Trials@uspto.gov
`Tel: 571-272-7822
`
`Paper 11
`Entered: July 24, 2017
`
`UNITED STATES PATENT AND TRADEMARK OFFICE
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`
`
`
`MICRON TECHNOLOGY, INC.,
`Petitioner,
`
`v.
`
`PRESIDENT AND FELLOWS OF HARVARD COLLEGE,
`Patent Owner.
`
`
`
`Case IPR2017-00664
`Patent 8,334,016 B2
`
`
`Before CHRISTOPHER L. CRUMBLEY, JON B. TORNQUIST, and
`CHRISTOPHER M. KAISER, Administrative Patent Judges.
`
`TORNQUIST, Administrative Patent Judge.
`
`DECISION
`Institution of Inter Partes Review
`37 C.F.R. § 42.108
`
`
`
`
`
`
`
`
`
`
`
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`IPR2017-00664
`Patent 8,334,016 B2
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`I. INTRODUCTION
`Micron Technology, Inc. (“Petitioner”) filed a Petition (Paper 1,
`“Pet.”) requesting an inter partes review of claims 1, 2, 7, 8, and 10 of U.S.
`Patent No. 8,334,016 B2 (Ex. 1001, “the ’016 patent”). The President and
`Fellows of Harvard College (“Patent Owner”) filed a Preliminary Response
`to the Petition (Paper 8, “Prelim. Resp.”).
`We have authority to determine whether to institute an inter partes
`review. 35 U.S.C. § 314; 37 C.F.R. § 42.4(a). The standard for instituting
`an inter partes review is set forth in 35 U.S.C. § 314(a), which provides that
`an inter partes review may not be instituted “unless the Director
`determines . . . there is a reasonable likelihood that the petitioner would
`prevail with respect to at least 1 of the claims challenged in the petition.”
`After considering the Petition and the Preliminary Response, we
`determine that Petitioner has demonstrated a reasonable likelihood of
`prevailing with respect to claims 1, 2, 7, 8, and 10 of the ’016 patent.
`Accordingly, we institute inter partes review with respect to those claims.
`
`A. Related Proceedings
`The parties note that the ’016 patent is at issue in President and
`Fellows of Harvard College v. Micron Tech., Inc., 1:16-cv-11249 (D.
`Mass.), President and Fellows of Harvard College v. GlobalFoundries U.S.,
`Inc., IPR2017-00663, and IPR2017-00666. Pet. 2; Paper 5, 1. The parties
`further note that related U.S. Patent No. 6,969,539 is at issue in the above–
`noted district court proceedings as well as IPR2017-00662. Pet. 2; Paper 5,
`1.
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`B. The ’016 Patent
`The ’016 patent discloses “reagents for use in thin film deposition
`processes such as chemical vapor deposition (CVD) and atomic layer
`deposition (ALD).” Ex. 1001, 1:30–32.
`“In CVD processes, a reactant vapor or vapor mixture is brought into
`contact with a heated surface on which a thin film is deposited.” Id. at 1:46–
`48. In ALD (which is a type of CVD process) “a metered amount of a first
`reactant component” is introduced into a deposition chamber to deposit a
`thin layer of this first reactant on a substrate. Id. at 20:57–60. Excess vapor
`is removed from the chamber and “a metered amount of a second reactant
`component is then introduced into the deposition chamber” where it
`“interacts with the already deposited layer of the first reactant.” Id. at
`20:60–21:5. The ’016 patent explains that, because the surface reactions in
`the ALD process are “self-limiting,” the process may be used to provide a
`“reproducible layer of predictable composition” with “improved step
`coverage and thickness uniformity compared to CVD with mixed vapors.”
`Id. at 1:48–54, 20:64–67, 21:5–7.
`In certain embodiments of the ’016 patent, metal or metalloid amides
`may be used as a reactant. Id. at 10:4–9. Table I of the ’016 patent provides
`a list of known amides for use in the disclosed ALD process, including
`tetrakis(dimethylamino)–, tetrakis(diethylamino)–, and
`tetrakis(ethylmethylamino)–hafnium and zirconium. Id. at Table I.
