INGEVITY SOUTH CAROLINA, LLC, EXHIBIT 2001
`BASF Corporation v. Ingevity South Carolina, LLC
`IPR2019-00202
`
`
`BASF Corporation v. Ingevity South Carolina, LLC
`IPR2019-00202
`
`
`
`Table of Contents
`
`I.
`
`II.
`
`QualificatiOns...........cccccceseccecsssrscceeseecscesssateceeeesesscsnsceseeescusaueeessneesesussseensnseeees 1
`
`Person of Ordinary Skill in the Art... ee cseesscceseeeeeeeeeeeesscsteesrnesseeesseeeseees 5
`
`Il.
`
` Petitioner’s Asserted Prior Art ..0........:ceesescceeeseeeceeseetesseceacecseesseerersesesneasaeeenes 6
`
`A.
`
`B.
`
`C.
`
`USS. Patent No. 6,896,852 to Meiller......... ccc ececccecssseeereseeeessaeeeeeess 7
`
`Japanese Patent Application Publication No. H10-37812 to Abe........ 8
`
`US. Patent No. 5,914,294 to Park .........ccccccsssccccccceecssessnserteessssteesseeess 10
`
`1.
`
`2.
`
`3.
`
`Park’s Honeycombs Do Not Necessarily Have An IAC Less
`Than 35 g/Li wee ecsscesscesensecsseceeeseeesssecenseeceseecssnessnsesasesatenseseenes 10
`
`Petitioner’s Hypothetical Honeycomb Basedon Park’s
`Formulation D Contradicts Park’s Disclosure......... cesses 15
`
`It Is Impossible to Deduce the IAC ofPetitioner’s Hypothetical
`HONGYCOMD 0... eceeceseeeeeseetesssesseseseececseaereaeeraeenaeseneeseeasereesees 25
`
`TV.
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`COnCIUSI001 ose e cece ee eeeceeseccccececccccccescevseccnseesccesecssccnsssesucceecsucuseceaeeseteeseccaveees 28
`
`
`
`I, James A. Ritter, make this declaration based on my personal knowledge and
`
`in support of Patent Owner’s Preliminary Response to BASF’s Petition for Inter
`
`Partes Review.
`
`If sworn as a witness, I could and would testify to the matters
`
`referred to below.
`
`I.
`
`Qualifications
`
`1.
`
`Tam the L. M. Weisiger Professor of Engineering and a Carolina
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`Distinguished Professor in the Department of Chemical Engineering at the
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`University of South Carolina. A copy of my resumeis attached as Appendix A to
`
`this declaration.
`
`2.
`
`I received my associates degree in mathematics and science at
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`Onondaga Community College in Syracuse, New York in 1980.
`
`I earned
`
`bachelor’s and master’s degrees in chemical engineering from the State University
`
`of New York at Buffalo in 1983 and 1985, respectively. The State University of |
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`New York at Buffalo awarded me a Ph.D. degree in chemical engineering in 1989.
`
`3.
`
`After completing my education, I worked as a senior engineerat the
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`Westinghouse Savannah River Company, Savannah River Technology Center, in
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`Aiken, South Carolina from 1989 to 1993.
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`4.
`
`In 1993, I joined the faculty of the University of South Carolina,
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`Department of Chemical Engineering, as an assistant professor.
`
`I became a
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`tenured associate professor in 1999 and a full professor in 2003. Today, I am the
`
`
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`L.M. Weisiger Professor of Engineering and a Carolina Distinguished Professor.
`
`Myresearch at the University focuses on the physio-chemical phenomenaof
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`adsorption, including adsorption processes for gas separation and purification,
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`nanoporous adsorbents for adsorptive separation and purification, and the
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`measurementof diffusion rates in nanoporous adsorbents. Under mydirection, my
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`laboratory at the University has collaborated with numerousindustry partners in
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`researching adsorbents and their commercial uses. Past and current research
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`partners include, for example, MeadWestvaco (which is the predecessor of
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`Ingevity), BASF Corporation, Exxon Research and Engineering Company, BP-
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`Amoco Chemical Company, Shell, NASA, the Department of Energy, and the
`
`Idaho National Engineering and Environmental Laboratory, to name a few.
`
`5.
`
`I am a memberofthe prestigious American Association for the
`
`Advancement of Science anda fellow ofthe leading professional organizations for
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`chemists and chemical engineers, the American Chemical Society and American
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`Institute of Chemical Engineers, respectively.
`
`6.
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`Tam a named inventor on four patents and author of nine copyrighted
`
`works.
`
`7.
