Prosecution Insights
Last updated: April 19, 2026
Application No. 18/066,106

CHEMICAL VACUUM DEPOSITION OF A THIN TUNGSTEN AND/OR MOLYBDENUM SULFIDE FILM METHOD

Final Rejection §102§103§112
Filed
Dec 14, 2022
Examiner
ZHANG, HAI Y
Art Unit
1717
Tech Center
1700 — Chemical & Materials Engineering
Assignee
COMMISSARIAT À L'ÉNERGIE ATOMIQUE ET AUX ÉNERGIES ALTERNATIVES
OA Round
2 (Final)
68%
Grant Probability
Favorable
3-4
OA Rounds
3y 1m
To Grant
99%
With Interview

Examiner Intelligence

Grants 68% — above average
68%
Career Allow Rate
215 granted / 318 resolved
+2.6% vs TC avg
Strong +43% interview lift
Without
With
+43.4%
Interview Lift
resolved cases with interview
Typical timeline
3y 1m
Avg Prosecution
17 currently pending
Career history
335
Total Applications
across all art units

Statute-Specific Performance

§101
0.5%
-39.5% vs TC avg
§103
40.1%
+0.1% vs TC avg
§102
23.9%
-16.1% vs TC avg
§112
25.8%
-14.2% vs TC avg
Black line = Tech Center average estimate • Based on career data from 318 resolved cases

