DETAILED ACTION
Continued Examination Under 37 CFR 1.114
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on April 4, 2026 has been entered.
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office 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 amendment filed on April 4, 2026, claims 1 – 3 are pending. Claim 1 has been amended and claims 4 has been canceled.
Claim Rejections - 35 USC § 103
The rejections of the claims under 35 USC § 103 in the previous Office Action are withdrawn due to Applicant amendment.
Claim(s) 1 – 3 is/are rejected under 35 U.S.C. 103 as being unpatentable over Sakurai et al. US2007/0122947 A1 (hereafter “Sakurai”) in view of Jones US 2005/0008781 A1 (hereafter “Jones”) and Okada et al. WO 2019/044448 A1 (with US 2020/0140463 A1 acting as the official translation and referenced herein, hereinafter “Okada”) , and optionally in view of Cremers et al. “Conformality in atomic layer deposition: current status overview of analysis and modelling”. Appl. Phys. Rev. 6, 021302 (2019) https://doi.org/10.1063/1.5060967.
Regarding claims 1, 3:
Sakurai discloses a method of producing a thin film containing zirconium on a surface of a substrate by ALD [0036] comprising: a step 1 of causing a raw material gas to adsorb to the surface of the substrate [0025]; a step 2 of evacuating the raw material gas remaining unreacted [0085]; and a step 3 of causing the precursor thin-film to react with a reactive gas at a temperature of 250°C – 800°C, such as 300°C, and a reaction pressure between 10 Pa to atmospheric pressure for thermal CVD methods and 10Pa to 2000Pa for plasma CVD methods; e.g. 1300 – 1400 Pa for a precursor material and a system pressure of less than 1300 Pa for reaction with a water vapor reactant ([0037], [0081]). Sakurai expressly teaches that atomic layer deposition is a type of chemical vapor deposition wherein the deposition reaction of CVD is divided into elementary reaction steps ([0036]). Sakurai discloses that the reactive gas is an oxidizing gas, such as water vapor [0086], ozone, or oxygen to form a zirconium oxide film [0032]. The raw material includes a compound represented by a general formula ([0012]):
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wherein R1, R2, R3, and R4 each represent an alkyl group having 1 to 4 carbon atoms; A represents an alkanediyl group having 1 to 8 carbon atoms; M represents a lead atom, a titanium atom or a zirconium atom; n represents 2 when M is a lead atom or 4 when M is a titanium or zirconium atom. Examples of the raw material include ([0019]):
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zirconium tetrakis (1-dimethylamino) -2- methyl -2- propanolate
Zirconium tetrakis (1-dimethylamino) -2- methyl -2- butanolate
Sakurai also discloses as a comparative compound the structure:
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Zirconium tetrakis (1-dimethylamino)-2-propanolate
where the comparative compound is the same as that recited in present claim 1. Sakurai further discloses that the comparative compound would be less suitable as a precursor chemical vapor deposition compared to the inventive compounds of Sakurai, implying that the comparative compound can be used in the process of Sakurai to produce a film by CVD1.
Sakurai generally does not teach the practice of the recited steps of the claimed method using Zirconium tetrakis (1-dimethylamino)-2-propanolate; that the pressure of the film forming chamber at the time of causing the precursor thin-film to react with the reactive gas is at 10Pa or more and 1000Pa or less; and that the residual carbon content in the thin film is less than 0.01 atm%.
With regards to the practice of the recited steps of the claimed method using Zirconium tetrakis (1-dimethylamino)-2-propanolate:
Jones is directed to inter alia zirconium precursors for use in metalorganic chemical vapor deposition (MOCVD) and alternatively atomic layer deposition techniques (Abstract; [0018]). Jones discloses precursors having the general formula: M(Lx)[OCR1(R2)CH2X]4-x
Wherein M may be zirconium, L is a generic ligand, X is selected from OR and NR2 wherein R is an alkyl group or a substituted alkyl group, R1 is hydrogen or an alkyl group, R2 is an alkyl group that may be optionally substituted, and subscript x is between 0 to 3 ([0007] – [0009]). The general formula therefore encompasses, when x is 0, compounds of the formula:
M[OCR1(R2)CH2X]4
Although not specifically disclosed, the general formula encapsulates Zr[OCHMeCH2NEt2]4 (Zirconium tetrakis (1-dimethylamino)-2-propanolate, where M is Zr, x is 0, R1 is H, R2 Is a methyl (unsubstituted) group, and X is NR2 where R2 are alkyl groups) ([0007]).
