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 .
Status of the Claims
Claims 1-14, 16 and 20-22 are pending and rejected. Claims 17 and 18 are withdrawn. Claims 1 and 3-14 are amended. Claims 15 and 19 are cancelled and claims 20-22 are newly added.
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and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114.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 9/4/2026 has been entered.
Claim Objections
Claim 14 is objected to because of the following informalities: lines 2-3 state “the second element (d) to form a third film”, where (d) should be deleted. Appropriate correction is required.
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.
Claim 1-14, 16 and 20-22 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.
Regarding claim 1, the claim recites the limitation "the NH-terminated group" in line 14. There is insufficient antecedent basis for this limitation in the claim. For the purposes of examination, the claim is being interpreted as reading “a NH-terminated group”. Since none of the dependent claims remedy the clarity of claim 1, they are also rendered indefinite. Appropriate action is required without adding new matter.
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 (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 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 1-4, 11-14, 16, and 20-22 are rejected under 35 U.S.C. 103 as being unpatentable over Clark, US 2008/0241382 A1 in view of Ogawa, US 2020/0194269 A1, Kuroda, US 2021/0225643 A1 and Spiegelman, US 2019/0309411 A1.
Regarding claims 1 and 2, Clark teaches a method of processing a substrate (a method for forming a strained metal nitride film on a substrate, abstract), comprising:
(a) supplying a first processing gas containing a first element and a halogen to a substrate (exposing a substrate to a gas pulse of a metal precursor at step 322, 0092 and Fig. 3B, where the metal precursors include those having a metal element and a halogen, 0060, 0061, 0082-0084);
(b) supplying a second processing gas including an N-N bond and an N-H bond to the substrate (exposing the substrate to a gas pulse containing a first nitrogen precursor or a gas pulse containing a first nitrogen precursor and a second nitrogen precursor in a first ratio at step 324, where the first and second nitrogen precursors are selected from gases including ammonia and hydrazine, 0093 and Fig. 3B, such that the process gas will include an N-N bond and an N-H bond in hydrazine so as to provide a second processing gas or in a mixture of hydrazine and ammonia); and
(c) performing (a) and (b) X times, X being a natural number, in a state where the substrate is heated to a temperature of 250°C or lower to form a first film containing the first element (where steps 322 and 324 are repeated a first number of times, 0096 and Fig. 3B, where an example include performing the steps 3, 2, and 1 times so as to provide a natural number of 1 or greater, 0100, and where the temperature of the substrate is controlled in a range from approximately 150°C to 350°C, 0031, so as to overlap the range of claims 1 and 2).
According to MPEP 2144.05, “in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists.”
Clark teaches that the metal halide precursor includes TiCl4 (0060), where the film formed includes titanium nitride (abstract and 0024). They also teach that the film deposited can be a strained metal nitride or metal silicon nitride film (0015).
They do not teach supplying a fourth gas including hydrogen and a second element different from the first element to the substrate, where the fourth gas is provided for a time overlapping step (a).
Ogawa teaches a method of manufacturing a semiconductor device, including forming a metal nitride film substantially not containing a silicon atom on a substrate by sequentially repeating: (a) supplying a metal-containing gas and a reducing gas, which contains silicon and hydrogen and does not contain a halogen, to the substrate in a process chamber, (b) removing the metal-containing gas and the reducing gas that remain in the process chamber, (c) supplying a nitrogen-containing gas to the substrate, and (d) removing the nitrogen-containing gas remaining in the process chamber (abstract and Fig. 4). They teach using the process to form a TiN film where TiCl4 gas is supplied as a metal-containing gas, and a SiH4 gas is supplied as a reducing gas (0053 and Fig. 4). They teach that the TiCl4 and SiH4 gases are removed from the chamber and then NH3 gas is supplied as the nitrogen-containing gas (0053 and Fig. 4). They teach that after a predetermined time of supplying TiCl4, the supply of SiH4 is begun such that the TiCl4, SiH4, and N2 gases are supplied simultaneously to the wafer, where the supply of SiH4 continues after the supply of TiCl4 is stopped (0061, 0063, and Fig. 4). They teach that the process is repeated a predetermined number of times to form a TiN film having the desired thickness (0070). They teach that HCl is a byproduct of the TiCl4/NH3 reaction, where HCl can be adsorbed on the surface of the TiN film which reduces the deposition rate (0004). They teach that SiH4 reacts with HCl to provide SiCl4 and H2, which is discharged from the reaction so as to reduce the HCl in the film (0064). They teach that the process efficiently discharges HCl generated during film formation, allowing for an increased deposition rate, lowers the film resistivity, and improves the oxidation resistance (0073-0076). They teach that the pressure, flow rate, and time for supplying the silicon precursor can be adjusted to increase the Si content of the film and form a TiSiN film (0062, 0064, and 0118).