`
`I have published and contributed to hundreds of technical papers,
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`books and book chapters, conference proceedings, and other publications in my
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`
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`field. These include publications concerning adsorption ofvolatile organic
`
`compounds on activated carbon adsorbents, such as:
`
`C. E. Holland, $8. A. Al-Muhtaseb, and J. A. Ritter, "Adsorption of C1 to C7
`
`Normal Alkanes on BAX Activated Carbon: 1. Potential Theory Correlation and
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`Adsorbent Characterization,” Ind. Eng. Chem. Res., 40, 338-346 (2001); and
`
`S. A. Al-Muhtaseb, C. E. Holland and J. A. Ritter, “Adsorption of C1 to C7
`
`Normal Alkanes on BAX Activated Carbon:2. Statistically-Optimized Approach for
`
`Deriving Thermodynamic Properties from the Adsorption Isotherm”, Ind. Eng.
`
`Chem.Res., 40, 319-337 (2001).
`
`8.
`
`I have also authored publications concerning the adsorption of
`
`butane, including on activated carbon adsorbents, such as:
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`S. A. Al-Muhtaseb and J. A. Ritter, “New Methodology for the Measurement
`
`and Analysis of Adsorption Dynamics: Butane on Activated Carbon,” Ind. Eng.
`
`Chem.Res., 43, 7075-7082 (2004);
`
`Y. Liu, C. E. Holland and J. A. Ritter, “Pressure Swing Adsorption-Solvent
`
`Vapor Recovery-III: Comparison of Simulation with Experiment for the Butane-
`
`Activated Carbon System,” Sep. Sci. Tech., 34, 1545-1576 (1999);
`
`Butane Vapor Recovery by Pressure Swing Adsorption, AIChE Annual
`
`Meeting, Los Angeles, CA, November 1997, contributed;
`
`
`
`Y. Liu, C. E. Holland and J. A. Ritter, “Butane Vapor Recovery by Pressure
`
`Swing Adsorption,” in Proceedings of the Topical Conference on Separation
`
`Science and Technologies,” American Institute of Chemical Engineers, NY (1997);
`
`Liu, C. E. Holland and J. A. Ritter, “Pressure Swing Adsorption-Solvent
`
`Vapor Recovery-I: Experimental Transient and Periodic Dynamic Behaviorofthe
`
`Butane-Activated Carbon System,” Sep. Sci. Tech., 33, 2311 (1998);
`
`Y. Liu, C. E. Holland and J. A. Ritter, “Pressure Swing Adsorption-Solvent
`
`Vapor Recovery-II: Experimental Periodic Performance of the Butane-Activated
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`Carbon System,” Sep. Sci. Tech., 33, 2431 (1998);
`
`Y. Liu, J. A. Ritter and B. K. Kaul, “Simulation of Gasoline Vapor Recovery
`
`by Pressure Swing Adsorption,” Separation and Purification Technology, 20, 111-
`
`127 (2000).
`
`9.
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`I have also authored publications concerning the measurement and
`
`derivation of adsorption isotherms, suchas:
`
`S. A. Al-Muhtaseb, M. D. LeVan and J. A. Ritter, “On the Correlation of
`
`Modified Antoine’s Adsorption Isotherm Models with Experimental Data,”
`
`Langmuir, 16, 8536-8538 (2000);
`
`J. A. Ritter, et al., “On Deriving Thermodynamic Properties from the
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`Adsorption Isotherm, 24th Biennial Conference on Carbon,” Charleston, SC, July
`
`1999, contributed;
`
`
`
`J. A. Ritter, S. J. Bhadra and A. D. Ebner “On the Use of the Dual Process
`
`Langmuir Model for Correlating Unary and Predicting Mixed Gas Adsorption
`
`Equilibria,” Langmuir, 27, 4700-4712 (2011).
`
`10. Over the course of my career, I have personally measured, and
`
`overseen others who have measured, adsorption of various adsorbates (the
`
`compound to be adsorbed) on various adsorbents (the substrate on which the
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`adsorbate is being adsorbed). From these measurements,I have personally
`
`derived, and overseen others who have derived, adsorption isotherms. My
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`laboratory at the University of South Carolina includes equipmentthat we use to
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`measure adsorptive properties and derive adsorption isotherms, including industry-
`
`standard volumetric and gravimetric physisorption analyzers. Specifically, my
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`laboratory equipment includes an ASAP 2010 volumetric adsorption analyzer from
`
`Micromeritics Instrument Corporation, a Microbalance gravimetric adsorption
`
`analyzer from VTI Corporation (now part of TA Instruments), and a volumetric
`
`adsorption analyzer for high pressures purpose-built in my laboratory.
`
`I consider
`
`myself an expert in such analytical techniques.
`
`II.
`
`Person of Ordinary Skill in the Art
`
`11.