`
`C. Illustrative Claim
`Claim 1, reproduced below, is the only independent claim of the ’016
`patent and is illustrative of the challenged claims:
`1. A process for making an insulator in a microelectronic
`device, the process comprising:
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`introducing a first reactant component into a deposition
`chamber;
`introducing a second reactant component into the deposition
`chamber; and
`alternately repeating introducing the first reactant
`component and the second reactant component into the
`deposition chamber;
`wherein deposition of the first reactant component and the
`second reactant component are self-limiting;
`wherein said first reactant component comprises a metal
`alkylamide;
`wherein said second reactant component interacts with the
`deposited first reactant component to form the insulator;
`and
`wherein said insulator comprises oxygen and the metal from
`the metal alkylamide.
`Ex. 1001, 30:9–26.
`
`D. The Asserted Grounds of Unpatentability
`Petitioner contends that claims 1, 2, 7, 8, and 10 of the ’016 patent are
`unpatentable based on the following grounds (Pet. 29–50):1
`References
`Basis Claim(s) Challenged
`Senzaki2 and Min3
`§ 103 1, 2, 7, and 10
`
`Senzaki, Min, and Shin4
`
`§ 103 8
`
`
`1 Petitioner also relies on a declaration from Dr. Sanjay Banerjee (Ex. 1003).
`2 U.S. Patent No. 6,537,613 B1, filed Apr. 10, 2000 and issued Mar. 25,
`2003 (Ex. 1005).
`3 Jae–Sik Min, et al., Atomic Layer Deposition of TiN Films by Alternate
`Supply of Tetrakis (ethylmethylamino)–Titanium and Ammonia, 37
`JAPANESE JOURNAL OF APPLIED PHYSICS, No. 9A, 1998, pp. 4999–5004 (Ex.
`1006).
`4 Korean Patent No. 0156980, published Jan. 28, 1997 (Ex. 1007).
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`Petitioner presents evidence that Min and Shin are prior art under 35
`
`U.S.C. § 102(b) and Senzaki is prior art under §102(e). Pet. 22 n.10, 25
`n.13, 27 n.14 (noting that Shin was published on January 28, 1997). Patent
`Owner does not, at this stage of the proceeding, challenge the prior art status
`of any reference.
`
`II. ANALYSIS
`
`A. Claim Construction
`In an inter partes review, “[a] claim in an unexpired patent shall be
`given its broadest reasonable construction in light of the specification of the
`patent in which it appears.” 37 C.F.R. § 42.100(b); Cuozzo Speed Techs.,
`LLC v. Lee, 136 S. Ct. 2131, 2142 (2016) (upholding the use of the broadest
`reasonable interpretation standard). In determining the broadest reasonable
`construction, we presume that claim terms carry their ordinary and
`customary meaning. See In re Translogic Tech., Inc., 504 F.3d 1249, 1257
`(Fed. Cir. 2007). A patentee may define a claim term in a manner that
`differs from its ordinary meaning; however, any special definitions must be
`set forth in the specification with reasonable clarity, deliberateness, and
`precision. See In re Paulsen, 30 F.3d 1475, 1480 (Fed. Cir. 1994).
`Petitioner and Patent Owner do not propose a construction for any
`claim terms of the ’016 patent. Pet. 21; Prelim. Resp. 22. And, upon review
`of the parties’ arguments and supporting evidence, we determine that no
`claim terms require construction for purposes of this Decision. See Vivid
`Techs., Inc. v. Am. Sci. & Eng’g, Inc., 200 F.3d 795, 803 (Fed. Cir. 1999)
`(“[O]nly those terms need be construed that are in controversy, and only to
`the extent necessary to resolve the controversy.”).
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`B. Claims 1, 2, 7, and 10 over Senzaki and Min
`Petitioner contends that the subject matter of claims 1, 2, 7, and 10
`would have been obvious over Senzaki and Min. Pet. 29–45.
