’s position that the application contains inadequate disclosure that there is
no teaching as to how to obtain the claimed properties with only the claimed ingredients,
amounts, process steps, and process conditions.
Claim 20 is obvious because the proposed prior art modification involves no surfactant.
Claim(s) 5 and 19 is/are rejected under 35 U.S.C. 103 as being unpatentable over Yokogawa (US6740416B1) in view of Chen et al (US2024/0199835 A1) further in view of Rao et al (30 Microporous and Mesoporous Materials).
Regarding claim 5 Yokogawa does not explicitly disclose wherein the first solution comprises methyl silicate 51 at a weight percent of greater than or equal to 30.8% and less than or equal to 53.8% and methanol at a weight percent of greater than or equal to 46.2% and less than or equal to 69.2%, the second solution comprises methanol at a weight percent of greater than or equal to 63.5% and less than or equal to 67.6%, water at a weight percent of greater than or equal to 32.4% and less than or equal to 36.5%, and ammonium hydroxide at a weight percent of greater than or equal to 0.03% and less than or equal to 0.06%, and the third solution comprises methanol at a weight percent of greater than or equal to 89.1% and less than or equal to 91.7% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5%. However, analogous art, Rao et al, teaches that aerogels can be made as both transparent (>90%) and translucent to the visible light, depending on the sol–gel processing conditions, but they exhibit Rayleigh scattering in the blue region. Rao at page 268, col. 1. Rao teaches that these properties of aerogels can be utilized for thermal superinsulations in windows and heat-storage systems, acoustic devices, luminescent solar systems, gas filters, catalysts or catalyst supports. Rao at page 268, col. 1.
Rao teaches a study regarding effects of adding methyltrimethoxysilane (MTMS) to the synthesis formulation on the hydrophobicity and physical properties of silica aerogels. Rao at Abstract. Rao teaches that the molar ratio of the methanol (MeOH) solvent, water (H2O), and the ammonia (NH4OH) catalyst to tetramethoxysilane (TMOS) precursor was fixed at 1 TMOS : 12 MeOH : 4 H2O : 3.6×10−3 NH4OH throughout the experiment and the MTMS/TMOS molar ratio M was varied from 0 to 1.55. Rao at Abstract.
Rao teaches that for M<0.26 the aerogels were less hydrophobic but more transparent (>90% in the visible range), whereas for M>1.03 the aerogels were more hydrophobic but semi-transparent to opaque. Rao at Abstract. Rao further teaches that aerogels with good hydrophobicity and transparency (~85% in the visible range) were obtained with an M about 0.70 and an increase in the MTMS content in the gels shifted the pore size distribution towards larger pore radii with a broad distribution. Rao at Abstract.
Rao thus teaches that the molar ratio M of MTMS/TMOS is clearly an optimizable, result-effective variable depending on the physical properties desired in the respective application. MPEP 2144.05 In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Claim 19 further limits claim 1 by reciting “subjecting the hydrophobic silica wet gel to drying to form the hydrophobic silica aerogel with a visible transmission of at least 97.8% and a haze value of 3% or less”. As discussed above, Rao teaches that the molar ratio M of MTMS/TMOS is clearly an optimizable, result-effective variable depending on the physical properties desired in the respective application and that decreasing the amount of MTMS in increases the transparency of the aerogel. Rao at Abstract. Here the obviousness rationale proposes lowering the molar ratio M of MTMS/TMOS to arrive at hydrophobic aerogels in applications where higher transparency is desired, such as thermal superinsulations in windows, as taught by Rao. Because the proposed modification of Yokogawa and Chen employs the same reagent amounts as claimed, the resulting aerogel will have the same claimed transmission and haze values as claimed. Once a reference teaching product appearing to be substantially identical is made the basis of a rejection, and the examiner presents evidence or reasoning to show inherency, the burden of production shifts to the applicant. MPEP § 2112(V) (citing In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433-34 (CCPA 1977). Each and every limitation of claim 19 is asserted to be met by the cited art. The point is that Rao teaches that molar ratio M of MTMS/TMOS is clearly an optimizable, result-effective variable and one of ordinary skill is motivated to optimize this ratio to achieve the claimed transmission and haze values in relevant applications of the aerogel.
Claim(s) 6 and 11 is/are rejected under 35 U.S.C. 103 as being unpatentable over Yokogawa (US6740416B1) in view of Chen et al (US2024/0199835 A1) as applied claim 1, and further in view of Jana (US20100144962 A1).
