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 1-4, 9-10, 13-19, 21, and 22 are pending and rejected. Claims 5-8, 11, 12, and 20 are cancelled. Claims 17 and 22 are amended.
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, 3-4, 13-16, and 22 are rejected under 35 U.S.C. 103 as being unpatentable over Na, WO 2021/046058 A1 in view of Subrahmanyan, US 6,107,192, Thombare, WO 2022/150270 A1, Coolbaugh, US 2022/0229228 A1, and Lee, US 2022/0081759 A1.
It is noted that the second inventor is used for WO 2022/150270 A1 to differentiate between Na references.
Regarding claims 1 and 22, Na teaches a deposition method (method of selectively depositing Mo films, abstract) comprising:
exposing a top surface of a substrate comprising at least one feature to a chemical exposure (where a substrate having a feature, 0020 and Fig. 4-5, is exposed to a pre-treatment such as a hydrogen-containing plasma, 0029), the at least one feature comprising at least one surface defining a via, the via comprising a bottom surface comprising a metal material and two sidewalls comprising a dielectric (where the feature includes a bottom surface formed of a metal material and two sidewalls formed of an oxide or nitride, i.e. a dielectric, 0020-0024 and Fig. 4-5, where the feature may be a via or a trench, 0026 and Fig. 2), the chemical exposure is configured to clean the bottom surface (where the pre-treatment is used to reduce any metal-oxide on the metal-containing surface, 0029, such that it is configured to clean the bottom surface); and
in situ selectively depositing a molybdenum film on the cleaned bottom surface (selectively depositing molybdenum on the metal-containing bottom surface, 0031 and Fig. 3-5, where the selective deposition of the Mo film and the pre-treatment may be performed in the same station of a processing tool, 0046, such that it will be formed in situ).
They do not teach performing an ex-situ combined pump and purge process and thermal soak followed by an in situ combined pump and purge process and plasma exposure.
As noted above, Na teaches performing a hydrogen plasma to reduce any metal-oxide on the metal-containing surface (0029).
Subrahmanyan teaches a precleaning process prior to metallization for submicron features on substrates (abstract). They teach cleaning the submicron features with radicals from a plasma of a reactive gas such as oxygen, wherein the plasma is generated by a remote plasma source and the radicals are delivered to chamber in which the substrate is disposed (abstract). They teach that native oxides remaining in the submicron features are preferably reduced in a second step by treatment with radicals from a plasma containing hydrogen (abstract). They teach that the method includes removal of oxides form the bottom of contacts without damaging the underlying layer, including the removal of SiO2, aluminum oxide or copper oxide from the bottom of vias without redeposition of the material onto sidewalls, the removal of a thin layer of damaged silicon from the bottom of contact holes, and the removal of contaminants from the sidewalls of the features (Col. 3, lines 1-15). They teach that the method is suitable for precleaning vias, contacts, and other features etched into a dielectric layer, such as a silicon dioxide layer, which is deposited on a conductive or semi-conductive sublayer, such as Ge, Si, Al, Cu, or TiN sublayers (Col. 4, lines 41-52). They teach that the features can then be filled with a conductive or semi-conductive material which connects the sublayer and a subsequent metal interconnect layer to be deposited on the dielectric layer (Col. 4, lines 41-52). They teach that etching of the features in the dielectric typically leaves contaminants which should be removed to improve filling of the features and ultimately improve the integrity and reliability of the devices formed (Col. 4, lines 41-52). They teach that after etching of the dielectric layer, the features can have damaged silicon or metal residues within the features, residual photoresist or polymer, and redeposited material following a sputter etch preclean process (Col. 4, lines 53-67).
From the teachings of Subrahmanyan, 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 Na to have exposed the substrate surface to an oxygen plasma before the hydrogen plasma so as to remove contaminants on the sidewalls and bottom of the recesses because Subrahmanyan teaches that such a plasma exposure is desirable for removing various contaminants, including those on the sidewalls and bottom contacts, where the exposure is followed by a hydrogen plasma exposure for reducing oxides such that it will be expected to provide the desirable and predictable result of cleaning the surfaces of the substrate prior to deposition of molybdenum. Therefore, Na in view of Subrahmanyan suggest providing a plurality of chemical exposures defining a cleaning cycle configured to clean the bottom surface and two sidewalls where the plurality of chemical exposures comprise a plasma exposure comprising a H2 plasma exposure and an O2 plasma exposure.
They do not teach performing a thermal soak.
