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 .
Priority
Receipt is acknowledged of certified copies of papers required by 37 CFR 1.55.
Response to Amendment
The amendment filed on 04/24/2026 has been entered. Claims 1-21 are pending in the application. Claims 1-14 are withdrawn. Applicant’s amendments to the claims have not introduced new matter and are supported in the specification in at least [0001], [0007], [0049], and [0106].
Applicant’s amendments to the claims have overcome every Claim Objection and most of the 112(b) rejections previously set forth in the office action mailed 01/26/2026. However, the amendments have introduced new 112(b) issues, set forth below.
Response to Arguments
Applicant’s arguments, see Pg. 12-14 filed 204/24/2026 with respect to claim 15, have been fully considered however are solely directed to the claim limitation “without chemical reactions” introduced in the amendment filed 04/24/2026, which postdates the non-final rejection mailed 01/26/2026.
Upon further search and consideration and as necessitated by the amendment, the 35 U.S.C. 103 rejection of 01/26/2026 as being unpatentable over Reed et al. (US20120107224A1) in view of Isaka et al. (JP4996016B2 English), with evidentiary support provided by USGS pH Scale (2019) is updated. Details regarding this limitation are discussed further in the 112 and 103 sections below.
Applicant's remaining arguments filed 04/24/2026 have been fully considered but they are not persuasive.
Applicant argues on Pg. 14-15 that the secondary reference Isaka ‘016 describes preferred melting/boiling points of the dispersion medium and that a skilled artisan would not recognize this as an indication of the temperature during a grinding step. Applicant argues this is only a disclosure of the physical properties of the dispersion medium and not an indication of the temperature during the grinding step.
However, Isaka further teaches in [0019] that if the temperature of the dispersion medium does not melt above at least about 5 °C then danger is increased and heating may be required (i.e. temperature exceeding 5 °C would be required during pulverization). Isaka further teaches that at the high end, if the dispersion medium does not boil above 70 or particularly less than 50 °C, then the vapor pressure can become too high during pulverization, which is also dangerous. Accordingly, Isaka directs a skilled artisan to maintain temperatures during pulverization between about 5 and 70 °C, where too low of temperature require additional heating while too high of temperatures can boil off the dispersion medium, both of which can increase danger.
Applicant argues on Pg. 15 that the secondary references cited for claim 21 do not show why a skilled artisan would have arrived at a niobium nanoparticle process and that they fail to remedy the core deficiency of Reed.
However, in response to applicant's arguments against the references individually, one cannot show nonobviousness by attacking references individually where the rejections are based on combinations of references. See In re Keller, 642 F.2d 413, 208 USPQ 871 (CCPA 1981); In re Merck & Co., 800 F.2d 1091, 231 USPQ 375 (Fed. Cir. 1986). As outlined below and stated by Applicant on Pg. 15 of the remarks, the secondary references are applied to disclose various jet-milling parameters and are not being applied to teach the process of claim 15. Each secondary reference combination has motivation provided as to why a skilled artisan would arrive at that particular parameter.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 15-21 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention.
Claim 15, lines 1-2, the term “without chemical reactions” is not clear. Examiner notes the term language is supported in at least [0001], [0007], [0049], and [0106] of the instant specification however the scope of the term is indefinite. The term is indefinite because claims 16 and 19 require performing pH adjustment, which is acid/base reaction chemistry. Therefore, the term “without chemical reactions” is indefinite because it appears to be including pH balancing acid/base reactions while attempting to exclude other processes of which a skilled artisan viewing the disclosure would not be apprised of. For example, it is not clear if acid treatment of the powder during comminution would be considered a “chemical reaction” in the context of the claim. To the best of Examiner’s knowledge, the chemical reactions being avoided by the method are not clearly outlined in the instant specification, further supporting the position that the term “without chemical reactions” is not clear. In the interest of compact prosecution, the term is interpreted such that a process performed without additional processes outside of comminution of niobium feed particles meets the claim language. This is interpreted from at least [0001], [0007], [0049], and [0106] of the instant specification.
Claim 16, line 3, the phrase “the range from 2 to 13” lacks antecedent basis and is unclear. Claim 15 does not discuss a polar liquid pH range and therefore “the range” does not have antecedent basis.
Claims 16-21 depend from claim 15 and thus are also rejected.
Appropriate correction is required.
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 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 15-20 are rejected under 35 U.S.C. 103 as being unpatentable over Reed et al. (US20120107224A1) in view of Isaka et al. (JP4996016B2 English), with evidentiary support provided by USGS pH Scale (2019) and as outlined in the rejection of claims 15, 16, and 19.