Jones further discloses that a preferred ligand OCHButCH2NEt2 that is encompassed by formula [OCR1(R2)CH2X] ([0011], [0016]).
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Jones discloses that precursors encompassed by the recited general formula provide stable and volatile Zr precursors and is effective in inhibiting oligomerization in Zr alkoxide complexes ([0006]). While Jones discloses an alkoxide species where R1 of the claimed general formula would be a 4-carbon group, the Examiner notes that the Jones allows for an R2 (mapping to R1 in the present claim 1) to be a 1-carbon to 3-carbon group.
Therefore, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have modified the method of Jones to practice of the recited steps of the claimed method using Zirconium tetrakis (1-dimethylamino)-2-propanolate because Sakurai suggests the performance of such steps using Zirconium tetrakis (1-dimethylamino)-2-propanolate, Jones teaches that such precursors have enhanced stability and volatility which can inhibit precursor oligomerization, and because Jones teaches a preferred species that is chemically similar to the claimed species (e.g. where R1 is a propyl group or an ethyl group in combination of R2 being hydrogen) that would have such an enhanced stability and volatility. Where such a prior art species or subgenus is structurally similar to that claimed, its disclosure may provide a reason for one of ordinary skill in the art to choose the claimed species or subgenus from the genus, based on the reasonable expectation that structurally similar species usually have similar properties. See, e.g., In re Dillon, 919 F.2d 688, at 693, 696, 16 USPQ2d at 1901, 1904. See also In re Deuel, 51 F.3d 1552, 1558, 34 USPQ2d 1210, 1214 (Fed. Cir. 1995).
With regards to the pressure of the film forming chamber at the time of causing the precursor thin-film to react with the reactive gas is at 10Pa or more and 1000Pa or less.
As discussed above, Sakurai discloses that the reaction pressure during a CVD reaction, including ALD reactions, may be between 10 Pa to atmospheric pressure for thermal CVD methods and 10Pa to 2000Pa for plasma CVD methods. In an example embodiment, Sakurai discloses that the system pressure during reaction of a previously-deposited CVD precursor with a water vapor reactant may be any pressure under 1300 Pa ([0037], [0081]).
Additionally, Sakurai discloses that the reaction pressure affects deposition rates via material feed conditions, including the material feed condition of reactive gases ([0037]).
In the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art”, a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990); In re Geisler, 116 F.3d 1465, 1469-71, 43 USPQ2d 1362, 1365-66(Fed. Cir. 1997). See MPEP 2144.05.
Additionally, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have implemented an embodiment of Sakurai in view of Jones or otherwise have modified the method of Sakurai in view of Jones to set the pressure of the film forming chamber at the time of causing the precursor thin-film to react with the reactive gas at 10Pa or more and 1000Pa or less as a matter of routine experimentation in order to establish, in conjunction with the number of deposition cycles, the deposition rate of the full coating, and therefore time spent depositing material.
Optionally and additionally, Cremers is directed to the general knowledge of one of ordinary skill in the art concerning conformality in ALD (Abstract; 021302-3). Cremers discloses that the pressure regime for ALD deposition can range from 10-4 Pa to near-atmospheric pressure depending on reactor design (page 021302-4) 2nd col – page 7 1st col). Cremers additionally discloses that the reactor pressure plays a crucial role in ALD processes since it determines the impinging flux of reactant molecules on a given substrate; reactant exposure is a function of both the reactor pressure and the amount of time a substrate is exposed to a given reactant (page 021302-5). Total exposure is optimized to allow for effective deposition and conformality while compensating for substrate-dependent diffusion limitations and the particular reaction mechanisms and sticking probabilities between a given reactant-substrate interaction (page 021302-5 to 021302-6, page 02302-15, page 021302-19 2nd column).