Office Action

§102 §103 §112
DETAILED ACTION The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA . 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 Applicant’s amendment filed on September 03, 2025 was received. Claims 1-2, 8, 12, 13, 15, 17 were amended. The text of those sections of Title pre-AIA 35, U.S.C. code not included in this action can be found in the prior Office Action issued on June 03, 2025. Claim Interpretation The limitation in claim 1 “draining said gaseous mixture” is interpreted as passing inert gas, because Applicant defining “draining step d) is carried out by passage of an inert gas, in particular argon and/or helium and/or dinitrogen” ([0037] [0052]). The limitation in claim 2, “wherein step c) leads to the formation on the substrate of tungsten and/or molybdenum nitride”, the molybdenum nitride is formed by intruding nitrogen gas in to the molybdenum contained chamber as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”. Claim Objections The objection on claim 1 was withdrawn, because the claim has been amended. Claim Rejections - 35 USC § 112 The claim rejections under 35 U.S.C. 112 (b), or 35 U.S.C. 112 (pre-AIA ), second paragraph, on claims 1-14 are 16-20 are withdrawn, because the claims have been amended. Claim 15 is 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 pre-AIA the applicant regards as the invention. Regarding claim 15, the phrase "such as" renders the claim indefinite because it is unclear whether the limitations following the phrase are part of the claimed invention. See MPEP § 2173.05(d). Claim Rejections - 35 USC § 102 The claim rejections under 35 U.S.C. 102(a)(1) as being anticipated by He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) on claims 1-5, 8-12, 14 and 16-17 are withdrawn, because the claims have been amended. Support of amendment can be found in paragraphs [0021], [0055], [0089], [0107]). Claims 1-5, 8-12, 14 and 16-17 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) and as evidenced by Joo et al. (NPL titled: Atomic layer deposited Mo2N thin films using Mo(CO)6 and NH3 plasma as a Cu diffusion barrier, attached). Regarding claim 1, He teaches a method of preparing Molybdenum disulfide (MoS2) film on a surface of a substrate in the atomic layer deposition (ALD) system in the reaction chamber (as evidenced by Lee in paragraph [0011], the atomic layer deposition (ALD) is under a vacuum chamber) (Abstract, [0011], Lee: [0011]), comprising a) introducing the substrate in ALD deposition chamber (reads on a reactional chamber under vacuum as evidenced by Lee:[0011]), at a substrate temperature of 400°C for example ([0024], Lee: [0011]); b) preparing the substrate comprising the injection of dinitrogen for example ([0024]); c) injecting, into the reactional chamber, a gaseous mixture comprising an Mo hexacarbonyl and a nitrogen gas or a gas mixture comprising at least one nitrogen, and Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/SH (CH2) 2 SH (ethanedithiol) pulse/high purity nitrogen purge is equal to (2s/5s/2s/5s/0.5s/5s), which can form molybdenum nitride in reaction with a molybdenum hexacarbonyl for example as evidenced by Joo, Mo(CO)6 and NH3 plasma are used to establish an efficient ALD process to prepare molybdenum nitride thin films ([0024], Joo abstract, page 9, section 4, conclusion, as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”); d) passing nitrogen gas (reads on draining said gaseous mixture as defined by Applicant in [0037] and [0052] “draining step d) is carried out by passage of an inert gas, in particular argon and/or helium and/or dinitrogen”) ([0024]); and contacting the treated substrate such as obtained from step c) with a sulphurous gas comprising at least one free thiol group or forming a reactional intermediary comprising at least one free thiol group, such as SH (CH2)2 SH (ethanedithiol) to form on the substrate, a layer comprising the compound of formula MoS2 for example ([0024]). Regarding claim 3, He teaches wherein the substrate is Si for example ([0024]). Regarding claim 4, He teaches wherein at least one of the steps or all of the steps is/are carried out at a temperature of 400°C for example ([0024]). Regarding claim 5, He teaches wherein: the gas of step b) is nitrogen gas (dinitrogen) is carried out for 5s for example ([0024]). Regarding claim 8, He teaches wherein step c) is carried out for a duration of 2 to 20 seconds ([0024]), and a nitrogen gas or a gas mixture comprising at least one nitrogen, and Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/SH (CH2) 2 SH (ethanedithiol) pulse/high purity nitrogen purge is equal to (2s/5s/2s/5s/0.5s/5s), which can form molybdenum nitride in reaction with a molybdenum hexacarbonyl for example as evidenced by Joo, Mo(CO)6 and NH3 plasma are used to establish an efficient ALD process to prepare molybdenum nitride thin films ([0024], Joo abstract, page 9, section 4, conclusion, as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”). Regarding claim 9, He teaches wherein the draining step d) is carried out: by passage of nitrogen gas (an inert gas) ([0024]). Regarding claim 10, He teaches wherein the sulphurous gas is SH (CH2)2 SH (ethanedithiol) for example ([0024]). Regarding claim 11, He teaches wherein step e) is carried out: in the presence of nitrogen gas (an inert carrier gas) ([0024]). Regarding claim 12, He teaches wherein step e) is: carried out for a duration of 1 to 20 seconds ([0024]). Regarding claim 14, He teaches wherein step e) can followed by an annealing step ([0005]). Regarding claim 16, He teaches wherein x is 2 (is greater than 1.7) for example (Abstract, [0024]). Regarding claim 17, He teaches wherein the gaseous mixture comprises at least one hydrogen element ([0024), and a nitrogen gas or a gas mixture comprising at least one nitrogen, and Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/Mo (CO) 6 (molybdenum hexacarbonyl) pulse/high purity nitrogen purge/SH (CH2) 2 SH (ethanedithiol) pulse/high purity nitrogen purge is equal to (2s/5s/2s/5s/0.5s/5s), which can form