From the teachings of Ogawa, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have modified the process of Clark to have supplied a fourth gas including hydrogen and a second element different from the first element in the form of SiH4 to the substrate during a period overlapping with (a), i.e., the supply of TiCl4 and for a predetermined time after (a) because Ogawa teaches that such a process flow can be used to remove HCl from the film to increase the deposition rate, reduce resistivity, and provide oxidation resistance in the process of forming a TiN film using a process similar to that of Clark, where the process parameters such as pressure, flow rate, and supply time can be used to increase or minimize the silicon content in the film such that it will be expected to provide the benefits described by Ogawa while providing the strained TiN or TiSiN film by changing the pressure, flow rate, or flow time of the SiH4 gas.
They do not teach forming an NH-terminated group on the surface of the substrate.
Kuroda teaches methods and systems for pretreating a surface prior to depositing silicon nitride on the surface (abstract). They teach pretreating the surface by exposing the surface to activated species formed from one or more gases comprising nitrogen and hydrogen (abstract). They teach that the one or more gases comprising nitrogen and hydrogen can include, for example, one or more of nitrogen, hydrogen, ammonia, and/or hydrazine (0009). They teach that the substrate can be various materials including semiconductor materials, metal, oxides such as silicon oxides, metal oxides, metal nitrides, silicon nitride, silicon oxynitride, other dielectric materials, etc. (0041). They teach that an optional step can include supplying a silicon-containing precursor to form a surface terminated in Si-H bonds, which form Si-NH2 bonds on the surface during a subsequent pretreatment step, i.e., the nitrogen and hydrogen treatment step (0042, 0044, and Fig. 1). They teach that during the nitrogen and hydrogen treatment step, N-H and/or N-H2 groups can form on a surface of the substrate (0044). They teach that the formation of such groups on the surface of the substrate facilitates subsequent deposition of silicon nitride on the surface of the substrate (0044). They teach that the incubation period for plasma-enhanced deposition of silicon nitride can be highly dependent on a quality of an underlying layer (0045). They teach that the use of step 106, alone or in combination with step 104, can reduce or eliminate the incubation period, allowing for more uniform deposition of silicon nitride (0045). They teach that the silicon precursor is a silicon halide such as silicon tetrachloride (0050).
Spiegelman teaches a method for forming nitrogen-containing thin films by ALD using a substantially water free hydrazine gas (abstract). They teach pretreating the surface with hydrazine and then depositing a TiN film using TiCl4 and hydrazine (0009 and 0013). They depict the surface as being terminated in N-H bonds (Fig. 1). They teach that SiN can also be deposited using the claimed method with precursors including silicon tetrachloride (0009 and 0011).
From the teachings of Kuroda and Spiegelman, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have pre-treated the substrate surface with a hydrazine-containing plasma so as to provide NH termination on the substrate surface because Kuroda teaches that such a treatment provides more uniform SiN deposition form precursors such as SiCl4 and Spiegelman teaches that NH bonds on a substrate surface are desirable for the growth of nitrides and specifically both SiN and TiN materials from SiCl4 and TiCl4, suggesting that the treatment of Kuroda, while aimed at SiN, will also be desirable for nucleating TiN, where since they both use halogen precursors, the precursors are expected to have similar reactivity with the NH-terminated surface. Therefore, the process will include step (e) of supplying the second processing gas to the surface of the substrate to form NH-terminated groups before the first supply of the first processing gas in (d).