Thombare teaches deposition processes including deposition of a thin, protective Mo layer using a molybdenum chloride (MoClx) precursor followed by Mo deposition to fill the feature using a MoOyXz precursor (abstract). They teach an in-situ clean process in which a MoClx precursor is used to remove oxidation from underlying surfaces prior to deposition (abstract). They teach providing a substrate including a feature having a feature bottom and feature sidewalls, where the feature bottom includes an oxidized surface; soaking the feature in a molybdenum halide precursor to remove oxide from the oxidized surface to leave an unoxidized surface; and depositing molybdenum into the feature, including directly on the unoxidized surface (0023). They teach that the feature bottom includes a metal-containing surface, the feature sidewalls include a dielectric surface, and depositing molybdenum further includes selectively depositing molybdenum on the metal-containing surface relative to the dielectric surface (0027). They teach that soaking the feature in the molybdenum halide precursor and depositing the molybdenum into the feature can be performed in the same or in different chambers (0030-0031). They teach that the molybdenum soak last at least 10 seconds in duration (0032). They teach that the oxidized surface may be caused by exposing the surface to oxidizing conditions such as an oxygen-based thermal or plasma treatment (0084-0085). They teach performing an optional clean operation 202 that includes a hydrogen plasma treatment, a thermal hydrogen treatment, or a reducing treatment, to reduce oxidized metal on a metal substrate at the feature bottom (0086). After cleaning, they teach that the feature is soaked in a molybdenum chloride (MoClx) precursor to remove oxidation from the feature’s surfaces (0087). They teach that examples of MoClx compounds include MoCl5, where other halides can be used such as MoF6 (0067 and 0087). They teach that a Cl-containing precursor may be used where traditional cleaning with thermal or plasma hydrogen does not work, such as where the oxidized surface is stable on the surface material (0087). They teach that for the in-situ clean, the substrate may be heated between 300°C and 500°C where the total precursor exposure time is at least 10 seconds, at least 60 seconds (0089). Therefore, Thombare teaches filling a feature with molybdenum, where the feature is first treated with an oxygen plasma, cleaned with a hydrogen plasma, and then in-situ or ex-situ treated with a MoCl5 thermal soak (since the substrate is heated) to remove oxidation from the feature’s surfaces.
From the teachings of Thombare, 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 included a soak in MoCl5 at about 300-500°C to remove oxides for cleaning because Thombare teaches filling a feature with molybdenum, where the feature is first treated with a MoCl5 thermal soak (since the substrate is heated) to remove oxidation from the feature’s surfaces, where the treatment can be done in a different reactor from the deposition, and where the treatment is done in addition to an oxygen and hydrogen plasma such that it will be expected to facilitate the removal of oxides from the substrate surface.
They do not teach combining ex-situ and in-situ cleaning treatments.
Na further teaches that operations such as pre-treatment may be formed in the same station or another station of a multi-station processing tool (0046). They teach that the tool includes an ALD process station having a process chamber for maintaining a low-pressure environment (0045). They teach that a plurality of stations may be included in a common low-pressure process tool environment (0045). They teach that the plasma pretreatment may be a remote plasma (0030).
Coolbaugh teaches a method for fabricating a photonics structure having one or more photonics device that includes forming one or more conductive materials (abstract). They teach prior to epitaxially growing germanium, the photonics structure is subjected to an ex-situ and/or in-situ surface cleaning process consisting of a wet chemical or dry native oxide removal followed by a short in-situ high-temperature bake in a reducing hydrogen atmosphere to remove sub-stoichiometric surface oxide reformed by exposure to air between the cleaning tools and the reactor (0047). They teach using a plasmaless HF/NH3 process for performing chemical oxide removal (0034).
From the teachings of Coolbaugh, 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 combined ex-situ and in-situ cleaning techniques because Coolbaugh teaches that it is conventionally known to provide an ex-situ oxide removal step and an in-situ hydrogen treatment to remove remaining oxide from exposure to air such that it will be expected to provide the cleaning steps as desired. Further, since Thombare teaches that the soak can be performed in a different reactor from the deposition, where the soak is provided to remove oxides, 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 thermal soak ex-situ so as to have removed the native oxides as suggested by Coolbaugh.
Thombare teaches intentionally oxidizing the surface by an oxygen-plasma treatment prior to the thermal soak (0085 and 0087).
Subrahmanyan further teaches the precleaning can be performed in situ in a CVD chamber which deposits a barrier layer for copper or aluminum metallization by addition of a remote plasma source to the chamber (Col. 3, lines 27-49). They also teach that pre-cleaning can be done in a dedicated precleaning chamber (Col. 6, lines 47-57 and Fig. 1).
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 performed the oxygen plasma treatment ex-situ prior to the thermal soak and then to have performed the hydrogen plasma treatment in situ without breaking vacuum because Na teaches performing pre-treatment such as hydrogen plasma in the same processing tool as deposition, Thombare teaches exposing the substrate to an oxidizing plasma prior to the thermal soak, Subrahmanyan teaches performing the oxygen and hydrogen plasma precleaning in-situ or ex-situ, and Coolbaugh teaches performing a hydrogen treatment for removing remaining oxides in-situ such that it will be expected to provide the desired and predictable result of removing contaminants and remaining oxides prior to deposition, where the substrate will not be re-exposed to air prior to deposition. Specifically, by performing the oxygen plasma prior to the thermal soak it will improve the efficiency of the process by removing contaminants using the oxygen plasma, reducing oxides by the thermal soak and then by performing the hydrogen plasma treatment in-situ before deposition it will ensure that the surface is free of oxides.
They do not teach performing an ex-situ and in-situ pump and purge.