`
`1. Senzaki
`Senzaki discloses a process for the deposition of “a multiple metal and
`metalloid compound layer with a compositional gradient of the metal and
`metalloid.” Ex. 1005, 2:33–36.
`In the process of Senzaki, two or more metal–ligand and metalloid–
`ligand precursors are provided, wherein the ligands are selected from the
`group consisting of “alkyls, alkoxides, . . . [and] amides.” Id. at 2:36–43.
`These precursors are delivered to a depositions zone to contact a substrate
`under “deposition conditions.” Id. at 2:43–50. The temperature of the
`deposition is then varied by at least 40º C to deposit a metal/metalloid
`compound layer having a compositional gradient. Id. at 2:50–57.
`In one exemplary embodiment, precursors Zr(NEt2)4 and Si(NMe2)4
`are used to deposit a Zrx–Siy–Oz film. Id. at 3:40–42, 5:11–42. Senzaki
`explains that the metal applied may be selected from a broad range of
`additional metals, including titanium and hafnium. Id. at 4:63–5:3. Senzaki
`also discloses that “[a]n oxygen source can be added” as a reactant “to result
`in a metal–metalloid oxide” or “a nitrogen source can be added to result in a
`metal–metalloid nitride” layer. Id. at 2:57–61, 3:63–66.
`Although the process is generally described in terms of thermal low
`pressure CVD, Senzaki explains that the disclosed precursors could also be
`deposited by atomic layer deposition. Id. at 2:50, 4:4–9. Senzaki explains:
`In atomic layer deposition, an approximately single layer of
`precursor molecules are adsorbed on a surface. A second
`reactant is dosed onto the first precursor layer followed by a
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`reaction between the second reactant and the first reactant
`already on the surface. This alternating procedure is repeated to
`provide the desired thickness of element or compound in a near
`atomic thickness layer.
`Id. at 4:9–15.
`
`2. Min
`Min discloses the use of tetrakis(ethylmethylamino)-titanium, or
`TEMAT, and ammonia in an ALD process to form a TiN film. Ex. 1006,
`4999–5000. According to Min, the use of these components in an ALD
`process results in TiN films “with improved conformality,” which is “crucial
`for the interconnection of metals in ultralarge-scale integrated circuits.” Id.
`at 4999.
`In Min, the disclosed layers are deposited on a SiO2 substrate via
`alternate supply of TEMAT and NH3 in the reactor, with an inert Argon (Ar)
`pulse used to purge the reactor between each step. Id. Figure 2 of Min
`shows this gas switching method:
`
`
`Figure 2 shows the sequential injection of gas reactants in Min.
`As shown in Figure 2, the reactants of Min are injected into the reactor in the
`following order: “TEMAT vapor pulse, Ar purge gas pulse, NH3 gas pulse
`and Ar purge gas pulse.” Id. These four pulses define one cycle and may be
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`repeated multiple times to achieve a desired film thickness. Id. at 4999,
`5001, Abstract.
`
`Min explains that at temperatures of 175º C and 200º C, film thickness
`per cycle is saturated5 at around 0.5 nm/cycle. Id. at 5001. “After saturation
`level is reached, film thickness per cycle remains constant, and saturation
`level is independent of both the TEMAT pulse time and the substrate
`temperature.” Id. According to Min, these results indicate that the process
`is “self-limiting,” which is a “distinct characteristic” of ALD processes. Id.
`
`Min notes that “the carbon impurity in films produced by ALD was
`below” 4%, which “was much lower than the [25%] in films produced at
`300ºC using TEMAT without NH3 by MOCVD,” and “slightly lower than
`the [5%] in film produced at 200ºC using TEMAT with NH3 by MOCVD.”
`Id. at 5002. Min postulates that this reduction in carbon atom concentration
`in the disclosed ALD process “can be attributed to the post-purge process6
`followed by the introduction of reactant gas.” Id.
