UNITED STATES PATENT AND TRADEMARK OFFICE
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`
`UMICORE AG &CO KG,
`Petitioner
`
`v.
`
`BASF CORPORATION,
`Patent Owner
`
`Case IPR. Nos. 2016-00610, 2016-00612, 2006-00613
`U.S. Patent Nos. 8,899,023; 9,032,709; 9,039,982
`
`DECLARATION OF AHMAD MOINI IN SUPPORT OF
`PATENT OWNER'S PRELIMINARY RESPONSE TO PETITIONS FOR
`INTER PARTES REVIEW OF U.S. PATENT NOS. 8,899,023; 9,032,709;
`AND 9,039,982
`
`BASF-2017.001
`
`
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`
`UMICORE AG &CO KG,
`Petitioner
`
`v.
`
`BASF CORPORATION,
`Patent Owner
`
`Case IPR. Nos. 2016-00610, 2016-00612, 2006-00613
`U.S. Patent Nos. 8,899,023; 9,032,709; 9,039,982
`
`DECLARATION OF AHMAD MOINI IN SUPPORT OF
`PATENT OWNER'S PRELIMINARY RESPONSE TO PETITIONS FOR
`INTER PARTES REVIEW OF U.S. PATENT NOS. 8,899,023; 9,032,709;
`AND 9,039,982
`
`BASF-2017.001
`
`
`
`Ex. 2017 ("MoiniDecl")
`
`I, Dr. Ahmad Moini, hereby declare as follows:
`
`I. INTRODUCTION
`
`1. My name is Ahmad Moini. I make this declaration in connection with
`
`the above-captioned Petitions for Inter Partes Review (collectively, "the Petitions")
`
`of U.S. Patent Nos. 8,899,023 ("the '023 patent); 9032,709 ("the '709 patent); and
`
`9,039,982 ("the '982 patent) (collectively, "the BASF patents").
`
`2.(cid:9)I am a Senior Expert and Research Fellow at BASF Corporation. I
`
`received a B.Sc. in Chemistry from Eastern Washington University in 1982 and a
`
`Ph.D. in Chemistry from Texas A&M University in 1986. I have been employed by
`
`BASF Corporation (previously Engelhard Corporation) as a scientist for 20 years. I
`
`have been involved with diesel exhaust catalysts for the past 12 years. I am a named
`
`inventor on 48 granted US patents, some of which relate to zeolites for diesel exhaust
`
`applications.
`
`3.(cid:9)I understand that the Petitions rely upon expert witness testimony from
`
`Dr. Magdi Khair, who opines that the Japanese Patent Application Publication Hl-
`
`151706 to Muraki ("Muraki") discloses washcoat loadings that meet the ranges
`
`claimed in the BASF patents. I have reviewed an English translation of Muraki and
`
`Dr. Khair's calculations carefully, and I believe there are numerous errors in his
`
`calculations.
`
`V.
`: •$'
`
`1
`
`BASF-2017.002
`
`
`
`Ex. 2017 ("Moini Decl.")
`
`4.(cid:9)Dr. Khair's calculations are set forth in ^ 141-52 of his declaration in
`
`IPR2016-00612, which pertains to the '709 patent. He submits nearly identical
`
`calculations in IPR Nos. 2016-00610 and IPR 2006-00613. For simplicity my
`
`references and citations to Dr. Khair's declaration shall be to Dr. Khair's declaration
`
`in IPR2016-00612.
`
`5.(cid:9)Dr. Khair asserts in Tf 142 of his declaration that Muraki includes
`
`information from which the "preferred loading levels can be estimated." Dr. Khair
`
`relies upon three pieces of information from Muraki:
`
`•(cid:9)Muraki' s statement that his zeolites have a silicon to aluminum ratio
`
`that is greater than 1. Ex. 1009 If 145. Dr. Khair states that "[s]ince
`
`the molecular formulas of alumina and silica are respectively AI2O3
`
`and SiOz, by requiring a Si:Al atomic ratio of at least 1, Muraki is
`
`calling for zeolites with a silica to alumina ratio (or £SAR') of at
`
`least 2." Id.
`
`•(cid:9)Muraki's use of 20g/L of ion-exchanged copper in his examples. Id.
`
`1(147.
`
`•(cid:9)Muraki's use of an 89% ion exchange rate in his examples. Id.
`
`6.(cid:9)Dr. Khair does not identify the exact value of the SAR of the zeolite
`
`that is used in Muraki. Dr. Khair states that as "of the '709 patent's filing date, it
`
`was known that aluminosilicate zeolites with a SAR in excess of 10 could be
`
`beneficially used in an exhaust gas treatment system." Id. ^ 146. Based on this, and
`
`BASF-2017.003
`
`
`
`Ex. 2017 ("Moini Decl")
`
`his earlier conclusion that Muraki requires a SAR of at least 2, Dr. Khair performs
`
`calculations using SARs of 2, 10, and 15.
`
`7.(cid:9)Dr. Khair's calculations are used to determine the g/in3 of catalyst
`
`loading based on the g/L of copper that is loaded onto the filter. Dr. Khair's
`
`calculations start by converting 20 g/L of Cu+ to mol/L of Cu+. See, e.g., Ex. 1009
`
`1149 (first bullet). There is no mathematical error in this preliminary step.