`
`Petitioner’s declaranthas stated: “[A] person of ordinary skill in the
`
`art in the field of evaporative emission control systems and component design
`
`would possess at least a bachelor’s degree in chemistry or chemical or mechanical
`
`
`
`engineering. They would also haveat least one year of experience working
`
`primarily on issues related to the control of automotive evaporative emissions.
`
`They would, given both their education background and experience, understand the
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`chemistry and physics associated with the phenomenaoffuel vapor adsorption,
`
`desorption, and diffusion.” (Ex. 1003 at 718.)
`
`12.
`
`For purposes of my present declaration only, I have adopted
`
`Petitioner’s proposedlevel of skill for a person of ordinary skill in the art
`
`(POSITA)at the time of the ’844 Patent.
`
`Ill.
`
`Petitioner’s Asserted Prior Art
`
`13.
`
`Petitioner relies on alleged applicant admitted prior art (AAPA) and
`
`four primary prior art references: U.S. Patent No. 5,914,294 to Park, U.S. Patent
`
`No. 6,896,852 to Meiller, Japanese Patent Application Publication No. H10-37812
`
`to Abe, and International Patent Publication No. WO 92/01585. Onthe basis of
`
`these four primary prior art references, Petitioner asserts three grounds for
`
`invalidity:
`
`“Ground 1: Claims1, 2, 6, 8, 11, 12, 14-16, 18, 20, 21, 24, 25, 27-29, 31-33,
`
`36, 37, 39-41, 43-45, 48, 49, and 51-53 are rendered unpatentable [obvious] by
`
`Meiller in view of Park and AAPA under 35 U.S.C. §103(a).
`
`
`
`Ground 2: Claims1, 2, 6, 8, 11, 12, 14-16, 18, 20, 21, 24, 25, 27-29, 31-33,
`
`36, 37, 39-41, 43-45, 48, 49, and 51-53 are rendered unpatentable [obvious] by Abe
`
`in view of Park and AAPA under 35 U.S.C. §103(a).
`
`Ground 3: Claims 3-5, 7, and 19 are rendered unpatentable [obvious] by
`
`Meiller in view of Park and Tennison under 35 U.S.C. §103(a).” (Petition at 3-5.)
`
`14.
`
`I discuss the disclosures of Meiller, Abe, and Park below.
`
`A.
`
`U.S. Patent No. 6,896,852 to Meiller
`
`15. Meiller discloses a hydrocarbon emissions scrubber element with an
`
`elongated body,asillustrated in Meiller’s Figures 1, 2, 3A, and 3B, for example.
`
`(Ex. 1016 at 3:51-57.)
`
`
`
`
`
`
`
`
`
`
`
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`16. Méeiller’s disclosure concerns the physical configuration of the
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`scrubber and howit can be adapted to work in conjunction with a fuel vapor
`
`canister. (Ex. 1016 at, e.g., Figures 1-11, 3:53-58.) Meiller does not disclose,
`
`however, anything with regard to the adsorptive properties of its scrubber. In
`
`particular, Meiller does not disclose the adsorption capacity or IAC ofits scrubber.
`
`Nor does Meiller disclose how its scrubber is manufactured. For example, Meiller
`
`does not disclose that the methods of Park can be used to manufacture Meiller’s
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`scrubber. Meiller also does not disclose that scrubbers for air intake systems can
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`be deployed in evaporative emissions control systems or with fuel vapor
`
`canisters—Meiller’s intended use for its scrubber. (Ex. 1016 at 3:58-65.)
`
`17.
`
`Thus, Meiller does not point the POSITAto any particular scrubber—
`
`whether disclosed in Park or elsewhere—for use in an automotive evaporative
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`emissions control system.
`
`B.
`
`Japanese Patent Application Publication No. H10-37812 to Abe
`
`18. Abe discloses an auxiliary canister for use with a main fuel vapor
`
`canister, as illustrated in Abe’s Figure 4, for example. (Ex. 1009 at [0030].).
`
`
`
`[FIG. 4]
`
`
`
`19. Abe discloses that an activated carbon honeycombis preferred for use
`
`in the second,auxiliary canister. (Ex. 1009 at [0016].) The only thing Abe
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`discloses regarding the adsorptive properties of its hydrocarbon scrubberis that it
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`has a “high adsorption speed.” (Ex. 1009 at [016].) (I note that the butane
`
`working capacities Abe discloses in Table 2, for instance, are for the first, main
`
`canister—notthe second, auxiliary canister—which can be seen in the reporting of
`
`working capacities for Comparative Example 1 and Comparative Example 2 even
`
`though those examples do not have a second canister. (Ex. 1009 at [0033].)) Abe
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`does not disclose the adsorption capacity or IAC ofits activated carbon
`
`honeycomb. Nor does Abedisclose howits activated carbon honeycombis
`
`manufactured. For example, Abe does not disclose that the methods of Park can be
`
`used to manufacture Abe’s activated carbon honeycomb. Abealso does not
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`disclose that activated carbon honeycombforair intake systems can be deployed in
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`evaporative emissions control systems or with fuel vapor canisters—Abe’s
`
`intended usefor its activated carbon honeycomb. (Ex. 1009 at Abs.)