Lee teaches methods in which a pre-clean chamber receives a semiconductor wafer from a metal gate layer deposition chamber and at least partially removes an oxide layer on a metal gate layer (abstract). They teach a first cluster includes one or more degas chambers that are used to remove moisture from the semiconductor wafers, e.g., from one or more layers or structures formed on the semiconductor wafers (0029). They teach that the degas chambers may remove moisture or residual gas from the semiconductor wafers prior to formation of one or more metal gate features, e.g., by deposition in a processing chamber of the apparatus (0029). They teach that the degassing processes are performed in the presence of an ambient gas of argon, helium, etc., and a pressure of about 0.1 Torr to about 10 Torr (0029). They teach that the degassing chambers may include a vacuum pump in order to purge gas from the degas chambers (0029). They teach performing deposition using processes such as ALD (0037). Therefore, Lee teaches removing moisture from structures on a substrate before deposition by flowing a gas such as argon while pumping (so as to provide a pressure of about 0.1 Torr to about 10 Torr), such that the process is considered to be a pumping and purging step because the chamber will be purged with the gas during pumping.
From the teachings of Lee, 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 a pumping and purging step to remove water vapor or moisture from the via on the substrate before performing the ex-situ thermal soak and before performing the in-situ plasma treatment because Lee teaches that it is desirable to remove moisture from structures and residual gas on a substrate prior to deposition such that it will be expected to help remove undesired moisture from the substrate in preparation for cleaning so as to avoid any undesired side reactions between the process gases and the moisture or residual gas (air) on the surface while also providing an exposure surface for cleaning.
Further, since the Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee indicate that oxygen plasmas, hydrogen plasmas, and thermal soaks are used to clean substrate surfaces of contaminants and oxides prior to deposition, where the cleaning steps can be performed in-situ and/or ex-situ, 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 cleaning process to provide the desired steps either in-situ or ex-situ so as to have cleaned the surfaces. 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). Additionally, according to MPEP 2144.04(IV)(C): Ex parte Rubin, 128 USPQ 440 (Bd. App. 1959) (Prior art reference disclosing a process of making a laminated sheet wherein a base sheet is first coated with a metallic film and thereafter impregnated with a thermosetting material was held to render prima facie obvious claims directed to a process of making a laminated sheet by reversing the order of the prior art process steps.). See also In re Burhans, 154 F.2d 690, 69 USPQ 330 (CCPA 1946) (selection of any order of performing process steps is prima facie obvious in the absence of new or unexpected results); In re Gibson, 39 F.2d 975, 5 USPQ 230 (CCPA 1930) (Selection of any order of mixing ingredients is prima facie obvious.).
Regarding claim 3, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches that the metal-containing surface is selected from a group including cobalt, copper, tungsten, molybdenum, and ruthenium (0006, 0008, and 0021).
Subrahmanyan teaches that the conductive sublayer located beneath the dielectric layer is selected from materials including copper (Col. 4, lines 41-52).
Regarding claim 4, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches that the sidewall surfaces are dielectric surfaces formed from silicon-based oxides, i.e. SiOx, or silicon nitrides (0023-0024).
Subrahmanyan teaches that the dielectric layer is silicon dioxide (Col. 4, lines 41-52).
Regarding claim 14, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches selectively depositing the molybdenum film by ALD (0005).
Regarding claims 13, 15, and 16, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1.
They do not teach the selectivity compared to similar processes performed without the plurality of chemical exposures, the roughness of the molybdenum film, or the grain size.
Na teaches selectively depositing Mo using Mo precursors such as MoOCl4 and MoO2Cl2 with a reducing agent such as hydrogen (0032). They teach that temperature affects selectivity, grain size, and resistance (0033). They teach that higher temperatures may reduce selectivity of the Mo film and result in growth on the oxide or nitride of the sidewall surfaces as well as on the metal-containing bottom surface, but if the temperatures are too low, the impurity level may be increased and grain size may be reduced, increasing resistance (0033). They teach that the substrate temperature may be between 350°C and 600°C to selectively deposit Mo using a chlorine-containing chemistry, where the temperature may be between 350-550°C, or 350-450°C (0033). They teach that the chamber pressures may range from 1 to 100 torr (0037).
The instant specification at paragraph 0052 indicates using molybdenum precursors such as MoOCl4 and MoOCl2 with hydrogen and paragraph 0053 indicates using temperatures in the range of 300-550°C with pressures in the range of 10-300 torr.
Therefore, Na teaches depositing molybdenum using the same precursors, a temperature within the range used in the instant specification, and at a pressure overlapping the range used in the instant specification. Since Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1, where Na indicates that the selectivity and grain size of the film is dependent on temperature and they deposit the films at a temperature within the range used in the instant specification (with the same precursors and an overlapping pressure range) the resulting films are expected to have properties meeting the requirements of claims 13 (i.e. selectivity), 14 (surface roughness), and 15 (grain size). According to MPEP 2112.01 I, “Where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established. In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977)”.
Subrahmanyan further teaches that performing a precleaning treatment on a barrier layer before depositing a metal that fills the feature improves the texture, grain orientation, and grain size of copper on the barrier layer resulting in good surface topography and tighter distribution of grain orientations (Col. 8, lines 8-31), indicating that such a cleaning process is known to improve grain size and topography of a deposited film.
Claim 2 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee as applied to claim 1 above, and further in view of Schloss, WO 2021/076636 A1.