Additionally and optionally as taught by Cremers, in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art”, a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990); In re Geisler, 116 F.3d 1465, 1469-71, 43 USPQ2d 1362, 1365-66(Fed. Cir. 1997). See MPEP 2144.05.
Additionally and optionally as taught by Cremers, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have implemented an embodiment of Sakurai in view of Jones or otherwise have modified the method of Sakurai in view of Jones to set the pressure of the film forming chamber at the time of causing the precursor thin-film to react with the reactive gas at 10Pa or more and 1000Pa or less as a matter of routine experimentation in order to optimize material deposition and conformality of the deposited material for a given ALD reactor design as taught by Cremers.
With regards to the residual carbon content in the thin film being less than 0.01 atm%.
Okada is directed to metal alkoxide compounds represented by:
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where M is a lanthanum group atom, e.g. scandium; R1 is hydrogen or a C1-4 alkyl group, R2 is an isopropyl group, s-butyl group, t-butyl group, s-pentyl group, ethylpropyl group or t-pentyl group; R3 is hydrogen or a C1-4 alkyl group; and R4 is a C1-4 alkyl group; and films formed from such compounds in a CVD deposition process, including an ALD deposition process (Abstract; [0010]; [0041], [0044]). Similar to the claimed compound, Okada discloses specific compounds having similar alkoxide ligands ([0023] Compound No. 3, Compound No. 7, Compound No. 11, Compound No. 47, 48). Okada discloses that precursor materials should have minimal contaminants ([0039]); that the production conditions include substrate temperatures between e.g. 200°C to 350°C ([0046], [0050]); and pressures between e.g. 10 Pa to 1000 PA ([0046], [0050]).
Okada further discloses examples of the production of yttrium oxide thin films by atomic layer deposition using a disclosed compounds ([0106] – [0108]) under conditions including reaction at 250 °C and system pressure of 100 Pa ([0108] – [0111], [0114] – [0116]). Like Jones, Okada’s disclosed compounds have in common alkoxide ligands where the alpha carbon – adjacent to the oxygen atom – are bonded with a hydrogen atom and an alkyl group. Okada discloses that the films created by their embodied methods have a residual carbon content smaller than 1.0 atom%. Finally, Okada discloses that the disclosed compounds are to result in compounds having a small residual carbon content and high quality, i.e. a motivation to minimize carbon in resultant films ([0052]).
In view of the prior art as a whole, it would have been obvious to one of ordinary skill before the effective filing date of the claimed invention to have recognized or validate that the process of Sakurai in view of Jones would render a film with a residual carbon content in the thin-film be less than 0.01 atom % (atm%), or otherwise would have modified the conditions of the reaction (such as substrate temperature) disclosed in Sakurai to render such a film because Okada teaches a desire to minimize carbon content in oxide films, and Okada also suggests a reasonable expectation of success to achieve such a low residual carbon content with precursors having an alkoxide ligand with a hydrogen atom bound to the alpha carbon within the claimed reaction conditions.
Regarding Claim 2:
Sakurai discloses that step 1 is performed under a substrate temperature of 250°C-800°C [0037], such as 300°C [0081].
Response to Arguments
Applicant’s arguments, filed April 4, 2026, with respect to the rejection(s) of the claim(s) under 35 USC 103 have been fully considered and are persuasive. Therefore, the rejection has been withdrawn. However, upon further consideration, a new ground(s) of rejection is made in view of Okada.
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to JOSE I HERNANDEZ-KENNEY whose telephone number is (571)270-5979. The examiner can normally be reached M-F 6:30-3:30.
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/JOSE I HERNANDEZ-KENNEY/
Primary Examiner
Art Unit 1717
1 "[I]n considering the disclosure of a reference, it is proper to take into account not only specific teachings of the reference but also the inferences which one skilled in the art would reasonably be expected to draw therefrom." In re Preda, 401 F.2d 825, 826, 159 USPQ 342, 344 (CCPA 1968)
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