`
`
`
`20.
`
`Thus, Abe does not point the POSITAto anyparticular activated
`
`carbon honeycomb—whetherdisclosed in Park or elsewhere—for use in an
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`automotive evaporative emissions control system.
`
`C.
`
`21.
`
`U.S. Patent No. 5,914,294 to Park
`
`Petitioner relies solely on Park to attempt to show that adsorbent
`
`volumes with an JACless than 35 g/L were knowninthe art, as the Challenged
`
`Claimsof the ’844 Patent require. (Ex. 1001 at claims 1, 18, 31, and 45.)
`
`22.
`
`Park discloses a method for creating an adsorptive monolith
`
`comprising activated carbon. (Ex. 1010 at 4:1-6.) Park discloses thatits
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`adsorptive monolith can have a honeycomb shapeorstructure. (Ex. 1010 at Abs.,
`
`4:9-13.) Park does not disclose using any ofits honeycombsto capture
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`evaporative emissions from automotive fuel tanks. Park does notdisclose usingits
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`honeycombsin conjunction with fuel vapor canisters. Indeed, Park does not
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`disclose any evaporative emissions control systemsfor fuel tanksat all, such as
`
`those disclosed by Meiller and Abe.
`
`1.
`
`Park’s Honeycombs Do NotNecessarily Have An IAC Less
`Than 35 g/L
`
`23.
`
`Park does not disclose the adsorptive properties, such as the IAC, of
`
`honeycombs made accordingto its invention. Based on Park’s broad disclosure,
`
`honeycombs madeaccordingto its invention would have a wide range of IACs,
`
`including IACs greater than 35 g/L.
`
`10
`
`
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`24.
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`Park discloses making monoliths using an extrudable mixture of
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`activated carbon, a ceramic forming material, a flux material, and water. (Ex. 1010
`
`at 2:22-28.) Park then dries and fires the monoliths. (Ex. 1010 at 2:28-32.)
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`Limited only by this broad disclosure, monoliths created according to Park could
`
`have a very wide range of adsorption capacities, and therefore [ACs. But even
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`limited to Park’s disclosed preferred embodiments, the range of potential [ACsis
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`great—andcertainly capable of exceeding 35 g/L.
`
`25.
`
`Park’s extrudable mixture includes activated carbon. (Ex. 1010 at
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`2:27.) This is the material that actually does the adsorbing in Park’s honeycombs.
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`Thus, the type of activated carbon used will have a great effect on IAC. The
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`adsorption capacity of different carbons can differ greatly depending ontheir
`
`source and howthey have been processed for activation. Park discloses that the
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`activated carbon in its honeycombs“may be madefrom a variety of precursors
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`including bituminouscoal, lignite, peat, synthetic polymers, petroleum pitch,
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`petroleum coke, coal tar pitch, and lignocellulosic materials. Suitable
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`lignocellulosic materials include wood, wood dust, wood flour, sawdust, coconut
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`shell, fruit pits, nut shell, and fruit stones.” (Ex. 1010 at 5:19-25.) Activated
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`carbons from different sources differ in their pore structures, including the number
`
`of pores, size of pores, and distribution of pore sizes. Such variation results in a
`
`wide range of adsorptive properties. Thus, as taught by the ’844 Patent, some
`
`11
`
`
`
`activated carbons can have naturally low IAC values (and flat adsorption
`
`isotherms), whereas others have high IAC values (and steep adsorption isotherms).
`
`(Ex. 1001 at 6:26-30, 7:56-58.) This wide range ofpotential sources for the
`
`activated carbon will provide a wide range of IACs for honeycombs made using
`
`the activated carbons.
`
`26. Additionally, the amount of activated carbon that goesinto the
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`extrudable mixture will have a great effect on the IAC of resulting honeycombs.
`
`The more carbon used,the greater the adsorption capacity—andthe greater the
`
`IAC,all other factors being equal. Park discloses that “activated carbon is
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`desirably present in the extrudable mixture in an amount from about 20 to about 70
`
`parts, by weight, and moredesirably, in an amount from about 30 to about 50 parts,
`
`by weight.” (Ex. 1010 at 4:64-67.) This range from 20 to 70 parts by weight
`
`represents a 250% increase in carbon content from the low endofthe rangeto the
`
`high end. This variation will havea large effect on the range of resulting
`
`adsorption capacities and IACsin Park’s honeycombs.
`
`27.