`
`8.(cid:9)Next, Dr. Khair computes the g/L of zeolite that is present. This
`
`requires computing both the amount of AI2O3 and the amount of Si02 that is present.
`
`9.(cid:9)For the AI2O3, Dr. Khair reasons that for every 2 moles of Cu+ there
`
`must be one mole of AI2O3 so that the charges all balance. Thus, the mol/L of Cu+
`
`should be divided by 2 to determine the mol/L of AI2O3 that is necessarily present to
`
`balance the charge on the CuV To get the total AI2O3, however, one must take into
`
`account the ion exchange rate, which is the fraction of zeolite that includes a Cu+
`
`1 While there is no error in Dr. Khair's mathematics in this calculation, I note that
`
`Dr. Khair's use of the +1 oxidation state of copper is unjustified. One of skill in the
`
`art would have understood that the +2 oxidation state of copper is far more common
`
`than the +1 oxidation state and would have used this oxidation state rather than the
`
`+1 oxidation state. For simplicity, I will proceed as if the +1 oxidation state of
`
`copper is appropriate.
`
`BASF-2017.004
`
`
`
`Ex. 2017 ("Moini Decl")
`
`ion. Only 89% of the zeolite includes a Cu+ ion. Therefore, to get the total amount
`
`of zeolite, one must further divide by the ion-exchange rate. Dr. Khair, however,
`
`multiplies by the ion-exchange rate. See Ex. 1009 ^ 149 (second bullet). This is Dr.
`
`Khair's first error, and it leads to an underestimation of the amount of catalyst
`
`loading that is used in Muraki. It should be noted that, if the total Cu content does
`
`not fully satisfy the exchange capacity of the zeolite (e.g. 89% exchange), the
`
`remaining exchange sites would be occupied by other types of cations, e.g. H+ of
`
`Na+. This has a minor contribution to the overall mass of the final catalyst, and has
`
`been ignored by Dr. Khair, and in our calculations.
`
`10.(cid:9)Once the moles of AI2O3 have been determined, the moles of Si02 can
`
`be computed simply by multiplying by the SAR. See id. K 149 (second bullet,
`
`multiplying the Si02 by 2 for the calculation using a SAR of 2); id. If 150 (second
`
`bullet, multiplying the Si02 by 10 for the calculation using a SAR of 10); id. If 151
`
`(second bullet, multiplying the Si02 by 15 for the calculation using a SAR of 15).
`
`Once both the mol/L of AI2O3 and mol/L of Si02 are determined, Dr. Khair computes
`
`the g/L of each component by using each component's molecular weight. See id.
`
`There is no error in this calculation.
`
`11.(cid:9)Finally, Dr. Khair computes the total amount of catalyst loading by
`
`adding together (1) the g/L of AI2O3, (2) the g/L of Si02, and (3) the g/L of Cu+. See,
`
`e.g., id. If 149 (third bullet). Here, Dr. Khair makes another significant error.
`
`-4-
`
`BASF-2017.005
`
`
`
`Ex. 2017 ("Moini Decl.")
`
`Specifically, Dr. Khair neglects to take into account the fraction of the washcoat
`
`loading in Muraki that consists of non-zeolite components, such as a binder. As
`
`Muraki states, "100 parts of zeolite powder having a particle size of 20 jim and 80
`
`parts of silica sol were ball-milled together...Ex. 1003 at 12:2-6. In other words,
`
`the washcoat in Muraki actually consists of five parts catalyst and four parts silica
`
`sol. Therefore, once one knows the g/L of catalyst that is present, one must multiple
`
`this number by 0.8 and add the resulting number to the g/L of catalyst to get the total
`
`washcoat loading. This takes into account both the binder and the catalyst. Dr.
`
`Khair neglects this step entirely. Because of this error, Dr. Khair again
`
`underestimates the amount of catalyst loading used in Muraki.
`
`12. Yet another error by Dr. Khair pertains to the SAR values he selects.
`
`Dr. Khair carries out calculations using SAR values of 2, 10, and 15. See Ex. 1009
`
`fTf 149-51. These are arbitrary SAR values selected by Dr. Khair, ostensibly so that
`
`he covers a range of different SARs. However, Example 3 of Muraki provides
`
`sufficient information to compute the SAR actually used in Muraki such that there
`
`is no need to guess. Specifically, in Example 3, Muraki uses a 1.3 L filter with 200
`
`g of zeolite {i.e., about 154 g/L of zeolite). See Ex. 1003 at 16:17-18, 16:26-28.
`
`Muraki further states that there is lOg/L of Cu+ and an ion-exchange rate of 93%.
`
`For all of these conditions to be satisfied, the SAR must be roughly 28.6, as shown
`
`in the following set of calculations:
`
`BASF-2017.006
`
`
`
`Ex. 2017 ("Moini Decl.")