Regarding claims 3 and 4, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claims 1 and 2. Clark further teaches supplying a second gas pulse of the metal precursor at step 326 and exposing the substrate to a gas pulse containing the second nitrogen precursor or a gas pulse containing the first nitrogen precursor and the second nitrogen precursor in a second ratio different from the first ratio at step 328 (0094 and Fig. 3B). As noted above, the first and second nitrogen precursors are selected from ammonia and hydrazine (0093). They teach repeating steps 326 and 328 a second number of times prior to repeating steps 322 and 324 (0097 and Fig. 3B), where an example is provided of performing the steps 1, 2, and 3 times (0100). Therefore, they provide supplying a third processing gas including the N-H bond (ammonia and hydrazine) and having a composition different from that of the second processing gas to the substrate (where the composition is different due to the different ratio of ammonia and hydrazine), and performing (a) and (e) Y times, where Y is a natural number of 1 or greater, after (d) to form a second film containing the first element on the first film.
Alternatively, they provide an example where hydrazine is provided to form a first metal nitride film and ammonia is used to form a second metal nitride film on the first metal nitride film (0016). Therefore, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have used hydrazine as the first gas for step (b) and ammonia as the second gas for step (d) because they indicate that hydrazine can be used as the first gas and ammonia can be used as the second. Therefore, the third process gas will include the N-H bond from ammonia and will have a composition different from that of the second processing gas (which would be hydrazine so as to include the N-H and N-N bond).
Regarding claims 11 and 12, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claims 1 and 2. As noted above for claims 3 and 4, Clark teaches and/or suggests supplying a third process gas including the N-H bond and having a composition different from that of the second processing gas after supplying the second processing gas. Therefore, providing the third processing gas after supplying the silicon precursor, i.e., steps 326 and 328, is considered to meet the requirements of claims 11 and 12 because it provides steps (a) and (b) with a processing gas including the N-H bond and having a composition different from that of the second processing gas.
Alternatively, since they indicate that in step 324, the gas can include a mixture of hydrazine and ammonia (0093 and Fig. 3B), step (b) will include a second process gas including an N-N bond and an N-H bond in hydrazine and a third process gas will be included having the N-H bond in ammonia where it will have a different composition than the second processing gas.
Regarding claims 13 and 14, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claim 1. Clark further teaches forming a strained metal silicon nitride film by exposing a substrate to a gas pulse containing a metal precursor at step 622, exposing the substrate to a gas pulse containing a first nitrogen precursor or a gas pulse containing the first nitrogen precursor and a second nitrogen gas precursor in a first ratio in step 624, where steps 622 and 624 are sequentially performed a first number of times (0130-0131, 0134, and Fig. 6B). They teach that the first and second nitrogen precursors are selected from ammonia and hydrazine (0131). They teach in step 626, the substrate is exposed to a gas pulse containing a silicon precursor followed by step 628 where the substrate is exposed to a gas pulse containing the second nitrogen precursor or a gas pulse containing the first nitrogen precursor and the second nitrogen precursor in a second ratio different from the first ratio (0132 and Fig. 6B). As discussed above, the metal nitride precursors are selected from precursors that include halides. Therefore, they provide step a) of providing a metal precursor that includes a halide and then supplying a third processing gas after step (a) and after step (c), where the fourth processing gas contains a second element different from the first element, i.e., silicon compared to the metal of the first element, so as to form a film containing a second element on the first film.
As discussed above, Ogawa teaches that the process conditions can be tuned to increase or minimize the amount of silicon provided in the film. Therefore, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have provided the silicon precursor at conditions minimizing the amount of inclusion during step 622 of Clark and then to have provided only the silicon precursor at step 626 so as to form the silicon layer in forming the TiSiN film so as to have controlled the amount of silicon included in the film. Alternatively, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have provided conditions to include the silicon precursor while flowing SiH4 during step (a) and after step (a) so as to provide the desired amount of silicon to the film, where in such a case, the third processing gas and the fourth processing gas are the same, having a second element different from the first element, where the second element is included into the film.
Regarding claim 16, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claim 1. Clark further teaches forming the strained metal nitride in a semiconductor device (abstract), such that the method is included in manufacturing a semiconductor device.