`
`3. Claim 1
`Petitioner contends that Senzaki teaches or suggests every limitation
`of claim 1 of the ’016 patent. Pet. 31–35. In particular, Petitioner contends
`that Senzaki teaches using both a metal dialkylamide (Zr(NEt2)4) and an
`oxidant in an ALD process to form an insulating oxide layer on a
`
`
`5 The ’016 patent explains that “[n]ormally, in an ALD process, the dose of
`precursor” delivered “is chosen to be large enough to cause the surface
`reactions to go to completion (also called ‘saturation’).” Ex. 1001, 22:22–
`26.
`6 Min describes a “post-TEMAT Ar purge” and a “post-NH3 Ar purge.” Ex.
`1006, 5000. We understand the term “post-purge process” to refer to these
`Ar purge steps.
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`microelectronic device. Id. Petitioner concedes that Senzaki does not
`explicitly state that the depositions of the first precursor and the second
`reactant are self–limiting, but contends Senzaki’s disclosure of applying “an
`approximately single layer of precursor molecules” on the surface of the
`substrate would indicate to one of ordinary skill in the art that the deposition
`processes in Senzaki “are or can be made to be self-limiting.” Id. at 33
`(citing Ex. 1003 ¶ 121).
`To the extent Senzaki does not expressly disclose that the ALD
`deposition processes are self–limiting, Petitioner contends one of ordinary
`skill in the art would have found it obvious to make the disclosed processes
`self–limiting in view of both Senzaki and Min. Id. at 37–42. Petitioner
`reasons that one of the express goals of Senzaki’s ALD process was to
`provide “a near atomic thickness layer” of the desired element or compound
`and Min discloses that its ALD method provides a film with a “desired
`thickness” through the use of a self–limiting process. Id. at 38–39.
`Patent Owner contends Senzaki and Min would not have rendered the
`subject matter of claim 1 obvious because Senzaki does not disclose a self–
`limiting ALD process using a metal alkylamide to form a metal oxide layer
`and one of ordinary skill in the art would not have sought to modify Senzaki
`in view of Min to yield such a process. Prelim. Resp. 30–31 (citing Ex.
`2101 ¶¶ 179–180). First, Patent Owner contends that Petitioner’s asserted
`combination would “change the cited CVD process described in the
`examples of Senzaki to an ALD process to control film thickness.” Prelim.
`Resp. 28, 35 (asserting that “a person of ordinary skill in the art would not
`have modified the cited Senzaki CVD process in view of Min”), 38 (“A
`person of ordinary skill in the art would have had no reasonable expectation
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`of success modifying Senzaki’s CVD process in view of Min”). Petitioner
`does not assert, however, that one of ordinary skill in the art would have
`modified Senzaki’s disclosed CVD examples. Petitioner contends, instead,
`that Senzaki discloses using its precursors and reactants in both a CVD
`process and an ALD process. Pet. 32–33 (citing Ex. 1005, 4:4–15).
`Second, Patent Owner contends that “Senzaki does not disclose any
`ALD process using a metal alkylamide to form a metal oxide layer.” Prelim.
`Resp. 30–31 (citing Ex. 2101 ¶¶ 179–180). We agree that Senzaki does not
`disclose an explicit example of forming a metal oxide layer using a metal
`alkylamide in an ALD process. Senzaki does disclose, however, the use of a
`Zr(NEt2)4 precursor and an oxidant reactant in a CVD process to form a
`mixed metal/metalloid oxide layer. Ex. 1005, 3:40–43, 3:54–66; Pet. 31–35.
`Senzaki goes on to explain that, “[i]n addition to thermal low pressure CVD,
`the above precursors could be used for . . . atomic layer deposition” and that
`in this ALD process a precursor is added to the reactor and then a second
`reactant is dosed onto the first precursor layer to form the desired
`compositional layer having a “near atomic thickness.” Ex. 1005, 4:4–15
`(emphases added). Finally, Senzaki indicates that the disclosed metal–
`metalloid materials are useful as “gate oxides.” Ex. 1005, 2:18–30, 3:40–66,
`5:15–23. In view of these disclosures, as well as the disclosures of Senzaki
`as a whole, Petitioner has explained sufficiently where Senzaki teaches or
`suggests an ALD process using a metal alkylamide to form a metal oxide
`layer.