Regarding claim 15, Reed teaches a process for producing niobium powders, comprising niobium metal, niobium oxide, and niobium suboxides, by high-energy ball milling in order to provide niobium particles within the sub-micron (i.e. nanoparticle) to micron range (Abstract; [0040]; [0072]; [0084]; [0088]). Claim 1 describes two options for the comminution conditions, selected from high-energy milling or jet milling. Reed teaching milling with a high-energy mill meets the “high-energy mill” option.
Reed teaches the process includes treating samples of niobium pentoxide with a vacuum heat treatment that comprises evacuating a furnace containing the niobium pentoxide, admitting Argon to a pressure of 0.11 torr, and heating the sample to 1450 °C prior to passivation with air ([0229]). Following this treatment, agglomerated niobium pentoxide particles were milled with water to reduce the particle size ([0230]). As stated above, term “niobium nanoparticles” and “niobium particles” are interpreted according to the definition provided in the instant specification in [0071] that defines “niobium particles” as encompassing “various chemical entities containing Niobium, including Niobium metal, oxides, hydrates, hydrides, carbides, or nitrides of Niobium, Niobium iron or Niobium bonded to other metals or transition metals, or combinations thereof. It also includes Niobium Pentoxide.” As such, Reed teaching providing niobium pentoxide in Example 7 meets the limitation.
Furthermore, regarding the term “without chemical reactions,” Reed teaches a process that includes comminution of a niobium-containing feedstock with water addition (see at least [0229]-[0230]). Reed teaches other examples that can include a heat treatment in an inert atmosphere containing hydrogen that causes thermal agglomeration ([0115]-[0117]). Reed teaches the heat treatment is conducted under inert conditions, where the heat is serving to reduce the niobium oxide particles and that the milling treatment can include granulating the starting niobium oxide, the niobium powder, both the starting niobium oxide and the niobium powder either separately before the mixing or as the powder mixture, or the oxygen reduced niobium oxide after formation ([0072]). Performing comminution of a niobium-containing feedstock in the presence of water to obtain sub-micron (i.e. nanometric) particles is consistent with performing a process “without chemical reactions,” as detailed in this section as well as the 112(b) section, and meets the claim limitation.
Reed further teaches the milling treatment is a wet process performed in water where niobium powder and water are mixed prior to adding milling media with a size ranging from 3/16” to 1/32” (i.e. 4.76 mm to 0.79 mm) and milling at 350 rpm or higher ([0076]-[0077]; [0087]-[0088]). Water is a polar liquid and is acknowledged as such in [0127] of the instant specification. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the ranges taught by Reed (milling media 0.79 mm to 4.76 mm; milling speed 350 rpm or higher) overlaps with the claimed ranges (5 µm to 1.3 mm grinding balls; rotation speed 500 to 4500 rpm). Therefore, the ranges in Reed render obvious the claimed ranges.
Reed teaching the milling occurs in water is considered to meet the limitation “stabilize the suspension until obtaining a stable colloidal suspension”. This conclusion is based on [0051] of the instant specification and claim 16 that describe stabilization of the colloidal suspension as requiring adjusting the pH of the polar liquid medium to the range from 2 to 13. Water is known to have a pH of 7, as evidenced by USGS pH Scale (Pg. 1), and accordingly the teaching of Reed of a mixture of niobium particles and water meets this criteria and would provide a stable colloidal suspension with a pH within the range of 2 to 13. See MPEP 2112.II.
Reed further teaches the milling operations can be performed multiple times to arrive at powders with the desired granules size and that the particles can be sub-micron (i.e. nanometric) in size ([0072]; [0074]; [0082]-[0084]; [0088]), meeting the limitation of “comminuting the particles until obtaining niobium preparations with predominantly or entirely nanometric granulometry”.
The claim further requires the method “suspend particles to be comminuted in a liquid, in a concentration between 1 % and 90% m/m” and “grinding the particles at a temperature below 60C” to which Reed is silent.
Isaka teaches a method of preparing a niobium oxide powder slurry that can be used to prepared niobium powders where the slurry is mixed in a mixing ratio of 65 mL-1900 mL per 100 g of niobium oxide powder, where the liquid medium is water (Claims; Abstract; [0006]-[0008]; [0019]). The claimed range of “1% to 90% m/m” is interpreted as a mass percent ratio of niobium to water based on the Examples 1-9 in the instant specification ([0114]-[0167]). Put in terms of the claim, Isaka teaches a ratio from 5.26% to 153% m/m (e.g. 100* (100 g/65 mL) = 153%). Isaka further teaches a pulverization step of the slurry is performed at a temperature higher than 5 °C and lower than 70 °C ([0019]). In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the ranges taught by Isaka (slurry mixture from 5.26% to 153% m/m; temperature higher than 5 °C and lower than 70 °C) overlaps with the claimed ranges (between 1% to 90% m/m; griding at temperatures below 60 °C). Therefore, the ranges in Isaka render obvious the claimed ranges.