Regarding claim 2, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1. Subrahmanyan teaches that the decrease in the width of features in forming vias, contacts, and other features results in larger aspect ratios for the features and increased difficulty in cleaning the features prior to filling (Col. 1, lines 22-35). They teach that there is a great amount of effort directed at cleaning small features having high aspect ratios, especially where the ratio of feature height to width is 4:1 or larger (Col. 1, lines 22-35). They teach that the submicron features have a high aspect ratio with steep sidewalls (Col. 5, lines 12-21).
They do not teach the aspect ratio of the via for depositing molybdenum.
Schloss teaches method of filling features with molybdenum (abstract). They teach that substrates have features such as vias or contact holes, which may be characterized by high aspect ratios (0038). They teach that the feature may have an aspect ratio of at least about 2:1, at least about 4:1, at least about 6:1, etc. (0038). Therefore, Schloss teaches filling vias with molybdenum where the vias have an aspect ratio of at least about 2:1 or at least about 4:1.
From the teachings of Subrahmanyan and Schloss, 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 Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee to have deposited the molybdenum films in vias having aspect ratios of at least 2:1 or at least 4:1 because Schloss teaches that such aspect ratios are desirable for vias that are filled with molybdenum and Subrahmanyan teaches that it is known to use vias with an aspect ratio of 4:1 or larger such that it will be expected to provide a suitable via size range for filling with molybdenum. Therefore, the aspect ratio will overlap the range of claim 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.” In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976).
Claim 9 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee as applied to claim 1 above, and further in view of Hawrylchak, US 2019/0067006 A1 and Theodosiou, US 2015/0075973 A1.
Regarding claim 9, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1, where the hydrogen plasma removes oxides. Subrahmanyan teaches that the features may contain redeposited material on the feature surfaces following a sputter etch preclean process (Col. 4, lines 53-67), indicating that the cleaning process can be used to remove any redeposited material resulting from a previous sputter etching process.
They do not teach using a hydrogen plasma with argon sputtering.
Hawrylchak teaches a processing sequence for removing oxides and contaminants from a substrate (0023 and Fig. 1). They teach removing oxides from a surface of a semiconductor substrate using a cleaning process (0024). They teach that the substrate may have an oxide layer and contaminants disposed thereon (0024). They teach that due to the sensitivity of epitaxial deposition processes to oxides and contaminants, such as carbon containing contaminants, surface contamination resulting from exposure to most typical cleanroom environments for a few hours can become significant enough for the accumulated oxides and contaminants to affect the quality of a subsequently formed epitaxial layer (0024). They teach that the surface may be cleaned by performing an oxide removal process and a contaminant removal process (0025). They teach removing the oxides using a cleaning process and removing the contaminants using a reducing process (0025 and Fig. 1). They teach cleaning using a plasma formed from a gas such as hydrogen, helium, argon, ammonia, etc., or any combination thereof (0025 and Fig. 1). After removing the oxides from the surface of the substrate, any remaining contaminants on the surface of the substrate are removed (0032 and Fig. 1). They teach that contaminants such as carbon or hydrocarbons are removed from the surface using a reducing process such as a plasma process (0032 and Fig. 1). They teach that the oxide and contaminant processes can be repeated as many times as necessary where an optional thermal treatment may also be performed to remove any residual by-products or contaminants, and to anneal the surface to remove any surface defects (0035). Therefore, Hawrylchak teaches performing multiple cleaning steps to remove oxides and any other contaminants where the cleaning steps can be repeated as needed and include plasma treatments and thermal treatments.
Theodosiou teaches a method of pre-cleaning a semiconductor substrate by performing an Ar/H2 sputter etch to remove material from an exposed electrically conductive structure (abstract). They teach reducing the amount of unwanted contaminants produced during the sputter etch and reducing the pumping time required to achieve a desired pressure so that contamination of the semiconductor structure, in particular the metal layer, is reduced (0009). They teach that the precleaning step removes native oxide from the exposed electrically conductive structures (0017). They teach that an ICP source is used for plasma production and an RF bias is applied to the wafer, causing ions from the plasma to be accelerated onto the wafer surface (0046 and Fig. 1). They teach that the process removes native oxide from metal contacts on semiconductor wafers using an Ar/H2 sputter etch that reduces levels of organic contamination within the chamber, and provides productivity benefits, since residence time in the process module can be reduced (0050). They teach that the argon/hydrogen plasma reduces the levels of CO contamination considerably in comparison to sputter etching using argon alone (0050).
From the teachings of Hawrylchak and Theodosiou, 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 a hydrogen plasma/Ar sputter etching process so as to remove oxide from the metal surface with using an RF bias source so as to provide directionality in an ICP plasma (because the ions will be attracted to the substrate) because Hawrylchak teaches that multiple cleaning steps can be performed, Subrahmanyan teaches that the cleaning process can be done following a sputter etch clean, and Theodosiou teaches that adding hydrogen to an Ar sputter etching process formed from and ICP plasma with directionality provided by an RF bias reduces the level of CO contamination, reduces unwanted contaminants produced during the sputter etching process, removes oxides, and improves the productivity of the process such that it will be expected to provide a desirable oxide removal step.
Claim 10 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee as applied to claim 1 above, and further in view of Hein, US 2004/0076837 A1.