`
`Patent Owner also argues that the ALD disclosure of Senzaki is
`limited to a single paragraph and fails to provide any specifics regarding
`how an ALD process could be used to form a compositional gradient.
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`Prelim. Resp. 36, 41–44. And, according to Patent Owner, modifying the
`deposition temperature in an ALD process to affect the composition of the
`resulting layer is contrary to Min’s teaching that the growth rate of the
`deposited film is independent of deposition temperature (at least within the
`ALD window). Id. at 31–33, 44. Patent Owner does not explain, however,
`why the temperature would necessarily be modified in the ALD process of
`Senzaki, as opposed to the CVD processes that are the primary focus of the
`reference.7 Moreover, a prior art patent is presumed enabled and Patent
`Owner’s general questions regarding how Senzaki’s ALD process could
`produce a compositional gradient are not, on this record, sufficient to
`overcome this presumption. See In re Antor Media Corp., 689 F.3d 1282,
`1287–88 (Fed. Cir. 2012) (explaining that “both claimed and unclaimed
`materials disclosed in a patent are presumptively enabling” and that it is the
`patentee’s burden to demonstrate otherwise).
`Patent Owner also contends that Petitioner has conceded that the
`deposition processes of Senzaki are not self–limiting. Prelim. Resp. 30–31;
`Ex. 2101 ¶ 179 (“Petitioner indicates that Senzaki does not disclose wherein
`deposition of the first reactant component and the second reactant
`component are self–limiting.”). We do not agree. The Petition states that a
`person of ordinary skill in the art would have understood that “Senzaki’s
`
`
`7 Patent Owner’s arguments are not without support in Senzaki. For
`example, in the summary of the invention section the disclosed process
`includes depositing a precursor using, inter alia, “atomic layer deposition,”
`and then varying the temperature of the second deposition step. See Ex.
`1005, 2:33–62. Whether this disclosure is separate from the more specific
`disclosure of ALD without temperature modification provided in the detailed
`description of the invention section of Senzaki is a question of fact that is
`better resolved at trial. Compare id. at 2:44–57 with id. at 4:4–15.
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`deposition processes are . . . self-limiting.” Pet. 33; Ex. 1003 ¶ 121. It is
`only “[t]o the extent that [it is determined] that Senzaki does not expressly
`disclose ‘self–limiting’ depositions,” that Petitioner contends it would have
`been obvious to make the process of Senzaki self–limiting in view of Min.
`Pet. 33.
`
`Substantively, the only evidence in support of Patent Owner’s
`argument that Senzaki’s ALD process is not self–limiting is presented by Dr.
`Gladfelter. Ex. 2101 ¶ 179. Dr. Gladfelter provides no support or
`explanation, however, for his conclusion that one of ordinary skill in the art
`would not have understood Senzaki to disclose a self–limiting ALD process.
`Id. Moreover, Senzaki indicates that the disclosed ALD process results in “a
`near atomic thickness layer” and Min discloses that “a self–limiting process”
`is a “distinct characteristic of [an] ALD process.” Ex. 1005, 4:15; Ex. 1006,
`5001. Likewise, numerous prior art references indicate that self–limiting
`growth is a fundamental characteristic of ALD. See Ex. 1008, 937 (noting
`that Atomic Layer Epitaxy8 (ALE) is characterized by its “self–limiting
`growth process”), Abstract (“As the film is growing in a self–limiting
`manner ALE is a promising method to deposit thin, high–quality films for
`micro– and optoelectronics.”); Ex. 1011, 13121 (“Whatever the name, the
`basic ALE strategy involves self–limiting surface reactions that provide the
`atomic layer control of growth.”); Ex. 1012, 837 (“The striking feature of
`ALD is the saturation of all the reaction and purging steps which makes
`growth self–limiting.”). And, in its complaint before the District Court,
`Patent Owner asserted that a “process wherein deposition of the first reactant
`
`
`8 Dr. Banerjee explains that when ALD was originally developed in the
`1970s it was referred to as ALE. Ex. 1003 ¶¶ 42–44.