Advantageously, performing pulverization within the mixing ratio and temperatures taught by Isaka avoids high viscosity mixtures which make pulverization become too difficult while providing slurries with good fluidity that are easy to sinter and provide fine particles with sharp particle distributions ([0019]; [0047]).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to provide a slurry concentration from 5.26% to 153% m/m and perform pulverization at temperatures higher than 5 °C and lower than 70 °C in the process of Reed in order to avoid high viscosity mixtures and provide slurries with good fluidity that in turn are easy to sinter and provides fine particles with sharp particle distributions, as taught by Isaka.
Regarding claim 16, Reed teaching the milling occurs in water is considered to meet the limitation “stabilize the suspension until obtaining a stable colloidal suspension”. This conclusion is based on [0051] of the instant specification and claim 16 that describe stabilization of the colloidal suspension as requiring adjusting the pH of the polar liquid medium to the range from 2 to 13. Water is known to have a pH of 7, as evidenced by USGS pH Scale (Pg. 1), and accordingly the teaching of Reed of a mixture of niobium particles and water meets this criteria and would provide a stable colloidal suspension. See MPEP 2112.II.
Regarding claim 17, Reed teaches the niobium feedstock material can be subjected to crushing and milling to produce a powder with a size of about 5 to 425 microns ([0079]-[0080]; [0082]). Reed teaches the first milling process of the niobium feedstock can be conducted with ball milling ([0087]). In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the range taught by Reed (5 to 425 microns) overlaps with the claimed range (mean particle size of less than 40 micrometers). Therefore, the range in Reed renders obvious the claimed range.
Regarding claim 18, Reed teaches the first milling process of the niobium feedstock can be conducted with ball milling ([0087]).
Regarding claim 19, Reed teaches the process for producing niobium powders comprises mixing niobium feedstock, comprising niobium pentoxide, with a particle size of about 5 to 425 microns in a high-energy mill, adding water, adding milling media with a ball size ranging from 3/16” to 1/32” (i.e. 4.76 mm to 0.79 mm) and milling at 350 rpm or higher in order to provide niobium particles within the sub-micron (i.e. nanoparticle) to micron range (Abstract; [0040]; [0072]; [0079]-[0080]; [0082]; [0084]; [0088]; [0207]). Reed further teaches the milling operations can be performed multiple times to arrive at powders with the desired granules size and that the particles can be sub-micron (i.e. nanometric) in size ([0072]; [0074]; [0082]-[0084]; [0088]), meeting the limitation of “comminuting the particles until obtaining niobium preparations with predominantly or entirely nanometric granulometry”. Water is known to have a pH of 7, as evidenced by USGS pH Scale (Pg. 1), and accordingly the teaching of Reed overlaps the claimed pH range. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the ranges taught by Reed (5 to 425 microns niobium feedstock comprising niobium pentoxide; pH of 7; milling balls 3/16” to 1/32” (i.e. 4.76 mm to 0.79 mm; pH of about 7 milling at 350 rpm or higher) overlaps with the claimed ranges (micrometric niobium pentoxide particles; pH from 5 to 10; mill balls between 50 µm to 400 µm; rotation speed 2000 to 4000 rpm). Therefore, the ranges in Reed render obvious the claimed ranges.
The claim further requires “grinding the particles at a temperature below 60 °C” to which Reed is silent.
Isaka teaches a method of preparing a niobium oxide powder slurry that can be used to prepared niobium powders where the slurry is mixed with water and pulverized (Claims; Abstract; [0006]-[0008]; [0019]). Isaka further teaches the pulverization step of the slurry is performed at a temperature higher than 5 °C and lower than 70 °C ([0019]). In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the range taught by Isaka (temperature higher than 5 °C and lower than 70 °C) overlaps with the claimed range (grinding at temperatures below 60 °C). Therefore, the range in Isaka renders obvious the claimed range.
Advantageously, performing pulverization within the temperatures taught by Isaka avoids high viscosity mixtures which make pulverization become too difficult while providing slurries with good fluidity that are easy to sinter and provide fine particles with sharp particle distributions ([0019]; [0047]).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to perform pulverization at temperatures higher than 5 °C and lower than 70 °C in the process of Reed in order to avoid high viscosity mixtures and provide slurries with good fluidity that in turn are easy to sinter and provide fine particles with sharp particle distributions, as taught by Isaka.