Regarding claim 10, Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee suggest the process of claim 1. Na teaches performing a hydrogen plasma pre-treatment for reducing metal oxides on the metal-containing surface (0029).
Lee teaches degassing at a temperature of within a range of about 100°C to about 600°C (0029).
Thombare teaches performing the thermal soak at a temperature of 300°C to 500°C (0087). They teach providing a clean/etch operation at 602, where examples of cleaning treatments are given above in operation 202, which include hydrogen plasma treatment (0086). They teach that operation 602 may also include soaking the feature in a Mo precursor to remove oxidation and/or remove or reduce a metal nitride layer from the feature (0129). They teach that in process 602, the substrate is heated between 300°C and 500°C (0121).
They do not teach the temperature for the oxygen plasma treatment.
Hein teaches applying a coating to a substrate, particularly a metal substrate (abstract). They teach that the substrate has an optically-transparent coating such as SiOxCyHz on at least a portion of the substrate (0005). They teach cleaning the substrate using a pre-clean process where the substrate temperature is maintained at more than 100°C (0027). They teach that oxygen is fed to the chamber for plasma cleaning (0027).
From the teachings of Lee, Thombare, and Hein, 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 temperature of the plurality of chemical exposures to be within the claimed range because Lee teaches pumping and purging at temperatures within the claimed range, Thombare teaches performing a hydrogen plasma and thermal soak at temperatures within the claimed range, and Hein teaches performing an oxygen plasma cleaning process at a temperature overlapping the claimed range, such that by optimizing the temperature to be within the claimed range it will be expected to provide a desirable temperature for removing oxides, moisture, and any other contaminants from the via using the pump/purge, oxygen plasma, and hydrogen plasma cleaning processes. According to MPEP 2144.05 II A, “Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. “[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).
Claims 1, 3-4, 13-16, and 21 are rejected under 35 U.S.C. 103 as being unpatentable over Na, WO 2021/046058 A1 in view of Subrahmanyan, US 6,107,192, Hawrylchak, US 2019/0067006 A1, Lin, US 2020/0111885 A1, Roy, US 2020/0194304 A1, Coolbaugh, US 2022/0229228 A1, and Lee, US 2022/0081759 A1.
It is noted that the second inventor is used for WO 2022/150270 A1 to differentiate between Na references.
Regarding claims 1 and 21, Na teaches a deposition method (method of selectively depositing Mo films, abstract) comprising:
exposing a top surface of a substrate comprising at least one feature to a chemical exposure (where a substrate having a feature, 0020 and Fig. 4-5, is exposed to a pre-treatment such as a hydrogen-containing plasma, 0029), the at least one feature comprising at least one surface defining a via, the via comprising a bottom surface comprising a metal material and two sidewalls comprising a dielectric (where the feature includes a bottom surface formed of a metal material and two sidewalls formed of an oxide or nitride, i.e. a dielectric, 0020-0024 and Fig. 4-5, where the feature may be a via or a trench, 0026 and Fig. 2), the chemical exposure is configured to clean the bottom surface (where the pre-treatment is used to reduce any metal-oxide on the metal-containing surface, 0029, such that it is configured to clean the bottom surface); and
in situ selectively depositing a molybdenum film on the cleaned bottom surface (selectively depositing molybdenum on the metal-containing bottom surface, 0031 and Fig. 3-5, where the selective deposition of the Mo film and the pre-treatment may be performed in the same station of a processing tool, 0046, such that it will be formed in situ).
They do not teach performing an oxygen and hydrogen plasma.
As discussed above, Subrahmanyan provides the suggestion to have exposed the substrate surface to an oxygen plasma before the hydrogen plasma so as to remove contaminants on the sidewalls and bottom of the recesses.
They do not teach performing a thermal soak.
Na further teaches that the metal-containing surface is selected from a group including cobalt, copper, tungsten, molybdenum, and ruthenium (0006, 0008, and 0021).
As discussed above, Hawrylchak teaches performing multiple cleaning steps to remove oxides and any other contaminants where the cleaning steps can be repeated as needed and include plasma treatments and thermal treatments.
Lin teaches methods for forming a semiconductor structure (abstract). They teach treating a first capping layer by contacting the first capping layer with a metal chloride in an amount sufficient to remove any oxide layer disposed upon a first surface of the first capping layer (0022). They teach that tungsten chloride, tungsten oxytetrachloride, etc. can be used (0022). They teach that metal chlorides are contacted with the first surface of the first capping layer under conditions sufficient to remove an oxide layer such as a native oxide layer disposed upon the first surface, where the temperature ranges from 300°C to 450°C for a duration of 1 second to 600 seconds (0022). Therefore, Lin teaches that a tungsten oxytetrachloride thermal soak is desirable for removing oxides.
Roy teaches removing WOx by etching using WCl5, WCl6, WOCl4, or other etchants (0014). They teach that the reactions proceed thermally (0047).