Regarding claim 20, Clark in view of Ogawa, Kuroda, and Spiegelman suggest the process of claim 1. Clark further teaches that the strained nitride film 118 is formed on a gate stack including a dielectric film 116 which can include SiO2, SiN, SiON, metal oxides, etc., and a conductive layer 117 such as TiN (0021-0024). They teach that the conductive layer and film 118 can be composed of the same metal nitride or metal silicon nitride (0024). From this, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have formed the conductive layer 117 on the oxide layer 116 using the process of Clark in view of Ogawa, Kuroda, and Spiegelman because Clark teaches that the films can be the same material and they provide a process for forming the material such that it will be expected to form the layer on an oxide surface. Therefore, the surface of the substrate on which the NH-terminated group is formed in (e) comprises an oxide film. Further, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have optimized the times the process is repeated to provide a conductive film having the desired thickness because Clark teaches that the ALD process is repeated until a desired thickness is achieved (0091 and 0095), such that the number of times the process is repeated is considered to be an optimizable parameter to provide a suitable film thickness. According to MPEP 2144.05 II A, “[W]here 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.” In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955).
Regarding claim 21, Clark in view of Ogawa, Kuroda, and Spiegelman suggest the process of claim 1. Ogawa further teaches that the SiH4 flow begins after flowing TiCl4 for 0.01 to 5 seconds (0061). After flowing TiCl4 for 0.01 to 10 seconds, the flow of TiCl4 is stopped (0063). They teach that after 0.01 to 60 seconds, 0.1 to 30 seconds, or 1 to 20 seconds, the flow of SiH4 is stopped (0064). Therefore, a time period from an end of the supply of TiCl4 in (a) to an end of the supply of silane in (c) overlaps a range in which it is longer than a time period form the start of supplying silane to the end of supplying TiCl4. According to MPEP 2144.05, “in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists.”
Regarding claim 22, Clark in view of Ogawa, Kuroda, and Spiegelman suggest the process of claim 1, as noted above the second processing gas is hydrazine and the fourth gas is silane so as to provide silicon and hydrogen and no halogen.
Claims 5-7 are rejected under 35 U.S.C. 103 as being unpatentable over Clark in view of Ogawa, Kuroda, and Spiegelman as applied to claims 1-3 above, and further in view of Vaartstra, US 2004/0043604 A1 and Kim, US 2006/0014385 A1.
Regarding claims 5-7, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claims 1-3.
They do not teach heat-treating the substrate at a temperature higher than the temperature of (d) after (d).
Vaartstra teaches a method of forming refractory metal nitride layers (including silicon nitride layers) on a substrate by an ALD process (abstract and 0016). They teach providing a vapor that includes one or more refractory metal precursor compounds of the formula MYn, where M is selected from a group including Ti and Y is a halogen atoms such as F, Cl, I, or combinations thereof (0012). They teach providing a vapor that includes one or more disilazanes, where silane is an alternative to the disilazane (0012 and 0038). They teach providing nitrogen sources such as ammonia, hydrazine, etc. and combinations thereof (0043). They teach that the ALD process is performed at temperatures of about 25°C to about 400°C (0052). They teach that after layer formation on the substrate, an annealing process can be performed in situ in a nitrogen atmosphere or an ammonia atmosphere (0062). They teach annealing at a temperature within the range of about 400°C to about 1000°C (0062). Therefore, Vaartstra teaches performing an ammonia annealing step on ALD films, where formed films include TiSiN and where the annealing temperature is higher than the deposition temperature.
Kim teaches forming a first titanium nitride layer by CVD or ALD using TiCl4 and ammonia and depositing a second titanium nitride layer on the first by CVD at a second temperature with TiCl4 and ammonia (abstract). They teach forming a lower metal layer composed of TiSiN by a CVD or process or an ALD process (0066). They teach that a thermal annealing process may be performed on the lower metal layer to minimize the chlorine content inside the lower metal layer (0066). They teach that after forming a first titanium nitride layer, the chlorine element inside the layer can be removed by exposing the layer to only an ammonia gas (0041).
