Inter Partes Reexamination No. 95/001 ,453
`Declaration of A.hmad Moini, Ph,D,
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`IN THE UNITED STATES PATENT AND TRADEMARK OFFICE
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`Examiner: DIAMOND, ALAN D
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`Group Art lfnjt: 3991
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`Confinnation No: 2755
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`In Inter Partes Reexa1nination of:
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`BULLET AL.
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`Reexamination Control No. 95/001,453
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`PatentNo, 7,601,662
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`Issued: October 13, 2009
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`For: COPPER CHA
`ZEOLITE CATALYSTS
`Mail Stop Inter Partes Reexa:m
`Central Reexamination Unit
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
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`DECLARATION OF AHMAD MOINI. PH.D.~ UNDER 37 C.KR. § 1.132
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`1, Ahmad Moini, do declare and say as follows:
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`1. I am a Senior Research Associate for BASF Corporation, the successor in interest to
`Engelhard Corporation and BASF Catalysts LLC (BASF), the mvner of United States patent number
`7,601,662 (11the '662 patent'} I received a RS. in Chemistry from Eastern Washington University in
`1982 and a Ph.D. in Chemistry from Texas A&M University in 1986. I have been a scientist at
`BASF Corporation. I am a co-inventor of the subject matter described and claimed in the 1662
`patent
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`l have been involved in heterogeneous catalyst research fi.1r rnore than 20 years. first as a
`2,
`researcher at Mobjl Research and Development Corporation, and later at BASF Corporation. I am a
`nmned inventor on 30 granted United States patents, some of which pertain to zeolites for use as
`automotive catalysts.
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`3. As part of the research team that discovered the copper chabazite catalysts of the '662 patent,
`we were tasked with the challenge to provide a material for selective catal)iic reduction that would
`have tv,ro main properties: (1) excellent NOx conversion over a 1.:vide ten1perature range, including
`the low temperature range of 200° C to 350° C; and (2) hydrothennal stability-meaning that the
`NOx conversion would not degrade significantly upon hydrothermal ag1ng at temperatm·es in excess
`of 650° C. Befr)re begjnning research, I initially believed that a metal promoted zeolite v.rou1d not
`have both of these properties. Prior to the invention of the subject matter of the '662 patent, it was
`believed that Fe zeolites had better hydxothermal stability than Cu zeolites.
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`4. Our initial studies included a sn1al1 scale rapid screening test that we d(wdoped and used to
`initially scre~~n over 900 zeolite materials indud1ng over twelve different structure types, different
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`Exhibit 2003.001
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`Inter Partes Reexamination No, 95/001 ,453
`Declaration of Ahrnad Moini, Ph.D.
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`silica to alumina ratios, different meta! ions, and different metal ion/aluminum ratios. After initial
`studies were completed, selected samples were screened further on the basis ofNOx conversion, low
`degradation ofNOx conversion after hydrothermal aging at 800° C in l 0% H20, and low generation
`ofN20. The materials claimed in the t662 patent emerged as the lead rnaterial, and we fi.mnd that
`zeo1Hes having the CH.A structure type and a sifa~a to aJumina ratio greater than 15 and \'.~opper to
`aluminum ratios exceeding 0.25 mei. the requirements stated above. I believe the properties of these
`materials were highly unexpected.
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`5. It is my understanding that the invention is not limited to zeolites containing free or non(cid:173)
`exchanged copper. Examples l, lA, 2, 3, 4, 6, 7, 8, 9, 16, 17 and 18 all show the unexpected results
`achieved by zeolites that have the CHA structure type and silica to alumina ratio greater than 15 and
`copper to aluminum ratio exceeding 0.25. The properties of the exarnples tested were quite
`unexpected in that the literature had reported that Cu zeolites exhibited poor hydrothermal stability.
`Then.~ had been a longstanding need for a metal promoted zeolite that exhibited both low
`temperature conversion in the range of 200° to 350° C and hydrothermal stability. The Examples in
`the '662 patent include various copper loadings, variations in ion exchange techniques (e.g.,
`concentration of exchange solution, temperature, time, munher of exchanges, exchange
`prior/during/after fonnation/appHcation of slurry, etc). A person of ordinary skill in the art wiU
`readily understand that these variations vv1.11 affect NOx conversion. Aside from th(~se variations in
`preparation, the Examples shmv that when additional steps were taken beyond a traditional ion
`excfo.=mge, enhanced NOx conversion was obtained. Cornparing Examples 1A and I, it is believed
`that the level of NOx conversion for Example IA \Vas higher than Example I for the aged samples;
`because Example IA included the addition of copper to the coating slurry after traditional ion
`~~xchange to provide additional copper. Example 3, which involved. traditional ion exchange plus
`impregnation also showed enhanced NOx conversion performance for aged samples compared to
`other aged samples.
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`6. Example 18 shows the effoc:t of using different ion exchange conditions (e.g., copper acetate
`versus copper sulfate) on the perforrmmce of the catalyst. ln Example 18, a relatively high
`concentration of copper acetate was used and the ion exchange \Vas conducted at 70'' C for one hour.
`Example 18 is a unique preparation.
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`7. A person of ordinary skill in the rut could determine the presence of free or non--exchanged
`copper in each Example of the '662 patent from available techniques such as X-ra.Y Ahsmvfam Near(cid:173)
`Edgc Structure spectroscopy.
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`I hereby declare that all statements made herein of my ow11 kno>vvledge are tme and that an
`statements made herein on information and belief are believed to be true; and further that these
`statements were made with the knowledge that wlllful 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, and that such willful false statements may jeopardize the validity of the above-identified
`patent
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`Dated: February 9, 2011
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`RespecHhlly submitted,
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`Ahrnad Moini, Ph.D.
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`By:
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`Exhibit 2003.002