`
`____________________
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`
`____________________
`
`APPLIED MATERIALS, INC.
`Petitioners
`
`v.
`
`DEMARAY LLC
`Patent Owner
`
`____________________
`
`Patent No. 7,381,657
`____________________
`
`DECLARATION OF DR. VIVEK SUBRAMANIAN
`IN SUPPORT OF PETITION FOR INTER PARTES REVIEW
`OF U.S. PATENT NO. 7,381,657
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`Page 1 of 122
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`APPLIED MATERIALS EXHIBIT 1002
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`
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`Declaration of Dr. Vivek Subramanian
`U.S. Patent No. 7,381,657
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`
`TABLE OF CONTENTS
`
`INTRODUCTION .......................................................................................... 1
`
`BACKGROUND AND QUALIFICATIONS ................................................ 2
`
`I.
`
`II.
`
`III. MATERIALS REVIEWED ........................................................................... 6
`
`IV. PERSON OF ORDINARY SKILL IN THE ART AND THE TIME
`OF THE ALLEGED INVENTION .............................................................. 11
`
`V.
`
`TECHNICAL BACKGROUND .................................................................. 13
`
`A.
`
`B.
`
`C.
`
`D.
`
`Sputter Deposition .............................................................................. 13
`
`Reactive Sputter Deposition ............................................................... 16
`
`Power Supplies Used for Reactive Sputtering ................................... 17
`
`Filter(s) ............................................................................................... 21
`
`VI. THE ’657 PATENT ...................................................................................... 31
`
`A. Description ......................................................................................... 31
`
`VII. OVERVIEW OF THE PRIOR ART ............................................................ 33
`
`A.
`
`B.
`
`Licata .................................................................................................. 33
`
`Collins................................................................................................. 34
`
`VIII. CLAIM CONSTRUCTION ......................................................................... 37
`
`IX. THE PRIOR ART DISCLOSES OR SUGGESTS ALL RECITED
`FEATURES OF CLAIMS 1-8 and 10-17 OF THE ’657 PATENT ............ 38
`
`A.
`
`Licata in view of Kelly and Collins Discloses and/or Suggests
`the Limitations of Claims 1-4, 6, 8, 10, 11, and 12 ............................ 38
`
`1.
`
`Claim 1 ..................................................................................... 38
`
`a)
`
`b)
`
`Claim 1[a] “A method of depositing a film on an
`insulating substrate, comprising:” ................................. 38
`
`Claim 1[b] “providing a process gas between a
`conductive target and the substrate;” ............................. 46
`
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`U.S. Patent No. 7,381,657
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`c)
`
`Claim 1[c] “providing pulsed DC power to the
`target through a narrow band rejection filter such
`that the target alternates between positive and
`negative voltages;”......................................................... 48
`
`(1) Claim 1[c](1) “providing pulsed DC power
`to the target…such that the target alternates
`between positive and negative voltages;” ........... 48
`
`(2) Claim 1[c](2) [providing pulsed DC power
`to the target] “through a narrow band
`rejection
`filter”
`[such
`that
`the
`target
`alternates between positive and negative
`voltages] .............................................................. 62
`
`Claim 1[d] “providing an RF bias at a frequency
`that corresponds to the narrow band rejection filter
`to the substrate;” ............................................................ 70
`
`Claim 1[e] “providing a magnetic field to the
`target; and” ..................................................................... 71
`
`Claim 1[f] “reconditioning the target; wherein
`reconditioning
`the
`target
`includes
`reactive
`sputtering in the metallic mode and then reactive
`sputtering in the poison mode.” ..................................... 71
`
`d)
`
`e)
`
`f)
`
`2.
`
`Claim 2 ..................................................................................... 76
`
`a)
`
`b)
`
`c)
`
`d)
`
`Claim 2[a] “A method of depositing an insulating
`film on a substrate, comprising:” ................................... 76
`
`Claim 2[b] “providing a process gas between a
`target and a substrate;” .................................................. 78
`
`Claim 2[c] “providing pulsed DC power to the
`target through a narrow band rejection filter such
`that the voltage on the target alternates between
`positive and negative voltages;” .................................... 80
`
`Claim 2[d] “providing an RF bias that corresponds
`to the narrow band rejection filter to the substrate;
`and” ................................................................................ 80
`
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`U.S. Patent No. 7,381,657
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`e)
`
`f)
`
`Claim 2[e] “providing a magnetic field to the
`target;” ........................................................................... 81
`
`Claim 2[f] “wherein an oxide material is deposited
`on the substrate, and the insulating film is formed
`by reactive sputtering in a mode between a
`metallic mode and a poison mode.” .............................. 81
`
`3.
`
`Claim 3 ..................................................................................... 88
`
`a)
`
`“The method of claim 2 wherein the target is a
`metallic target and the process gas includes
`oxygen.” ......................................................................... 88
`
`4.
`
`Claim 4 ..................................................................................... 90
`
`a)
`
`“The method of claim 2 wherein the target is a
`metallic target and the process gas includes one or
`more of a set consisting of N2, NH3, CO, NO, CO2,
`halide containing gasses.” .............................................. 90
`
`5.
`
`Claim 6 ..................................................................................... 92
`
`a)
`
`“The method of claim 2 wherein the magnetic field
`is provided by a moving magnetron.” ........................... 92
`
`6.