molybdenum nitride in reaction with a molybdenum hexacarbonyl for example as evidenced by Joo, Mo(CO)6 and NH3 plasma are used to establish an efficient ALD process to prepare molybdenum nitride thin films ([0024], Joo abstract, page 9, section 4, conclusion, as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”). Claim Rejections - 35 USC § 103 The claim rejections under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) as applied to claims 1-5, 8-12, 14 and 16-17, and further in view of Myo (US 2008/0099147 A1) on claims 6 and 18 are withdrawn, because the independent claim has been amended. The claim rejections under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) as applied to claims 1-5, 8-12, 14 and 16-17, and further in view of Robin (US 2014/0235014 A1) on Claim 7 is withdrawn, because the independent claim has been amended. The claim rejections under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) as applied to claims 1-5, 8-12, 14 and 16-17, and further in view of Robin (US 2014/0235014 A1) and Myo (US 2008/0099147 A1) on claims 13 and 19-20 are withdrawn, because the independent claim has been amended. Claims 2, 6 and 18 are rejected under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) and as evidenced by Joo et al. (NPL titled: Atomic layer deposited Mo2N thin films using Mo(CO)6 and NH3 plasma as a Cu diffusion barrier, attached) as applied to claims 1, 3-5, 8-12, 14 and 16-17, and further in view of Myo (US 2008/0099147 A1). Regarding claim 2, He teaches introducing nitrogen gas in to the reaction chamber containing molybdenum compound which reads on the formation of molybdenum nitride on the substrate in step c), step e) being carried out under sulphurous gas saturation to totally or substantially convert the molybdenum nitride formed from step c) into the compound of formula ([0024], as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”). He doesn’t explicitly teach so that a residual nitrogen rate of the layer obtained from step e) is less than 5 atomic%. However, examiner interprets the reference as a teaching that disclosed the residual nitrogen rate of the layer obtained from step e) is too big, the final product crystallinity will be affected ([0005). Therefore, it would have been obvious to one of ordinary skill in the art at the time the invention to have a residual nitrogen rate of the layer obtained from step e) is less than 5 atomic% in He, because He teaches the removing residual content to improve the crystallinity is obtained by optimizing the residual nitrogen rate of the layer obtained from step e) is less than 5 atomic%. Discovery of optimum value of result effective variable in known process is ordinarily within skill of art. In re Boesch, CCPA 1980, 617F.2d 272,205 USPQ215 Regarding claim 6, He teaches a deposition method using ALD as disclosed above. He does not explicitly teach wherein the substrate is: a silicon nitride or a metal nitride, and step b) is carried out without plasma, the gas of step b) being, dihydrogen, a dihydrogen-argon mixture, ammoniac, a dinitrogen- dihydrogen mixture, a dinitrogen-ammoniac mixture, a dihydrogen-ammoniac mixture, helium, a dihydrogen-helium mixture, or an argon-helium mixture. However, an analogous art, Myo teaches deposition method by ALD on silicon or silicon nitride for examples without plasma process with nitrogen or helium as carrier gases for examples ([0036]). Silicon and silicon nitride are considered functionally equivalent substrate in ALD process, and nitrogen and helium are considered functionally equivalent carrier gases in ALD process ([0036]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to substitute silicone nitride substrate for silicon substrate disclosed by He, and to substitute or comprising helium as carrier gases with nitrogen gas disclosed by He. Regarding claim 18, He teaches a deposition method as disclosed above. He does not explicitly teach wherein step b) is carried out under plasma enhancement, in the presence of dihydrogen, argon and/or helium. However, an analogous art, Myo teaches deposition method wherein gases can be heated and/or energized to form a plasma ([0004]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply heating and/or energizing to form a plasma to the method of coating in He, because Myo disclosed this is a generally semiconductor processing ([0004]). Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) and as evidenced by Joo et al. (NPL titled: Atomic layer deposited Mo2N thin films using Mo(CO)6 and NH3 plasma as a Cu diffusion barrier, attached) as applied to claims 1, 3-5, 8-12, 14 and 16-17, and further in view of Robin (US 2014/0235014 A1). Regarding claim 7, He teaches a deposition method using ALD as disclosed above. He does not explicitly teach wherein the vacuum is a primary or secondary vacuum. However, an analogous art, Robin teaches deposition method by ALD for example, which is accomplished within a chamber in which a primary or higher vacuum is present ([0118]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply a primary or higher vacuum chamber in the ALD process to the method of coating in He, because Robin disclosed such a vacuum is important for the dielectric properties ([0120]). Claims 13 and 19-20 are rejected under 35 U.S.C. 103 as being unpatentable over He et al. (CN 107740069 A with English translation attached) as evidenced by Lee et al. (US 2004/0007179 A1) and as evidenced by Joo et al. (NPL titled: Atomic layer deposited Mo2N thin films using Mo(CO)6 and NH3 plasma as a Cu diffusion barrier, attached) as applied to claims 1, 3-5, 8-12, 14 and 16-17, and further in view of Robin (US 2014/0235014 A1) and Myo (US 2008/0099147 A1). Regarding claim 13, He teaches a deposition method using ALD as disclosed above and which comprises the following steps: a) a step of introducing the substrate into reactional chamber under vacuum, at a substrate temperature of 400°C for example ([0024]); b) a step of preparing the substrate comprising the injection of a nitrogen (dinitrogen) gas, for a