From the teachings of Hawrylchak Lin, and Roy, 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 included an in situ thermal soak in tungsten oxytetrachloride at about 300-450°C to remove oxides for cleaning because Hawrylchak teaches that thermal treatments can be used in combination with plasma treatments for cleaning substrates where the cleaning treatments can be performed and repeated as needed, Lin teaches that a tungsten oxytetrachloride thermal soak at such a temperature is desirable for removing oxides, and Roy teaches that a WOCl4 thermal treatment also removes oxides from tungsten surfaces, where Na teaches that the metal-containing surface is tungsten such that it will be expected to further facilitate the removal of metal oxides from the substrate surface.
They do not teach using ex-situ and in-situ cleaning steps.
As discussed above Coolbaugh provides the suggestion to have combined ex-situ and in-situ cleaning techniques because Coolbaugh teaches that it is conventionally known to provide an ex-situ oxide removal step and an in-situ hydrogen treatment to remove remaining oxide from exposure to air such that it will be expected to provide the cleaning steps as desired. Further, since Lin suggests performing the thermal soak for the purposes of removing oxides, 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 this step ex-situ and then to have performed at least the hydrogen plasma step in-situ because Coolbaugh suggests an ex-situ oxide removing step followed by an in-situ hydrogen treatment step to remove remaining oxides, suggesting that such a sequence is suitable.
They do not teach performing a pump and purge step.
As discussed above Lee provides the suggestion to have performed a pumping and purging step to remove water vapor or moisture from the via on the substrate before performing the ex-situ thermal soak and before performing the in-situ plasma treatment because Lee teaches that it is desirable to remove moisture from structures and residual gas on a substrate prior to deposition such that it will be expected to help remove undesired moisture from the substrate in preparation for cleaning so as to avoid any undesired side reactions between the process gases and the moisture or residual gas (air) on the surface and to ensure an exposed surface for cleaning.
Regarding claim 3, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches that the metal-containing surface is selected from a group including cobalt, copper, tungsten, molybdenum, and ruthenium (0006, 0008, and 0021).
Subrahmanyan teaches that the conductive sublayer located beneath the dielectric layer is selected from materials including copper (Col. 4, lines 41-52).
Regarding claim 4, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches that the sidewall surfaces are dielectric surfaces formed from silicon-based oxides, i.e. SiOx, or silicon nitrides (0023-0024).
Subrahmanyan teaches that the dielectric layer is silicon dioxide (Col. 4, lines 41-52).
Regarding claim 14, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1. Na further teaches selectively depositing the molybdenum film by ALD (0005).
Regarding claims 13, 15, and 16, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1.
They do not teach the selectivity compared to similar processes performed without the plurality of chemical exposures, the roughness of the molybdenum film, or the grain size.
Na teaches selectively depositing Mo using Mo precursors such as MoOCl4 and MoO2Cl2 with a reducing agent such as hydrogen (0032). They teach that temperature affects selectivity, grain size, and resistance (0033). They teach that higher temperatures may reduce selectivity of the Mo film and result in growth on the oxide or nitride of the sidewall surfaces as well as on the metal-containing bottom surface, but if the temperatures are too low, the impurity level may be increased and grain size may be reduced, increasing resistance (0033). They teach that the substrate temperature may be between 350°C and 600°C to selectively deposit Mo using a chlorine-containing chemistry, where the temperature may be between 350-550°C, or 350-450°C (0033). They teach that the chamber pressures may range from 1 to 100 torr (0037).
The instant specification at paragraph 0052 indicates using molybdenum precursors such as MoOCl4 and MoOCl2 with hydrogen and paragraph 0053 indicates using temperatures in the range of 300-550°C with pressures in the range of 10-300 torr.
Therefore, Na teaches depositing molybdenum using the same precursors, a temperature within the range used in the instant specification, and at a pressure overlapping the range used in the instant specification. Since Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1, where Na indicates that the selectivity and grain size of the film is dependent on temperature and they deposit the films at a temperature within the range used in the instant specification (with the same precursors and an overlapping pressure range) the resulting films are expected to have properties meeting the requirements of claims 13 (i.e. selectivity), 14 (surface roughness), and 15 (grain size). According to MPEP 2112.01 I, “Where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established. In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977)”.
Subrahmanyan further teaches that performing a precleaning treatment on a barrier layer before depositing a metal that fills the feature improves the texture, grain orientation, and grain size of copper on the barrier layer resulting in good surface topography and tighter distribution of grain orientations (Col. 8, lines 8-31), indicating that such a cleaning process is known to improve grain size and topography of a deposited film.
Claim 2 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of L Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee as applied to claim 1 above, and further in view of Schloss, WO 2021/076636 A1.
Regarding claim 2, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1. Subrahmanyan teaches that the decrease in the width of features in forming vias, contacts, and other features results in larger aspect ratios for the features and increased difficulty in cleaning the features prior to filling (Col. 1, lines 22-35). They teach that there is a great amount of effort directed at cleaning small features having high aspect ratios, especially where the ratio of feature height to width is 4:1 or larger (Col. 1, lines 22-35). They teach that the submicron features have a high aspect ratio with steep sidewalls (Col. 5, lines 12-21).
They do not teach the aspect ratio of the via for depositing molybdenum.
Schloss teaches method of filling features with molybdenum (abstract). They teach that substrates have features such as vias or contact holes, which may be characterized by high aspect ratios (0038). They teach that the feature may have an aspect ratio of at least about 2:1, at least about 4:1, at least about 6:1, etc. (0038). Therefore, Schloss teaches filling vias with molybdenum where the vias have an aspect ratio of at least about 2:1 or at least about 4:1.