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`and the second reactant component are self–limiting is part of ALD.” Ex.
`1042 ¶ 50. Thus, on this record, Petitioner has demonstrated sufficiently
`that Senzaki’s ALD process is “self–limiting.”
`
`As noted above, to the extent it is ultimately determined that Senzaki
`does not teach or suggest a self–limiting process, Petitioner presents
`arguments and supporting evidence to explain why one of ordinary skill in
`the art would have found it obvious in view of Min to modify the process of
`Senzaki to make it self-limiting. Pet. 37–42 (asserting that Min discloses a
`method for providing strict control over film thickness, which is an express
`goal of Senzaki). Patent Owner vigorously disputes the factual predicates
`upon which Petitioner bases its arguments. Prelim. Resp. 31–33 (asserting
`that Senzaki and Min have directly contrary goals), 33–36 (asserting that one
`of ordinary skill in the art would not have understood that Senzaki’s CVD
`process could be modified in a routine way to produce predictable results),
`36–38 (asserting that it was not possible to ascertain whether a precursor
`could be used in an ALD process without extensive experimentation), 38–42
`(asserting that a person of ordinary skill in the art would not have had a
`reasonable expectation of success in modifying the CVD process of Senzaki
`in view of Min), 42–44 (asserting that it would not have been obvious to
`modify Senzaki’s CVD process as precursor chemistry is unpredictable and
`CVD precursors cannot be assumed to work in an ALD process).
`The factual dispute presented by the parties, which is supported by the
`competing testimony of Dr. Banerjee and Dr. Gladfelter, creates a material
`issue of fact. In such a situation, we must view the competing testimonial
`evidence “in the light most favorable to the petitioner” when deciding
`whether to institute an inter partes review.
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`See 37 C.F.R. § 42.108(c). And, when the testimonial evidence is viewed in
`this fashion, we determine that Petitioner has demonstrated sufficiently that
`one of ordinary skill in the art would have sought to combine Senzaki and
`Min to use a metal dialkylamide in a self–limiting ALD process to form an
`insulating oxide layer.
`In view of the foregoing, Petitioner has demonstrated a reasonable
`likelihood that claim 1 of the ’016 patent would have been obvious over
`Senzaki and Min.
`
`4. Dependent Claims 2, 7, and 10
`Claim 2 depends from claim 1 and further requires “wherein the
`insulator insulates a gate or a capacitor.” Ex. 1001, 30:27–28. Claim 7
`depends from claim 2 and further requires “wherein the metal alkylamide is
`a zirconium dialkylamide,” and claim 10 depends from claim 7 and further
`requires “wherein the zirconium dialkylamide is
`tetrakis(diethylamido)zirconium.” Id. at 30:37–38, 30:43–44.
`Petitioner contends Senzaki expressly discloses applying the disclosed
`films as a “gate dielectric” in “IC fabrication,” which would insulate a gate.
`Pet. 36 (citing Ex. 1005, 3:40–53, 4:4–15, 5:11–42; Ex. 1003 ¶ 127).
`Petitioner further contends that Zr(NEt2)4 is tetrakis(diethylamido)
`zirconium, a zirconium dialkylamide, as recited in claims 10 and 7,
`respectively. Id.
`Patent Owner does not directly address Petitioner’s arguments with
`respect to claims 2, 7, and 10, but generally contends that these claims
`would not have been obvious over Senzaki and Min because claim 1, from
`which claims 2, 7, and 10 depend, would not have been obvious over these
`references. Prelim. Resp. 27–30.
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`For the reasons set forth above, Petitioner has demonstrated
`sufficiently that the subject matter of claim 1 is taught or suggested in
`Senzaki and Min. Petitioner has also identified sufficiently where Senzaki
`discloses the subject matter of claims 2, 7, and 10. Thus, on this record,
`Petitioner demonstrates a reasonable likelihood that claims 2, 7, and 10
`would have been obvious over Senzaki and Min.9
`
`C. Claim 8 over Senzaki, Min, and Shin
`Claim 8 depends from claim 7 and recites, “wherein the zirconium
`dialkylamide is tetrakis(ethylmethylamido)zirconium.” Ex. 1001, 30:39–40.