`
`Park discloses that various methods can be used to dry honeycomb
`
`monoliths in accordance with its invention, including vacuum drying,freeze
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`drying, humidity control drying, dielectric drying, and warm air drying with the
`
`monolith wrapped in plastic. (Ex. 1010 at 7:31-8:35.) Park further discloses that
`
`the selected drying method can affect the shape—and hence, volume—ofthe
`
`12
`
`
`
`resulting monolith. For example, freeze drying “immobilizes the water and
`
`stabilizes the size and shape of the monolith.” (Ex. 1010 at 7:51-53.) Thus, the
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`drying method selected for manufacture of the honeycomb canaffectits final
`
`shape and volume, and hence IAC,since IACis a volumetric measurement.
`
`28.
`
`Park discloses that, after drying, its honeycombsare fired at a high
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`temperature “from about 1600 to 1900° F.” (Ex. 1010 at 8:37-39.) The firing
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`temperature affects the apparent density of the honeycombduetoits effect on the
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`formation of ceramicstructures during firing. (Ex. 1010 at 10:45—48,Fig. 4.) This
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`will in turn affect IAC since IAC is a volumetric quantity dependent on apparent
`
`density, as the °844 Patent discloses. (Ex. 1001 at 9:33-42.) Thefiring
`
`temperature and time can also affect the adsorptive properties of the carbon in the
`
`monolith. In activated carbons, pores can be formed and/or enlarged at high
`
`temperatures, and these are the pores that act to adsorb compounds. Thus,asfiring
`
`temperatures and time increase, the adsorptive properties (including IAC) ofthe
`
`honeycombcan change.
`
`29. Other factors that will affect the adsorptive properties, including IAC,
`
`of a honeycombinclude the honeycomb’s cell density, or cells per square inch, and
`
`the cell wall thickness. These factors impact the carbon surface area available for
`
`adsorption, and hence affect the honeycomb’s adsorptive properties, including
`
`IAC. Park discloses a cell density ranging “from 1 to 800 cells per square inch or
`
`13
`
`
`
`higher;” and cell wall thickness ranging from “about 150 mils to about 5 mils” for
`
`honeycomb madeaccordingto its invention. (Ex. 1010 at 7:27-30.) With such
`
`broad ranges,it is clear that the range of adsorption capacities of resulting
`
`honeycombswill also be very broad.
`
`30.
`
`The honeycomb’s open frontal areais related to cell density and cell
`
`wall thickness in that the three properties compete for available spacein the cross-
`
`section of the honeycomb monolith. Thus, fixing any one ofthese three properties
`
`will affect the values that the other properties can take for a given honeycomb.
`
`Park describes “[t]he open frontal area of the monolith”as “the percentage of open
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`area of the monolith taken across a plane substantially perpendicular to the length
`
`of the monolith.” (Ex. 1010 at 7:18-20.) Park discloses that it prefers open frontal
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`areas for honeycombs madeaccordingto its invention of “greater than 70 percent
`
`and up to about 85 percent, and desirably about 73.8 percent.” (Ex. 1010 at 7:15-
`
`17.) Increasing the open frontal area of the monolith introduces open spaceto the
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`honeycomb,thus volumetrically diluting the activated carbon in the honeycomb
`
`and reducing its IAC, as taught by the °844 Patent. (Ex. 1001 at 6:24-27; 7:26—
`
`28.)
`
`31.
`
`Insum, Park discloses large variations in the types of honeycomb
`
`monoliths that can be created in accordance with its disclosures. Such large
`
`variations will result in large variationsin the adsorptive properties (including
`
`14
`
`
`
`IACs)of the resultant honeycombs. It is clear that at least some of Park’s
`
`honeycombsthat could result from invoking its disclosure would have IACs
`
`greater than 35 g/L.
`
`2.
`
`Petitioner’s Hypothetical Honeycomb Based on Park’s
`Formulation D Contradicts Park’s Disclosure
`
`32.
`
`Petitioner focuses on a particular honeycomb disclosed by Park—
`
`compositional Formulation D fired at 2000° F —and combinesit with other
`
`information to construct a hypothetical honeycombthat allegedly would
`
`necessarily have an IAC less than 35 g/L. (Petition at 39-41, 63-65; Ex. 1003 at
`
`qL09-111, 150.)
`
`33. AsI stated above, Park discloses that a broad array of honeycombs
`
`can be made accordingto its invention. Additionally, Park discloses four specific
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`recipes of ingredients (Formulations A—D) and fourfiring temperatures (1400,
`
`1600, and 1800, and 2000° F) for making honeycombs,as seen in Tables 1 and 2
`
`of Park. (Ex. 1010 at 9:18-10:10.)