From the teachings of Subrahmanyan and Schloss, 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 Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee to have deposited the molybdenum films in vias having aspect ratios of at least 2:1 or at least 4:1 because Schloss teaches that such aspect ratios are desirable for vias that are filled with molybdenum and Subrahmanyan teaches that it is known to use vias with an aspect ratio of 4:1 or larger such that it will be expected to provide a suitable via size range for filling with molybdenum. Therefore, the aspect ratio will overlap the range of claim 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.” In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976).
Claim 9 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of Subrahmanyan, Hawrylchak, Lin, Coolbaugh, Roy, and Lee as applied to claim 1 above, and further in view of Theodosiou, US 2015/0075973 A1.
Regarding claim 9, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1, where the hydrogen plasma removes oxides. Subrahmanyan teaches that the features may contain redeposited material on the feature surfaces following a sputter etch preclean process (Col. 4, lines 53-67), indicating that the cleaning process can be used to remove any redeposited material resulting from a previous sputter etching process.
As noted above, Hawrylchak teaches performing multiple cleaning steps to remove oxides and any other contaminants where the cleaning steps can be repeated as needed.
They do not teach using a hydrogen plasma with argon sputtering.
As discussed above, from the teachings of Hawrylchak and Theodosiou, 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 a hydrogen plasma/Ar sputter etching process so as to remove oxide from the metal surface with using an RF bias source so as to provide directionality in an ICP plasma (because the ions will be attracted to the substrate) because Hawrylchak teaches that multiple cleaning steps can be performed, Subrahmanyan teaches that the cleaning process can be done following a sputter etch clean, and Theodosiou teaches that adding hydrogen to an Ar sputter etching process formed from and ICP plasma with directionality provided by an RF bias reduces the level of CO contamination, reduces unwanted contaminants produced during the sputter etching process, removes oxides, and improves the productivity of the process such that it will be expected to provide a desirable oxide removal step.
Claim 10 is rejected under 35 U.S.C. 103 as being unpatentable over Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee as applied to claim 1 above, and further in view of Cen, US 2020/0303250 A1 and Hein, US 2004/0076837 A1.
Regarding claim 10, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 1. Na teaches performing a hydrogen plasma pre-treatment for reducing metal oxides on the metal-containing surface (0029).
Lee teaches degassing at a temperature of within a range of about 100°C to about 600°C (0029).
Lin teaches performing the thermal soak at a temperature in the range of 300°C to 450°C (0022).
They do not teach the temperature for the oxygen and hydrogen plasma treatments.
Cen teaches pre-cleaning using hydrogen radicals to reduce metal oxides, where the hydrogen radicals are formed in a remote plasma source and the substrate is maintained at a range from about 200°C to about 400°C (0017).
Hein teaches applying a coating to a substrate, particularly a metal substrate (abstract). They teach that the substrate has an optically-transparent coating such as SiOxCyHz on at least a portion of the substrate (0005). They teach cleaning the substrate using a pre-clean process where the substrate temperature is maintained at more than 100°C (0027). They teach that oxygen is fed to the chamber for plasma cleaning (0027).
From the teachings of Lee, Lin, Cen, and Hein, 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 temperature of the plurality of chemical exposures to be within the claimed range because Lee teaches pumping and purging at temperatures within the claimed range, Lin teaches performing a thermal soak at temperature within the claimed range, Cen teaches performing a hydrogen plasma cleaning for reducing oxides at temperatures within the claimed range, and Hein teaches performing an oxygen plasma cleaning process at a temperature overlapping the claimed range, such that by optimizing the temperature to be within the claimed range it will be expected to provide a desirable temperature for removing oxides, moisture, and any other contaminants from the via using the pump/purge, oxygen plasma, and hydrogen plasma cleaning processes. According to MPEP 2144.05 II A, “Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. “[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).
Claims 17-19 are rejected under 35 U.S.C. 103 as being unpatentable over Na, WO 2021/046058 A1 in view of Subrahmanyan, US 6,107,192, Hawrylchak, US 2019/0067006 A1, Lin, US 2020/0111885 A1, Roy, US 2020/0194304 A1, Coolbaugh, US 2022/0229228 A1, Lee, US 2022/0081759 A1, and Su, US 2022/0271130 A1.
Regarding claims 17 and 18, as discussed above for claims 1 and 21, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee suggest the process of claim 17, however, they do not teach recessing a line of metal material to form the feature.
Su teaches recessing a source/drain contact using a selective wet etch process so as to selectively recess metal fill layer 222 (0026 and Fig. 9). They teach that the process extends the source/drain contact via opening resulting in a crater like top surface (0026 and Fig. 9). They teach that the recess may improve adhesion and increase the interface surface area with the to-be-formed source/drain contact via 240 (0026 and Fig. 9). They teach forming the source/drain contact via 240 by metal deposition and surface planarization (0027 and Fig. 10). Therefore, Su teaches recessing a metal line in the bottom of a feature on a substrate where the recessing results in improved adhesion of a subsequently deposited metal fill material.