Regarding claims 6 and 11, Yokogawa discloses the total weight percent of the methyl silicate 51 is greater than or equal to 13.4% and less than or equal to 24.1% (Col 24, lines 56-57: mass composition of 17.80 wt% MS-51). Chen et al teaches the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]).
Yokogawa and Chen do not explicitly disclose wherein the density of the hydrophobic silica aerogel is between 120 mg/cc and 200 mg/cc. However, analogous aerogel art, Jana, discloses Silica aerogels are among the world's lightest solids, with density values ranging between 0.3-800 mg/cc [0010]. MPEP 2144.05 states In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Claim(s) 7-8 and 12-13 is/are rejected under 35 U.S.C. 103 as being unpatentable over Yokogawa (US6740416B1) in view of Chen et al (US2024/0199835 A1) and further in view of Jana (US20100144962 A1), as applied to claim 6/11 and further in view of Sink et al (Influence of Chemical Conditions on the Nanoporous Structure of Silicate Aerogels, Material 2010, herein referred to as Sinko).
Regarding claim 7, Yokogawa teaches the total weight percent of the methyl silicate 51 is greater than or equal to 13.4% and less than or equal to 24.1% (Col 24, lines 56-57: mass composition of 17.80 wt% MS-51); the methanol has a total weight percent of greater than or equal to 59.8% and less than or equal to 72.6%; the water has a total weight percent of greater than or equal to 10.8% and less than or equal to 11.6%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.125% (62.29 wt% methanol, and 0.109 wt% ammonium hydroxide Col 24, lines 56-57).
Chen teaches the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]).;
Yokogawa and Chen do not explicitly disclose the water. However, analogous art, Sinko, discloses that the amount of water used in the initial gelation solutions can significantly affect the silica framework (3.5. Effect of water content). At lower molar ratios, the H₂O is not sufficient to complete the hydrolysis reaction of the silicon precursor. The molar ratio of H₂O/Si(OR)₄ in the gelation solutions should accordingly be sufficient to approach the minimal hydrolysis degree of the alkoxide required for the gelation. Ratios of water/alkoxy group ≤ 2 favor the condensation reactions. In the case of silicon alkoxide precursor, the incomplete hydrolysis leads to linear chain formation with residual organic groups. On the other hand, at higher molar ratio, the hydrolysis proceeds faster, and the condensation takes place slowly. Water/alkoxy group ratios > 4 induce very loose gel networks with high porosity and smaller particles. Due to the presence of excess water, the rate of polymerization is lower than that of condensation, producing cyclization and enhancing the siloxane bond formation within the particles. At molar ratios lower than 2 and higher than 12, only dense and cracked aerogels will be formed. The lowest density (0.08 g cm-3) and the most transparent (90%) aerogels can be obtained with molar ratios between 6 and 10. Further, it is disclosed that the amount of water used in the precursor solution affects the surface area of the resulting aerogel. From this, it is clear that the amount of water in the initial gelation solution is a critical, result effective variable that may be manipulated in order to influence properties of the aerogel, including manipulating the rate of hydrolysis and condensation of the silicate precursor, thereby manipulating the properties of the framework of the produced aerogel, such as surface area and density. Accordingly, water is a result effective variable. As such, without showing unexpected results associated and commensurate in scope with the claimed range, the claimed range cannot be considered critical. Accordingly, one of ordinary skill in the art to of the claimed invention would have optimized, by routine experimentation, the amount of water in the second solution in Yokogawa in order to obtain chemical conditions in the resulting precursor comprising a mixture of the first and second solution, which would lead to desired aerogel properties, since it has been held that where the general conditions of the claim are disclosed in the prior art, discovering the optimum or workable ranges involves only routine skill in the art (In re Aller, 105 USPQ 223).
Regarding claim 8, Yokogawa teaches the total weight percent of the methyl silicate 51 is greater than or equal to 13.4% and less than or equal to 22.3% (Col 24, lines 56-57: mass composition of 17.80 wt% MS-51); the methanol has a total weight percent of greater than or equal to 62.5% and less than or equal to 72.6%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.016% (Col 24, lines 56-57: 62.29 wt% methanol, and 0.109 wt% ammonium hydroxide Col 24, lines 56-57).