`
`TABLE 1
`
`Formulation in parts by weight
`
`A
`
`50
`42
`8
`a
`~
`
`3
`83
`
`B
`
`50
`36
`7
`7
`4.5
`
`Cc
`
`30
`§8
`12
`
`nee
`
`3
`2
`
`28
`66
`
`D
`
`30
`50
`10
`10
`28
`
`25
`78
`
`Ingredient
`
`activated carbon!
`ball clay"
`calcined kaolin*
`nepheline syenite*
`sodiumsilicate®
`(solids from aqueous
`solution)
`methyl cellulose?
`water
`
`15
`
`
`
`TABLE 2
`
`Firing Temperature (° 6.)
`
`Formulation
`
`Sample 1
`Sample 2
`Sample 4
`Sample 3
`1600
`1400
`2000
`1800
`1400
`1600
`2000
`1800
`1400
`1600
`1800
`2000
`1400
`1800
`
`1600 2000
`
`ABcD
`
`34.
`
`Park doesnotstate that all these honeycomb formulations andfiring
`
`temperaturesfall within the scope of Park’s particular methodology for
`
`manufacturing honeycombs. Indeed, many of them do not. Rather, Park simply
`
`offers these formulations andfiring temperatures as experimentsto illustrate the
`
`effects of formulation andfiring temperature on axial strength and apparent density
`
`of the resulting honeycomb,asillustrated in Figures 3 and 4 of Park. (Ex. 1010 at
`
`10:12-54.)
`
`
`l
`
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`
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`
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`
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`
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`
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`
`100. 200~~300 500 G00, 700 800 0D 100D 1100S 1200-1295
`
`
`
`COMPRESSIVE STRENGTH,psi
`
`
`
`
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`‘\, FORMULATION A
`| i] FORMULATIONB
`|
`<¢> FORMULATION G
`(-) FORMULATION D
`
`
`
`
`
`16
`
`
`
`APPARENT DENSITY VERSUS TEMPERATURE
`
`
`
`0.4
`
`0.35
`
`0.3
`0.25
`
`APPARENT
`DENSITY
`(g/ml)
`
`1800
`FIG. 4 0 1600
`TEMPERATURE
`(deg. F)
`
`48-30% CARBON WITH FLUX
`
`Fi
`50% Wi0
`FO FLUX
`
`6
`
`35.
`
`The basis for Petitioner’s particular selection of Formulation D fired
`
`at 2000° F is Park’s disclosure about air intake adsorbents. In particular,
`
`Petitioner cites to Park’s statementthat “a monolithfor use as an automotive air
`
`intake VOC adsorption product demands a higher strength and a carbon content
`
`from about 25 to about 35%, by weight” and “[t]he axial crushing strengthfor an
`
`automotive air intake VOC adsorption product containing 25% carbon, by weight,
`
`ranges from 1200 to 1600 psi.” (Petition at 33; Ex. 1003 at 4105; Ex. 1010 at 9:4—
`
`14.) According to Petitioner, of the four compositional formulations (AD) and
`
`four firing temperatures (1400, 1600, and 1800, and 2000° F) that Park discloses
`
`here, only Formulation D fired at 2000° F meets both the carbon content and the
`
`axial strength criteria. (Petition at 33-35; Ex. 1003 at 4105.) Thus, accordingto
`
`Petitioner, a person ofskill in the art would have selected Park’s Formulation D
`
`fired at 2000° F as the best candidate for combination with Meiller or Abe.
`
`36. According to Park’s Figure 4, Formulation D fired at 2000° F resulted
`
`in a honeycomb with an apparent density of about 0.35 g/mL. (Ex. 1010 at 10:39-
`
`17
`
`
`
`54.) Thus, Petitioner proposesthat its hypothetical honeycomb made using Park’s
`
`Formulation D fired at 2000° F would have the same apparent density. (Petition at
`
`35, Ex. 1003 at 9105.)
`
`37.
`
`Park further discloses that its Formulation D was made into
`
`honeycombs with 200 cells per square inch. (Ex. 1010 at 10:11-15.) Thus,
`
`Petitioner proposesthat its hypothetical honeycomb would have had the same 200
`
`cpsi. (Petition at 36; Ex. 1003 at 4105.)
`
`38.
`
`Park also discloses that honeycombs madeaccordingto its invention
`
`preferably have an open frontal area between 70% and 85%, and more desirably an
`
`open frontal area of 73.8% in particular. (Ex. 1010 at 7:15-18.) Park does not
`
`disclose the open frontal area of the Formulation D honeycombs, however.
`
`Nevertheless, Petitioner proposes that its honeycomb based on Formulation D
`
`could be made with an open frontal area of 73.8%. (Petition at 36; Ex. 1003 at
`
`4105.)
`
`39.