From the teachings of Su, 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 L Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, and Lee to have recessed the metal material at the bottom of the via (i.e. a line of metal material) using a selective wet etch to form the feature comprising at least one surface defining a via having a bottom surface and two sidewalls, the via having a depth to the bottom surface comprising a recessed metal material and a width between the two sidewalls comprising a dielectric because Su teaches that such a recess improves adhesion between a metal material and a deposited metal fill material such that it will be expected to improve the adhesion of the molybdenum material to the metal contact as the bottom of the via.
Regarding claim 19, Na in view of Subrahmanyan, Hawrylchak, Lin, Roy, Coolbaugh, Lee, and Su suggest the process of claim 17. Na teaches filling the via with the molybdenum film (abstract and Fig. 4 and Fig. 5) such that the molybdenum film will be deposited entirely within the via.
Response to Arguments
Applicant's arguments filed 1/30/2026 have been fully considered.
Regarding Applicant’s arguments over the beneficial results of the claimed process, as discussed above, the prior art suggests performing a thermal soak, an oxygen plasma, and a hydrogen plasma for cleaning a substrate surface, where cleaning steps can be combined, and where in situ and ex situ cleaning steps are also known to be combined. Therefore, the combination of the prior art is also expected to provide the claimed benefits in the absence of a showing that the claimed combination provides unexpectedly better results.
In response to applicant's argument that the examiner's conclusion of obviousness is based upon improper hindsight reasoning, it must be recognized that any judgment on obviousness is in a sense necessarily a reconstruction based upon hindsight reasoning. But so long as it takes into account only knowledge which was within the level of ordinary skill at the time the claimed invention was made, and does not include knowledge gleaned only from the applicant's disclosure, such a reconstruction is proper. See In re McLaughlin, 443 F.2d 1392, 170 USPQ 209 (CCPA 1971). In the current case, the prior art provides the suggestion of performing a thermal soak, an oxygen plasma, and a hydrogen plasma for cleaning a substrate surface, performing pump and purge steps to remove moisture from substrates, where cleaning steps can be combined, and where in situ and ex situ cleaning steps are also known to be combined, therefore, the prior art is considered to suggest performing a combination of the claimed cleaning steps and optimizing the steps to be either ex-situ or in-situ as claimed to provide the desired cleaning. As noted in the rejection above, MPEP 2144.04(IV)(C) was also cited for the suggestion that the order of the claimed steps would be obvious over the prior art in the absence of showing that the order was critical.
In response to applicant's argument that Coolbaugh is nonanalogous art, it has been held that a prior art reference must either be in the field of the inventor’s endeavor or, if not, then be reasonably pertinent to the particular problem with which the inventor was concerned, in order to be relied upon as a basis for rejection of the claimed invention. See In re Oetiker, 977 F.2d 1443, 24 USPQ2d 1443 (Fed. Cir. 1992). In this case, Coolbaugh is directed to forming conductive materials in features by epitaxial deposition processes such as CVD, where they describe cleaning the surface prior to deposition (abstract, 0011, 0047, and 0051). Therefore, the reference is considered to be pertinent to the problem with which the inventor was concerned because it discussed cleaning the surface prior to deposition in a feature and further it is in the field of vapor deposition. While it is not directed to molybdenum, the process of cleaning substrates prior to deposition is also expected to be applicable to molybdenum deposition.
As discussed above, the combination of Na in view of Subrahmanyan, Thombare, Coolbaugh, and Lee is considered to suggest optimizing the order of the claimed cleaning steps in the absence of a showing that the order is critical.
Regarding Applicant’s arguments over Schloss, while Schloss teaches depositing a layer of molybdenum and then treating the deposited layer, the reference was relied upon for the suggestion of suitable aspect ratios for vias that are filled with molybdenum. Further, the treatment of Schloss is understood to be done in the process of filling and not for cleaning. Therefore, the modification with Schloss is not considered to change the principle of operation of Na because the only modification from Schloss is to provide a suitable aspect ratio for the vias. Additionally, it also is not considered to lead away from Na because Schloss provides the treatment in the deposition of the molybdenum layer. Further, the claimed process does not prohibit treating an already deposited molybdenum layer.
Regarding Applicant’s argument that nothing in Lin discloses, teaches, or suggests "a plurality of chemical exposures defining a cleaning cycle configured to clean the bottom surface (which comprises one or more of copper (Cu), cobalt (Co), tungsten (W), molybdenum (Mo), and ruthenium (Ru), while only claim 3 requires the use of the listed material, the rejection has been modified to include Roy which also indicates that WOCl4 removes oxides from tungsten.
Applicant’s arguments over Coolbaugh and Schloss are discussed above.
As to the combination of Na in view of Lee, Subrahmanyan, Hawrylchak, Lin, Roy, and Su, the combination is also considered to render the process of claims 17-19 obvious in the absence of a showing that the order of the claimed steps is critical.
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 CHRISTINA D MCCLURE whose telephone number is (571)272-9761. The examiner can normally be reached Monday-Friday, 8:30-5:00 EST.
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/CHRISTINA D MCCLURE/Examiner, Art Unit 1718 /GORDON BALDWIN/Supervisory Patent Examiner, Art Unit 1718
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