Chen teaches the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]).;
Yokogawa and Chen do not explicitly disclose the water. However, analogous art, Sinko, discloses that the amount of water used in the initial gelation solutions can significantly affect the silica framework (3.5. Effect of water content). At lower molar ratios, the H₂O is not sufficient to complete the hydrolysis reaction of the silicon precursor. The molar ratio of H₂O/Si(OR)₄ in the gelation solutions should accordingly be sufficient to approach the minimal hydrolysis degree of the alkoxide required for the gelation. Ratios of water/alkoxy group ≤ 2 favor the condensation reactions. In the case of silicon alkoxide precursor, the incomplete hydrolysis leads to linear chain formation with residual organic groups. On the other hand, at higher molar ratio, the hydrolysis proceeds faster, and the condensation takes place slowly. Water/alkoxy group ratios > 4 induce very loose gel networks with high porosity and smaller particles. Due to the presence of excess water, the rate of polymerization is lower than that of condensation, producing cyclization and enhancing the siloxane bond formation within the particles. At molar ratios lower than 2 and higher than 12, only dense and cracked aerogels will be formed. The lowest density (0.08 g cm-3) and the most transparent (90%) aerogels can be obtained with molar ratios between 6 and 10. Further, it is disclosed that the amount of water used in the precursor solution affects the surface area of the resulting aerogel. From this, it is clear that the amount of water in the initial gelation solution is a critical, result effective variable that may be manipulated in order to influence properties of the aerogel, including manipulating the rate of hydrolysis and condensation of the silicate precursor, thereby manipulating the properties of the framework of the produced aerogel, such as surface area and density. Accordingly, water is a result effective variable. As such, without showing unexpected results associated and commensurate in scope with the claimed range, the claimed range cannot be considered critical. Accordingly, one of ordinary skill in the art to of the claimed invention would have optimized, by routine experimentation, the amount of water in the second solution in Yokogawa in order to obtain chemical conditions in the resulting precursor comprising a mixture of the first and second solution, which would lead to desired aerogel properties, since it has been held that where the general conditions of the claim are disclosed in the prior art, discovering the optimum or workable ranges involves only routine skill in the art (In re Aller, 105 USPQ 223).
Regarding claims 12-13, Yokogawa discloses the total weight percent of the methyl silicate 51 is greater than or equal to 13.4% and less than or equal to 20.4% (Col 24, lines 56-57: mass composition of 17.80 wt% MS-51); the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 3.9%; the methanol has a total weight percent of greater than or equal to 66.2% and less than or equal to 72.6%; the water has a total weight percent of greater than or equal to 10.4% and less than or equal to 11.6%; and the ammonium hydroxide has a total weight percent of greater than or equal to 0.013% and less than or equal to 0.125% ((Col 24, lines 56-57: 62.29 wt% methanol, and 0.109 wt% ammonium hydroxide).
Chen teaches the total weight percent of the methyltrimethoxysilane is greater than or equal to 2.3% and less than or equal to 4.5% (methytrimethoxysilane is between 2-40% [0059]).;
Yokogawa and Chen do not explicitly disclose the water. However, analogous art, Sinko, discloses that the amount of water used in the initial gelation solutions can significantly affect the silica framework (3.5. Effect of water content). At lower molar ratios, the H₂O is not sufficient to complete the hydrolysis reaction of the silicon precursor. The molar ratio of H₂O/Si(OR)₄ in the gelation solutions should accordingly be sufficient to approach the minimal hydrolysis degree of the alkoxide required for the gelation. Ratios of water/alkoxy group ≤ 2 favor the condensation reactions. In the case of silicon alkoxide precursor, the incomplete hydrolysis leads to linear chain formation with residual organic groups. On the other hand, at higher molar ratio, the hydrolysis proceeds faster, and the condensation takes place slowly. Water/alkoxy group ratios > 4 induce very loose gel networks with high porosity and smaller particles. Due to the presence of excess water, the rate of polymerization is lower than that of condensation, producing cyclization and enhancing the siloxane bond formation within the particles. At molar ratios lower than 2 and higher than 12, only dense and cracked aerogels will be formed. The lowest density (0.08 g cm-3) and the most transparent (90%) aerogels can be obtained with molar ratios between 6 and 10. Further, it is disclosed that the amount of water used in the precursor solution affects the surface area of the resulting aerogel. From this, it is clear that the amount of water in the initial gelation solution is a critical, result effective variable that may be manipulated in order to influence properties of the aerogel, including manipulating the rate of hydrolysis and condensation of the silicate precursor, thereby manipulating the properties of the framework of the produced aerogel, such as surface area and density. Accordingly, water is a result effective variable. As such, without showing unexpected results associated and commensurate in scope with the claimed range, the claimed range cannot be considered critical. Accordingly, one of ordinary skill in the art to of the claimed invention would have optimized, by routine experimentation, the amount of water in the second solution in Yokogawa in order to obtain chemical conditions in the resulting precursor comprising a mixture of the first and second solution, which would lead to desired aerogel properties, since it has been held that where the general conditions of the claim are disclosed in the prior art, discovering the optimum or workable ranges involves only routine skill in the art (In re Aller, 105 USPQ 223).