`Petitioner contends that the subject matter of claim 8 would have been
`obvious in view of Senzaki, Min, and Shin. Pet. 45–50.
`
`1. Shin
`Shin discloses precursor compounds used to deposit a metal nitride
`film over a silicon substrate. Ex. 1007, 1.10 In particular, Shin disclose the
`use of an organicmetallic precursor compound defined by the formula
`M[N(CH3)C2H5]X, wherein M is selected from the metallic elements
`
`
`9 Petitioner also contends that it would have been obvious to use a hafnium
`dialkylamide precursor, as recited in claim 3, in Senzaki’s ALD process.
`Pet. 37. Petitioner does not assert a ground with respect to claim 3. Nor
`does Petitioner address claim 3 in its claim analysis or identify a prior art
`reference that teaches or suggests the use of hafnium dialkylamide
`precursors in an ALD process. Indeed, in another portion of the Petition
`Petitioner concedes that “Senzaki does not disclose hafnium-based
`precursors.” Id. at 31. Accordingly, to the extent Petitioner intended to
`include claim 3 within its ground based on Senzaki and Min, Petitioner has
`not demonstrated sufficiently that claim 3 would have been obvious over
`these references.
`10 Citations to Shin are to page numbers provided in the lower right corner of
`the document.
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`belonging to group 3, group 4, and group 5 on the periodic table, and X is an
`integer between 3–5. Id. at 1–2, 7.
`Shin discloses that any metallic element within groups 3–5 on the
`periodic table is “suitable,” but focuses its discussion primarily on the
`deposition of titanium films. Id. at 7. Shin notes that tetrakis diethyl amino
`amino titanium and tetrakis dimethyl amino amino titanium were widely
`used as precursors for the deposition of titanium nitride thin films. Id. Use
`of the dimethyl form, however, was found to result in carbon impurities “of
`about 27–30% within the film,” and use of the diethyl form, although it
`“showed a decrease of 15–25% in the content of carbon impurity and an
`increase in the speed of deposition,” was found to be inferior to the use of
`the dimethyl form with respect to depositing a thin film with an even
`thickness. Id. at 5–6.
`
`Shin discloses that tetrakis(ethylmethylamido) titanium “exhibits the
`intermediate characteristics” of tetrakis dimethyl amino amino titanium and
`tetrakise diethyl amino amino titanium, and can “neutralize more or less” the
`problems caused by those two compounds. Id. at 7. Shin also notes that the
`disclosed compounds “can be made easily,” and provides an example
`process for forming both tetrakis(ethylmethylamino) titanium and
`tetrakis(ethylmethylamino) zirconium. Id. at 7–9.
`
`2. Analysis
`Petitioner asserts that Shin expressly discloses
`tetrakis(ethylmethylamino) zirconium,11 as recited in claim 8. Pet. 27–28,
`
`
`11 Shin discloses tetrakise(ethylmethylamido) zirconium, whereas the claims
`recite tetrakis(ethylmethylamino) zirconium (tetrakise vs. tetrakis). Neither
`party asserts that there is a difference between these two compounds.
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`46–47. Petitioner further asserts that a person of ordinary skill in the art
`would have sought to use this compound in the ALD process of Senzaki and
`Min. In support, Dr. Banerjee testifies that Shin’s disclosure that the
`–ethylmethylamino form of a transition metal dialkylamide “exhibits the
`intermediate characteristics of” the –diethylamino and –dimethylamino
`forms of the same transition metal dialkylamides, while neutralizing the
`shortcomings of these compounds, would have suggested to one of ordinary
`skill in the art to try this intermediate form in Senzaki’s ALD process. Ex.
`1003 ¶¶ 142–143; Pet. 48–49.