duration of 2 to 900 seconds ([0024]); c) a step of injecting, into the reactional chamber, a gaseous mixture comprising an Mo hexacarbonyl for a duration of 2 to 20 seconds ([0024]); d) a step of draining said gaseous mixture by passage of an inert gas ([0024]); e) a step of contacting the treated substrate obtained from step c) with a with a sulphurous gas comprising at least one free thiol group or forming a reactional intermediary comprising at least one free thiol group, chosen from SH (CH2)2 SH (ethanedithiol) (ethane-1,2-dithiol (EDT)), to form on the substrate, a layer comprising the compound of formula MoS2, in the presence of an inert carrier gas, and/or under plasma activation, for a duration of 1 to 20 seconds ([0024]). He does not explicitly teach wherein the vacuum is a primary vacuum. However, an analogous art, Robin teaches deposition method by ALD for example, which is accomplished within a chamber in which a primary or higher vacuum is present ([0118]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply a primary vacuum chamber in the ALD process to the method of coating in He, because Robin disclosed such a vacuum is important for the dielectric properties ([0120]). He does not explicitly teach comprising NH3. However, an analogous art, Myo teaches deposition method by ALD for example, which is comprising NH3 as a reducing compound ([0036]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply a reducing compound NH3 in the ALD process to the method of coating in He, because Myo disclosed a reducing compound is including in the ALD process when depositing a metal compound ([0036]). He doesn’t explicitly draining said gaseous mixture by passage of an inert gas, for a duration less than or equal to 2 seconds. However, He recognizes the duration of passing the inert gas for draining is adjusted by changing the flow rate of passing the inert gas for example ([0024]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to adjust the duration of passing the inert gas for draining to yield a good deposition process ([0024]). Discovery of optimum value of result effective variable in know process is ordinarily within skill of art. In re Boesch, CCPA 1980, 617 F.2d 272, 205 USPQ215. Regarding claim 19, He teaches a deposition method using ALD as disclosed above. He doesn’t explicitly draining said sulphurous gas by passage of an inert gas for a duration less than or equal to 2 seconds. However, He recognizes the duration of passing the inert gas for draining is adjusted by changing the flow rate of passing the inert gas for example ([0024]). Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to adjust the duration of passing the inert gas for draining to yield a good deposition process ([0024]). Discovery of optimum value of result effective variable in know process is ordinarily within skill of art. In re Boesch, CCPA 1980, 617 F.2d 272, 205 USPQ215. Regarding claim 20, He teaches setting circulation number accurately controlling the thickness of the MoS2 film which reads on wherein steps b) to f) are renewed, until obtaining the desired number of sheets ([0018], [0031]). Response to Arguments Applicant's arguments filed on September 03, 2025 have been fully considered but they are not persuasive. Applicant’s principal arguments are He doesn’t teach a gas or a gas mixture comprising at least one nitrogen, and which can form tungsten nitride and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or a molybdenum hexacarbonyl. In response to Applicant’s arguments, please consider the following comments. In response to Applicant’s arguments, the examiner respectfully disagrees. a gaseous mixture comprising an Mo hexacarbonyl and a nitrogen gas or a or a gas mixture comprising at least one nitrogen, and which can form molybdenum nitride in reaction with a molybdenum hexacarbonyl for example as evidenced by Joo, Mo(CO)6 and NH3 plasma are used to establish an efficient ALD process to prepare molybdenum nitride thin films ([0024], Joo abstract, page 9, section 4, conclusion). the molybdenum nitride is formed by intruding nitrogen gas in to the molybdenum contained chamber as disclosed by Applicant in paragraphs [0088] and [0089] “any gas comprising at least one nitrogen and which can form tungsten and/or molybdenum nitride in reaction with a tungsten hexacarbonyl and/or an Mo hexacarbonyl”. Conclusion Applicant’s amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a). A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any extension fee 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 HAI YAN ZHANG whose telephone number is (571)270-7181. The examiner can normally be reached on MTTHF. If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, DAH-WEI YUAN can be reached on 571-272-1295. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300. Information regarding the status of an application may be obtained from the Patent Application Information Retrieval (PAIR) system. Status information for published applications may be obtained from either Private PAIR or Public PAIR. Status information for unpublished applications is available through Private PAIR only. For more information about the PAIR system, see http://pair-direct.uspto.gov. Should you have questions on access to the Private PAIR system, contact the Electronic Business Center (EBC) at 866-217-9197 (toll-free). If you would like assistance from a USPTO Customer Service Representative or access to the automated information system, call 800-786-9199 (IN USA OR CANADA) or 571-272-1000. /HAI Y ZHANG/ Primary Examiner, Art Unit 1717
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Prosecution Timeline

Dec 14, 2022
Application Filed
May 31, 2025
Non-Final Rejection — §102, §103, §112
Sep 03, 2025
Response Filed
Dec 14, 2025
Final Rejection — §102, §103, §112 (current)

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Prosecution Projections

3-4
Expected OA Rounds
68%
Grant Probability
99%
With Interview (+43.4%)
3y 1m
Median Time to Grant
Moderate
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