Claim(s) 9-10 and 14-15 is/are rejected under 35 U.S.C. 103 as being unpatentable over Yokogawa (US6740416B1) in view of Chen et al (US2024/0199835 A1) further in view of Jana (US20100144962 A1), as applied to claim 6/11, and further in view of Rao et al., 30 Microporous and Mesoporous Materials, 267-273 (1999) (“Rao”)
Regarding claims 9-10, Yokogawa does not explicitly disclose wherein the first solution comprises methyl silicate 51 at a weight percent of greater than or equal to 36.8% and less than or equal to 53.8% and methanol at a weight percent of greater than or equal to 46.2% and less than or equal to 63.2%, the second solution comprises methanol at a weight percent of greater than or equal to 63.5% and less than or equal to 67%, water at a weight percent of greater than or equal to 33% and less than or equal to 36.5%, and ammonium hydroxide at a weight percent of greater than or equal to 0.03% and less than or equal to 0.06%, and the third solution comprises methanol at a weight percent of greater than or equal to 84.5% and less than or equal to 91.7% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 15.5%. However, Rao teaches that aerogels can be made as both transparent (>90%) and translucent to the visible light, depending on the sol–gel processing conditions, but they exhibit Rayleigh scattering in the blue region. Rao at page 268, col. 1. Rao teaches that these properties of aerogels can be utilized for thermal superinsulations in windows and heat-storage systems, acoustic devices, luminescent solar systems, gas filters, catalysts or catalyst supports. Rao at page 268, col. 1.
Rao teaches a study regarding effects of adding methyltrimethoxysilane (MTMS) to the synthesis formulation on the hydrophobicity and physical properties of silica aerogels. Rao at Abstract. Rao teaches that the molar ratio of the methanol (MeOH) solvent, water (H2O), and the ammonia (NH4OH) catalyst to tetramethoxysilane (TMOS) precursor was fixed at 1 TMOS : 12 MeOH : 4 H2O : 3.6×10−3 NH4OH throughout the experiment and the MTMS/TMOS molar ratio M was varied from 0 to 1.55. Rao at Abstract.
Rao teaches that for M<0.26 the aerogels were less hydrophobic but more transparent (>90% in the visible range), whereas for M>1.03 the aerogels were more hydrophobic but semi-transparent to opaque. Rao at Abstract. Rao further teaches that aerogels with good hydrophobicity and transparency (~85% in the visible range) were obtained with an M about 0.70 and an increase in the MTMS content in the gels shifted the pore size distribution towards larger pore radii with a broad distribution. Rao at Abstract.
Rao thus teaches that the molar ratio M of MTMS/TMOS is clearly an optimizable, result-effective variable depending on the physical properties desired in the respective application. MPEP 2144.05 further states In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
Regarding claims 14-15, Yokogawa does not explicitly disclose wherein the first solution comprises wherein the first solution comprises methyl silicate 51 at a weight percent of greater than or equal to 36.8% and less than or equal to 44.7% and methanol at a weight percent of greater than or equal to 55.3% and less than or equal to 63.2%, the second solution comprises methanol at a weight percent of greater than or equal to 65.3% and less than or equal to 67%, water at a weight percent of greater than or equal to 33% and less than or equal to 34.7%, and ammonium hydroxide at a weight percent of greater than or equal to 0.03% and less than or equal to 0.06%, and the third solution comprises methanol at a weight percent of greater than or equal to 86.8% and less than or equal to 91.7% and methyltrimethoxysilane at a weight percent of greater than or equal to 8.3% and less than or equal to 13.2%. However, Rao teaches that aerogels can be made as both transparent (>90%) and translucent to the visible light, depending on the sol–gel processing conditions, but they exhibit Rayleigh scattering in the blue region. Rao at page 268, col. 1. Rao teaches that these properties of aerogels can be utilized for thermal superinsulations in windows and heat-storage systems, acoustic devices, luminescent solar systems, gas filters, catalysts or catalyst supports. Rao at page 268, col. 1.