`
`Finally, Park’s Formulation D doesnot identify the specific activated
`
`carbon used therein. Park only discloses the following:
`
`18
`
`
`
`TABLE 1
`
`Formulation in paris by weight
`
`Ingredient
`activated varboa!
`hall clay?
`caicined kaolin*
`nepheline syenite*
`sodiumsilicate"
`(solids from aqueous
`solution}
`methyl cellulose®
`water
`
`A
`50
`2
`8
`—
`~_
`
`3
`83
`
`B
`$0
`36
`?
`7
`4,8
`
`3
`102
`
`C
`3t)
`58
`12
`_
`—
`
`7
`66
`
`D
`30
`50)
`10
`10
`28
`
`a
`73
`
`
`
`To supplement Park’s disclosure here, Petitioner suggests that the activated carbon
`
`could have been BAX 1100 or BAX 1500. (Petition at 39-40; Ex. 1003 at 4110.)
`
`I note that none of Park, Meiller, and Abe disclose BAX 1100 or BAX 1500. (Exs.
`
`1010, 1016, 1009.)
`
`40.
`
`Insum,accordingto the Petitioner, the resulting hypothetical
`
`honeycomb achieved by combining Formulation D,a firing temperature of 2000°
`
`F, an open frontal area of 73.8%, and BAX 1100 or BAX 1500 would havethe
`
`following properties:
`
`
`
`
`|
`Property
`| Petitioner’s hypothetical honeycomb
`
`Cell density
`| 200 cpsi
`
`% vol voidages _| 73.8%
`| Carbon content
`—_| 30 parts of BAX 1100 or BAX 1500
`
`Ceramic material|60 parts
`
`
`Flux material
`12.8 parts
`Water
`75 parts
`Apparent density|approx. 0.35 g/mL
`
`
`
`
`
`41.
`
`Park, however, does not support—and indeed teaches away from—
`
`such a honeycomb.
`
`19
`
`
`
`a.
`
`Park Does Not Disclose Any HoneycombSpecific To
`Evaporative Emissions Control Systems
`
`42.
`
`Theentire basis of the Petitioner’s hypothetical honeycombis faulty
`
`because Park’s criteria that Petitioner uses to select Formulation D fired at 2000° F
`
`are intended for honeycombsused as scrubbers in emissions control systemsfor
`
`automotive air intake systems (AIS), not in evaporative emissions control systems
`
`for automotive fuel tanks (i.e. fuel vapor canisters). AIS emissions control systems
`
`are very different from fuel vapor canisters. This is illustrated by the fact that the
`
`automotive industry does not use fuel vapor canisters to capture AIS emissions.
`
`And because these applications are very different, a POSITAat the time ofthe
`
`"844 Patent would not have been guidedbycriteria specific to AIS to instead select
`
`a honeycombfor a fuel vapor canister application.
`
`43.
`
`One way in which AIS emissions control systems and fuel vapor
`
`canisters are different is in the make-up of vapors to be adsorbed. With regards to
`
`the fuel vapor canister application, the head space of the automobile fuel tank is
`
`filled with a mixture of air and fuel vapors. For gasoline tanks, this mixture is
`
`about a 50:50 ratio of air to fuel. (Fuel vapor canisters are used with gasoline
`
`powered automobiles, not diesel automobiles.) In comparison, the air-fuel ratio in
`
`gasoline engines is around 12:1 to 15:1.! Thatis, the air-fuel mixture is much
`
`FE.g.,
`
` https://haynes.com/en-us/tips-tutorials/what-afr-or-airfuel-ratio-your-
`
`20
`
`|
`
`
`
`richer in the head space above gasoline tanks than in the engineitself.
`
`Accordingly, fuel vapor canisters must adsorb a much moreconcentrated source of
`
`hydrocarbonsvapors than do AIS emissions control systems.
`
`44. Another way in which AIS emissions control systems and fuel vapor
`
`canisters differ is in the flow rate of vapors to be adsorbed. In the case of AIS
`
`emissions control systems, vapors flow from the engine and need to be captured
`
`only whenthe engineis not operating. In this scenario, there is no physical driving
`
`force pushing vapors from the engine throughthe air intake system, and the flow
`
`rate of vapors to be captured is slow. In comparison, fuel vapor canisters must be
`
`equippedto handle the high flow rate of vapors during refueling, in which an entire
`
`fuel tank’s volume of vapors may be expelled in about a minute. Thus, fuel vapor
`
`canisters must adsorb vapors at a much higher flow rate than AIS emissions control
`
`systems.
`
`45.