`Patent Owner responds that changing even a single alkyl group can
`result in unpredictable changes in the properties of a compound and “could
`affect a precursor’s applicability” in an ALD process. Prelim. Resp. 46–47
`(citing Ex. 2101 ¶ 220). In support, Patent Owner notes that Table 1 of the
`’016 patent shows that Hf(NEt2)4, which differs from Hf(NMe2)4 by only
`one alkyl group, is liquid at room temperature whereas Hf(NMe2)4 is a solid.
`Id. at 47 (citing Ex. 2116, Table 1; Ex. 2101 ¶ 220).
`As noted by Patent Owner, Table 1 of the ’016 patent indicates that
`Hf(NEt2)4 is liquid at room temperature and that Hf(NMe2)4 does not become
`a liquid until it reaches 30º C. Ex. 1001, Table 1. Neither Patent Owner nor
`Dr. Gladfelter explains sufficiently, however, why this result is
`unpredictable. Nor do they explain why the phase of a precursor at room
`temperature is relevant to whether that precursor will be useful in an ALD
`process; indeed, the ’016 patent indicates that Hf(NMe2)4 may be used
`successfully in an ALD process to form HfO2. Id. at 26:45–27:43.
`Patent Owner also argues that Shin is directed to CVD and not ALD
`and “[j]ust because one CVD precursor described in Shin was found to be
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`successful in achieving self-limiting ALD, it does not mean that the rest of
`the CVD precursors in Shin will work in ALD.” Prelim. Resp. 47–50. Here,
`Shin discloses the use of both tetrakis(ethylmethyl)titanium and zirconium
`and discloses that the ethylmethyl– form provides advantages over the
`diethyl and dimethyl forms in a CVD process. Ex. 1007, 7, Abstract.
`Whether these disclosures, when combined with the disclosures of Senzaki
`and Min, would have given an ordinary artisan a reasonable expectation of
`success in using tetrakis(ethylmethyl)zirconium in the ALD process of
`Senzaki to produce an oxide insulating layer, as asserted by Petitioner and
`Dr. Banerjee, is a question of material fact that is best resolved at trial.
`As noted above, Petitioner provides an explanation, supported by both
`documentary and testimonial evidence, as to why one of ordinary skill in the
`art would have sought to combine Senzaki, Min, and Shin to result in the
`process of claim 8. And, although Patent Owner vigorously contests the
`factual predicates underlying this explanation, on this record, and given the
`requirement that we view the testimonial evidence in the light most
`favorable to Petitioner at this stage of the proceeding, see 37 C.F.R.
`§ 42.108(c), we determine that Petitioner has demonstrated a reasonable
`likelihood that claim 8 of the ’016 patent would have been obvious over
`Senzaki, Min, and Shin.
`
`III. CONCLUSION
`Upon consideration of the Petition and the Preliminary Response, we
`conclude that Petitioner has demonstrated a reasonable likelihood that claims
`1, 2, 7, 8, and 10 would have been obvious over the recited prior art.
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`Accordingly, we institute inter partes review with respect to these claims as
`set forth in the Order.
`
`IV. ORDER
`
`It is hereby
`ORDERED that, pursuant to 35 U.S.C. § 314, an inter partes review
`is instituted on the following grounds:
`(1) Whether claims 1, 2, 7, and 10 are unpatentable under 35 U.S.C.
`§ 103 as having been obvious over Senzaki and Min; and
`(2) Whether claim 8 is unpatentable under 35 U.S.C. § 103 as having
`been obvious over Senzaki, Min, and Shin;
`FURTHER ORDERED that no ground other than those specifically
`granted above are authorized for inter partes review as to the claims of the
`’016 patent.
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`PETITIONER:
`
`Jeremy Jason Lang
`WEIL, GOTSHAL & MANGES LLP
`jason.lang@weil.com
`
`
`PATENT OWNER:
`
`Reza Mollaaghababa
`Thomas Engellenner
`Andrew Schultz
`PEPPER HAMILTON LLP
`mollaaghababar@pepperlaw.com
`engellennert@pepperlaw.com
`schultza@pepperlaw.com
`
`
`
`
`
`
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