`
`/10g Cu(I)\ (Imole Cu(0\ _ 0.157moles C-u(J)
`V(cid:9)L filter ) \63.55 g Cu(f)/ " L filter
`
`/0.157 mole Cu(/)\ /(cid:9)^ /1 mole A1203\ /101.96 g A1203\ _
`V(cid:9)L filter ) V0.93 mole CuQ)) V 2molcAl J V Imolc A1203 )
`
`8.61 g Al203(zeolite)
`L filter
`
`154 g zeolite 8.61 g Al203(zeolite) _ 145 g Si02 (zeolite)
`L filter L filter(cid:9)L filter
`
`fQ.ei g A1203\ / imole A1203 \ _ 0.0844 moles A1203
`V(cid:9)L filter ) \101.96 g A1203)(cid:9)L filter
`
`/145 g(cid:9)/Imole Si02\ _ 2Almoles Si02
`filter J \60.08 g-SiOlJ(cid:9)L filter
`V(cid:9)L filter J \60.08 g-Sim)
`
`SAR =
`
`2.41 moles Si02 28.6 moles Si02
`0.0844 moles A1203 mole A1203
`
`13. Applying a SAR of 28.6 (instead of SARs of 2,10, and 15) to Muraki's
`
`other examples (and then carrying out the calculations without Dr. Khair's errors),
`
`one obtains far different results from those obtained by Dr. Khair. The following is
`
`the calculation based on the parameters set forth in Example 1 of Muraki:
`
`/20g Cu(J)\ (Imole Cu(I)\ _ 0.315 moles CuQ)
`V L filter J \63.55g-Qttg})(cid:9)L filter
`
`f 0.315 mole Cu(I)\ ( 1 mole Al \ f Imole A1203\ /101.96 g A1203\ _
`# V L filter ) \0.89 molo Cu(T)) \ 2molcAl ) \ Imole A1203 J
`
`18.0 g Al203(zeolite)
`L filter
`
`f 0.315 mole Cu(I)\ ( Imole Al \ f Imole A1203\ (28.6 mole Si02\ (60.08 gSi02\ _
`9 V L filter ) \.0.89 molo Cu(I)) V 2moleAl ) V Imole A1203 ) \lmolc Si02)
`
`304 g Si02 (zeolite)
`L filter
`
`BASF-2017.007
`
`
`
`Ex. 2017 ("Moini Decl")
`
`18.0 g Al203(zeolite) 304 g Si02 {zeolite) _ 322 g zeolite
`L filter(cid:9)L filter(cid:9)L filter
`
`322 g zeolite 20 g Cu(f) _ 342 g Cu-zeolite
`L filter(cid:9)L filter(cid:9)L filter
`
`f342 g Cu-zeolite\ f L filter \ _ 5.60 g Cu-zeolite
`\ L filter ) \6l.024cu.in. filter J cu.in.f ilter
`
`To take into account that the washcoat slurry contains 100 parts zeolite powder
`
`(prior to the addition of Cu+) plus 80 parts other solid inorganic components,
`
`one carries out the following calculations:
`
`/322 g zcolitc\ /80 g other components\ _ 258 g other components
`V L filter ) V 100 g zeolite J(cid:9)L filter
`
`322 g zeolite 20 g Cu(/) 258 g other components _ 600 g total washcoat
`L filter(cid:9)L filter(cid:9)L filter(cid:9)L filter
`
`/ L filter \ _
`/600 g total washcoat\ ( L filter \ _ 9.83 g total washcoat
`/ V61.024 cu.in.f ilter J\(cid:9)i filter(cid:9)) V61.024 cu.in.f ilter/(cid:9)cu.in.f ilter
`
`
`14. The resulting washcoat loading of 9.83 g/in3 is roughly four times
`
`greater than the value of 2.63 g/in3 that Dr. Khair calculated using a SAR of 15, which
`
`is the largest SAR he considered. The calculations for Example 2 are identical to
`
`those for Example 1, except that the ion-exchange ratio is 90%. This leads to a
`
`washcoat loading of 9.73 g/in3. Using the parameters in Example 3 and a SAR of
`
`28.6, the washcoat loading in Muraki is calculated to be 4.70 g/in3.
`
`II. AVAILABILITY FOR CROSS-EXAMINATION
`
`15. I realize that this signed declaration will be filed as evidence in a
`
`contested case before the Patent Trial and Appeal Board of the United States Patent
`
`-7-
`
`BASF-2017.008
`
`
`
`Ex. 2017 ("Moini Decl")
`
`and Trademark Office. I also realize that I may be subject to cross examination in
`
`the case within the United States. If such cross examination is required, I will appear
`
`for cross examination within the United States during the time allotted.
`
`III. JURAT
`
`16.(cid:9)I declare that all statements made herein of my own knowledge are true
`
`and that all statements made on information and belief are believed to be true; and
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`further that these statements were made with the knowledge that willful false
`
`statements and the like so made are punishable by fine or imprisonment, or both,
`
`under Section 1001 of Title 18 of the United States Code.
`
`17.(cid:9)I declare under penalty of perjury that the foregoing is true and correct.
`
`Executed on May 31,2016
`
`Dr. Ahmad Moini
`
`-8-
`
`BASF-2017.009
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