Regarding claim 20, Reed teaches the high-energy milling is performed with agitation with milling balls of varying ball diameters ([0088]).
The claim further requires “said spheres are selected from zirconia, silicon carbide, alumina, said spheres being optionally stabilized with yttria or niobium pentoxide, or combinations thereof,” to which Reed is silent. Reed teaches using niobium balls ([0088]).
Isaka teaches a process of ball milling a slurry of niobium oxide in water with a ball mill where the balls are made of zirconia (Abstract; [0023]).
Advantageously, zirconia is high density, provides a high grinding efficiency, and transfers less contamination ([0023]).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to use zirconia milling balls in the process of Reed in order to provide a high density material with high grinding efficiency that transfers less contamination, as taught by Isaka.
Claim 21 is rejected under 35 U.S.C. 103 as being unpatentable over Reed et al. (US20120107224A1) in view of Isaka et al. (JP4996016B2 English), with evidentiary support provided by USGS pH Scale (2019) and as outlined in the rejection of claim 15, and further in view of Bludsuss et al. (CA2018346A1), Nied et al. (US8074907) and Benz et al. (Int. J. Miner. Process. 1996, 44-45, 507-519).
Regarding claim 21, Reed in view of Isaka teaches the process of claim 15 and the claim further requires “wherein the jet mill at superheated temperature or steam mill is adjusted with the following parameters: rotation of the air classifier at 20,000 rpm; compressed steam pressure at 50 bar; and temperature of the superheated fluid of 280°C” to which Reed and Isaka are silent.
Bludsuss teaches a method of obtaining niobium oxide powder that includes fine grinding of the material that is carried out in a jet mill (Abstract; Claim 10; Pg. 5, lines 5-19).
Advantageously, performing the process of Bludsuss, including jet milling, provides niobium oxide powders that have a narrow particle size distribution, a large specific surface area, and a very high degree of purity (Pg. 2, lines 23-29).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to perform jet milling in the process of Reed in order to provide a powder with a narrow particle size distribution, large specific surface area, and very high degree of purity, as taught by Bludsuss.
The claim further requires the jet milling is performed “with the following parameters: rotation of the air classifier at 20,000 rpm; compressed steam pressure at 50 bar; and temperature of the superheated fluid of 280°C” to which Reed, Isaka, and Bludsuss are silent.
Nied teaches a method of generating fine particles by jet milling where the process comprises a classifying wheel and superheated steam, where the superheated steam has a pressure of at least approximately 40 bar and a temperature of 200 to 800 °C (Abstract; col. 2, lines 52-59; col. 6, lines 1-10). The term “the superheated fluid” is interpreted as steam present in the “jet mill at superheated temperature” and accordingly steam is considered to teach the limitation of “the superheated fluid”. See at least [0053] in the instant specification. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the ranges taught by Nied (pressure at least 40 bar; temperature 200 to 800 °C) overlaps with the claimed ranges (pressure at 50 bar; temperature of superheated fluid of 280 °C). Therefore, the ranges in Nied render obvious the claimed ranges.
Advantageously, jet milling under the conditions taught by Nied provides very fine particles that are dried in the process (col. 3, lines 59-67; col. 5, line 61-col.6, line 9; col. 9, lines 20-38).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to perform jet milling with superheated steam at a pressure of at least approximately 40 bar and a temperature of 200 to 800 °C in the process of Reed in order to provide very fine powders that are dried in the process, as taught by Nied.
The claim further requires the jet milling classifier is operated with “rotation of the air classifier at 20,000 rpm” to which Reed, Isaka, Bludsuss, and Nied are silent.
Benz teaches a process of performing jet milling on hard materials where the classifier wheel was run between 2,000 to 22,000 rpm (Abstract; Pg. 509, 4. Experimental approach). In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. MPEP 2144.05 (I). In the instant case, the range taught by Benz (2,000 to 22,000 rpm) overlaps with the claimed range (20,000 rpm). Therefore, the range in Benz renders obvious the claimed range.
Advantageously, operating the jet mill classifier at high speeds tends to lead to narrow distribution of particle sizes and can allow for flexibility in the grinding pressure which can alleviate operational costs (Pg. 515, par. 2; Pg. 518, 7. Summary).
Thus, prior to the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to perform jet milling with a classifier operating between 2,000 to 22,000 rpm in the process of Reed in order to provide particles with narrow distributions and allow for flexibility in grind pressures that can reduce operational costs of the mill, as taught by Benz.
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to Jordan Wayne Taylor whose telephone number is (571)272-9895. The examiner can normally be reached Monday - Friday, 7:30 AM - 5 PM EST; Second Fridays Off.
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/JORDAN W TAYLOR/Examiner, Art Unit 1738