From the teachings of Vaartstra and Kim, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have annealed the TiSiN film in ammonia at a temperature in the range of 400°C to 1000°C (so as to be higher than the deposition temperature) because Vaartstra teaches that it is desirable to anneal a TiSiN film formed by an ALD process similar to that of Clark in view of Ogawa, Kuroda, and Spiegelman and Kim teaches that thermally annealing a TiSiN film reduces the chlorine content in the layer, where flowing ammonia helps to reduce chlorine in a TiN layer such that it will be expected to desirably treat the film while also reducing any residual chlorine. Therefore, the process will comprise heat-treating the substrate at a temperature higher than the temperature during deposition after the step of repeating the process. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Claims 8-10 are rejected under 35 U.S.C. 103 as being unpatentable over Clark in view of Ogawa, Kuroda, and Spiegelman as applied to claims 1-3 above, and further in view of Vaartstra, US 2004/0043604 A1, Kim, US 2006/0014385 A1, and Raaijmakers, US 6,348,420 B1.
Regarding claims 8-10, Clark in view of Ogawa, Kuroda, and Spiegelman suggests the process of claims 1-3.
As noted above Vaartstra and Kim provide the suggestion of annealing the films at a temperature higher than the temperature used in (c), where they suggest annealing in ammonia. Vaartstra teaches annealing in situ in the deposition chamber (0062).
They do not teach flowing ammonia to the substate during the temperature rise to the higher temperature.
Raaijmakers teaches performing multiple sequential processes in situ in a single-wafer processing chamber in forming dielectric stacks of high quality (abstract). They teach that the process forms silicon oxide, nitride, and/or oxynitride followed by in situ silicon nitride deposition (abstract). They teach annealing can also be conducted in situ, reducing transition time without commensurate loss in reaction rates (abstract). They teach that after deposition, the second or deposited dielectric layer is annealed to improve the quality the layer, where the anneal is a high temperature ammonia anneal that densifies the silicon nitride layer by reacting any excess silicon and producing more stoichiometric Si3N4 (Col. 11, lines 38-53). They teach forming a dielectric stack comprising interfacial oxynitride and overlying silicon nitride on a substrate followed by performing an in situ anneal (Col. 15, lines 14-37). They teach that after forming the dielectric stack, silane flow is stopped while nitrogen and ammonia flow are maintained at the same flow rate as during nitride deposition while the temperature is ramped from 780°C to about 900°C and the anneal is maintained for about 60 seconds (Col. 15, lines 21-37).
From the teachings of Vaartstra and Raaijmakers, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have performed the annealing treatment while flowing ammonia and increasing the temperature to the annealing temperature because Vaartstra teaches performing an anneal in the same chamber, where the annealing can be done in ammonia, and Raaijmakers teaches annealing a nitride in ammonia gas in situ by flowing ammonia while increasing the temperature so as to react excess silicon with ammonia, where they indicate that performing the process in situ reduces transition time without commensurate loss in reaction rates such that it will be expected to reduce the chlorine content while increasing the temperature for annealing while providing the benefits described by Raaijmakers. Therefore, the process will comprise (f) heat-treating the substrate at a temperature higher than the temperature of (c) after (c) (i.e., after forming the film), wherein a third processing gas including the N-H bond having a composition different than that of the second processing gas (i.e., ammonia) is supplied to the substrate during the temperature rise to the higher temperature.
Response to Arguments
Applicant’s arguments dated 9/4/2026 have been fully considered.
In light of the amendments to the claims, the previous 112 rejections are withdrawn, however, a new claim objection and 112(b) rejection have been made.
Further, in light of the amendment to claim 1, the rejections have been modified as indicated above.
Regarding Applicant’s arguments over Raaijmakers flowing ammonia to react excess silicon in silicon nitride, as noted above Vaartstra and Kim provide the suggestion to anneal in ammonia to remove excess chlorine, where Raaijmakers indicates that it is known to flow ammonia while increasing to an annealing temperature such that the process is expected to provide the benefits of both reducing chlorine and reacting excess silicon.
Conclusion
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/CHRISTINA D MCCLURE/Examiner, Art Unit 1718
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