Rao teaches a study regarding effects of adding methyltrimethoxysilane (MTMS) to the synthesis formulation on the hydrophobicity and physical properties of silica aerogels. Rao at Abstract. Rao teaches that the molar ratio of the methanol (MeOH) solvent, water (H2O), and the ammonia (NH4OH) catalyst to tetramethoxysilane (TMOS) precursor was fixed at 1 TMOS : 12 MeOH : 4 H2O : 3.6×10−3 NH4OH throughout the experiment and the MTMS/TMOS molar ratio M was varied from 0 to 1.55. Rao at Abstract.
Rao teaches that for M<0.26 the aerogels were less hydrophobic but more transparent (>90% in the visible range), whereas for M>1.03 the aerogels were more hydrophobic but semi-transparent to opaque. Rao at Abstract. Rao further teaches that aerogels with good hydrophobicity and transparency (~85% in the visible range) were obtained with an M about 0.70 and an increase in the MTMS content in the gels shifted the pore size distribution towards larger pore radii with a broad distribution. Rao at Abstract.
Rao thus teaches that the molar ratio M of MTMS/TMOS is clearly an optimizable, result-effective variable depending on the physical properties desired in the respective application. MPEP 2144.05 further states In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation. It would have been obvious to one having ordinary skill in the art to have determined the optimum values of the relevant process parameters through routine experimentation in the absence of a showing of criticality.
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 1-20 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1-20 of copending Application No. 18/636,681 (reference application). Although the claims at issue are not identical, they are not patentably distinct from each other because both applications refer to a method of making a hydrophobic silica aerogel, comprising the steps of: preparing a first solution by mixing tetramethyl orthosilicate and methanol; preparing a second solution by mixing methanol, ammonium hydroxide and water; mixing the first solution and the second solution together to form a mixed solution; allowing components in the mixed solution to react to form silica wet gel; preparing a third solution by mixing methyltrimethoxysilane and methanol; adding the third solution to the silica wet gel; allowing the third solution to react with the silica wet gel to form hydrophobic silica wet gel; and drying the hydrophobic silica wet gel to form hydrophobic silica aerogel; wherein the tetramethyl orthosilicate has a total weight percent of greater than or equal to 13.8% and less than or equal to 31% and the methyltrimethoxysilane has a total weight percent of greater than or equal to 3.2% and less than or equal to 4.6%, wherein total weight percent represents a total weight percent of a component in the first, second and third solutions
This is a provisional nonstatutory double patenting rejection because the patentably indistinct claims have not in fact been patented.
Claims 1 and 16-20 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1, 10, and 12-16 of copending Application No. 18/636,681 (reference application). Although the claims at issue are not identical, they are not patentably distinct from each other because both applications refer to a method of making a hydrophobic silica aerogel, comprising the steps of: first solution by mixing methyl silicate 51 and solvent; preparing a second solution by mixing solvent, ammonium hydroxide and water; mixing the first solution and the second solution together to form a mixed solution; allowing components in the mixed solution to react to form silica wet gel; preparing a third solution by mixing methyltrimethoxysilane and diluent, and wherein the third solution comprises the methyltrimethoxysilane in a controlled amount selected to provide a molar ratio of methyl silicate 51.
Claims 1-20 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1-20 of copending Application No. 18/636,497 (reference application). Although the claims at issue are not identical, they are not patentably distinct from each other because both applications refer to a method of making a hydrophobic silica aerogel, comprising the steps of: preparing a first solution by mixing methyl silicate 51 and methanol; preparing a second solution by mixing methanol, ammonium hydroxide and water; mixing the first solution and the second solution together to form a mixed solution; allowing components in the mixed solution to react to form silica wet gel; aging the silica wet gel for a period of time; preparing a third solution by mixing methyltrimethoxysilane and methanol; adding the third solution to the silica wet gel; allowing the third solution to react with the silica wet gel to form hydrophobic silica wet gel; and drying the hydrophobic silica wet gel to form hydrophobic silica aerogel; wherein the methyl silicate 51 has a total weight percent of greater than or equal to 1.8% and less than or equal to 4.8% and the methyltrimethoxysilane has a total weight percent of greater than or equal to 0.39% and less than or equal to 0.8%, wherein total weight percent represents a total weight percent of a component in the first, second and third solutions
Conclusion
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/FARAH TAUFIQ/ Primary Examiner, Art Unit 1754
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