`
`A further way in which AIS emissions control systems and fuel vapor
`
`canisters differ is in the flow rate of purge air. Purgeair is used to desorb captured
`
`hydrocarbons from the adsorbent and transport the desorbed hydrocarbonsto the
`
`engine for combustion when the engineis operating. In this way, the adsorbentis
`
`regenerated during engine operation so that more fumes can be adsorbed during the
`
`next cycle of non-operation. In the case of AIS emissions control systems, the
`
`flow of purgeair is very high because the AIS is the source of combustion air for
`
`21
`
`
`
`the engine. But in the case of fuel vapor canisters, the flow of purgeair is much
`
`lower. Purge air flow to fuel vapor canisters is restricted becausethe resulting
`
`air/fuel mixture flowing from the canister to the engine can upsetthe air/fuel
`
`balance in the engine, leading to incomplete combustion and increased tailpipe
`
`emissions.
`
`46.
`
`In view ofthe foregoing differences, a POSITAatthe time of the 844
`
`Patent would not have considered a honeycombfor use in AIS emissionscontrol
`
`systems to be applicable to evaporative emissions control systems (fuel vapor
`
`canisters). Thus, the disclosures of Meiller and Abe concerning evaporative
`
`emissions control systems would not have led a POSITAto the AIS embodiments
`
`in Park, or any other particular embodiments in Park for that matter, because Park
`
`does not disclose any embodiments specific to the unique context of evaporative
`
`emissions control systems.
`
`b.
`
`Park Teaches Away from a Firing Temperature of
`2000° F
`
`47.
`
`Tl also disagree with the basis ofthe Petitioner’s hypothetical
`
`honeycomb because Park teaches away from firing at 2000° F, as Petitioner
`
`proposesfor its honeycomb.
`
`48. As I explained above, Petitioner selects Formulation D fired at 2000°
`
`F becauseit is the only one ofthe sixteen formulation/firing temperature examples
`
`in Park that is reported as having a carbon content of 30% and an axial crushing
`
`22
`
`
`
`strength from 1200 to 1600 psi. (Petition at 33-35; Ex. 1003 at 4105; Ex. 1010 at
`
`9:10-14.)
`
`49.
`
`Elsewhere, however, Park teaches away from usingthis firing
`
`temperature. In its Background of the Invention, Park refers to a patentto
`
`Okabayashi, which Park characterizes as disclosing activated carbon/ceramic
`
`monoliths fired at temperatures of 1100° C (i.e., 2012° F). (Ex. 1010 at 1:36-43.)
`
`Park explicitly criticizes “[fliring at such higher temperatures” as “economically
`
`undesirable.” (Ex. 1010 at 1:36—43.) Park then identifies “a need for a formed
`
`body comprising activated carbon that can be ... fired at more economical
`
`conditions such as a lower temperature.” (Ex. 1010 at 1:65-2:4.) Park accordingly
`
`discloses that the honeycombofits invention “is fired at a temperature from about
`
`1600 to about 1900° F and desirably from about 1850 to about 1900° F.” (Ex.
`
`1010 at 8:36-39.)
`
`50.
`
`Park clearly taught away from the 2000° F firing temperature that
`
`Petitioner uses for its hypothetical honeycomb, which providesthe apparent
`
`density of 0.35 g/mL that Petitioner relies upon in seeking to deduce the IACofits
`
`honeycomb,as I discuss further below.
`
`Cc.
`
`The Apparent Density, Voidage Percentage, and
`Composition of Petitioner’s Hypothetical Honeycomb
`May Not Be Compatible
`
`23
`
`
`
`51.
`
`Furthermore, I disagree with the feasibility of Petitioner’s
`
`hypothetical honeycomb because the composition of Formulation D fired at 2000°
`
`F yielding an apparent density of about 0.35 g/mL may not be compatible with
`
`Petitioner’s proposed 73.8% open frontal area for its hypothetical honeycomb.
`
`52.
`
`The apparent density of a honeycombsuchas those disclosed by Park
`
`is a function ofits total mass and volumeof the space occupied by the honeycomb,
`
`including any voidages. (Contrast this to the honeycomb’s displacement volume,
`
`which would excludeits voidage space and be used to measure the honeycomb’s
`
`actual density.) The honeycomb’s mass,in turn, is a function of its composition.
`
`The honeycomb’s volume(for purposes of apparent density), is a function ofits
`
`voidage fraction, which Petitioner equates to the honeycomb’s openfrontal area.
`
`(Petition at 36; Ex. 1003 at 4105.) Thus, selecting the honeycomb’s composition
`
`and open frontal area will fix its apparent density. In other words, there are two
`
`degrees of freedom in this scenario, so that selecting any two properties will dictate
`
`the third property.
`
`53.
`
`In the case of Petitioner’s hypothetical honeycomb,selecting the
`
`composition (Formulation D) and openfrontal area (73.8%) will dictate the
`
`resulting density. Nowhere does Park disclose that Formulation D, if emplo
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