`
`Claim 8 ..................................................................................... 93
`
`a)
`
`“The method of claim 2 wherein the process gas
`includes a mixture of Oxygen and Argon.” ................... 93
`
`7.
`
`Claim 10 ................................................................................... 93
`
`a)
`
`“The method of claim 2 wherein the process gas
`further includes nitrogen.” ............................................. 94
`
`8.
`
`Claim 11 ................................................................................... 94
`
`a)
`
`“The method of claim 2 wherein providing pulsed
`DC power to a target includes providing pulsed
`DC power to a target which has an area larger than
`that of the substrate.” ..................................................... 95
`
`9.
`
`Claim 12 ................................................................................... 96
`
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`U.S. Patent No. 7,381,657
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`a)
`
`including
`“The method of claim 2, further
`uniformly sweeping the target with a magnetic
`field.” ............................................................................. 96
`
`B.
`
`Licata in view of Kelly, Collins, and Aokura Discloses and/or
`Suggests the Limitations of Claims 12 and 13 ................................... 97
`
`1.
`
`Claims 12 and 13...................................................................... 97
`
`a)
`
`b)
`
`[12] “The method of claim 2, further including
`uniformly sweeping the target with a magnetic
`field.” ............................................................................. 97
`
`[13] “The method of claim 12 wherein uniformly
`sweeping the target with a magnetic field includes
`sweeping a magnet in one direction across the
`target where the magnet extends beyond the target
`in the opposite direction.” .............................................. 97
`
`C.
`
`Licata in view of Kelly, Collins, and Dogheche Discloses
`Claims 5 and 7 .................................................................................. 102
`
`1.
`
`Claim 5 ................................................................................... 102
`
`a)
`
`“The method of claim 2 wherein the target is a
`ceramic target.” ............................................................ 102
`
`2.
`
`Claim 7 ................................................................................... 106
`
`a)
`
`“The method of claim 2 further including holding
`the temperature of the substrate substantially
`constant.” ..................................................................... 106
`
`D.
`
`Licata in view of Kelly, Collins, and Doessel Discloses and/or
`Suggests the Limitations of Claims 14-17 ....................................... 108
`
`1.
`
`Claim 14 ................................................................................. 108
`
`a)
`
`“The method of claim 2 wherein the target is an
`alloyed target.” ............................................................. 108
`
`2.
`
`Claim 15 ................................................................................. 112
`
`a)
`
`“The method of claim 14 wherein the alloyed
`target includes one or more rare-earth ions.” .............. 112
`
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`U.S. Patent No. 7,381,657
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`3.
`
`Claim 16 ................................................................................. 113
`
`a)
`
`“The method of claim 14 wherein the alloyed
`target includes Si and Al.” ........................................... 113
`
`4.
`
`Claim 17 ................................................................................. 114
`
`a)
`
`“The method of claim 14 wherein the alloyed
`target includes one or more elements taken from a
`set consisting of Si, Al, Er, Yb, Zn, Ga, Ge, P. As,
`Sn, Sb, Pb, Ag, Au, Ce, Pr, Nd, Pm, Sm, Eu, Gd,
`Th, Dy Ho, Tm, and Lu.” ............................................ 114
`
`X.
`
`CONCLUSION ........................................................................................... 115
`
`
`
`
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`Declaration of Dr. Vivek Subramanian
`U.S. Patent No. 7,381,657
`
`
`
`I, Vivek Subramanian, declare as follows:
`
`I.
`
`INTRODUCTION
`
`1.
`
`I have been retained as an independent expert consultant in this
`
`proceeding before the United States Patent and Trademark Office (“PTO”)
`
`regarding U.S. Patent No. 7,381,657 (“the ’657 patent”) (Ex. 1001).1 I have been
`
`asked to consider whether prior art references disclose or suggest the features
`
`recited in claims 1-21 (“the challenged claims”) of the ’657 patent. My opinions
`
`are set forth below.
`
`2.
`
`I am being compensated at a rate of $650/hour for my work in this
`
`proceeding. My compensation is in no way contingent on the nature of my
`
`findings, the presentation of my findings in testimony, or the outcome of this or
`
`any other proceeding. I have no other interest in this proceeding.
`
`
`
`
` In this Declaration, I refer to exhibits that I understand are to be attached to the
`
` 1
`
`petition for Inter Partes Review of the ’657 patent.
`
`
`
`
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`1
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`U.S. Patent No. 7,381,657
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`II. BACKGROUND AND QUALIFICATIONS
`
`3. My qualifications are stated more fully in my curriculum vitae, which
`
`is attached as Ex. 1003. Below is a summary of my education, work experience,
`
`and other qualifications.
`
`4.
`
`I received a bachelor’s degree summa cum laude in electrical
`
`engineering from Louisiana State University in 1994. I received M.S. and Ph.D.
`
`degrees in electrical engineering, in 1996 and 1998, respectively, from Stanford
`
`University.
`
`5.
`
`Throughout the course of my education, including my B.S., M.S., and
`
`Ph.D. degrees, I was involved in deposition technology for thin films, including
`
`sputtering technology, and more specifically reactive sputter technology. For
`
`example, during my PhD, I performed research on the deposition of films of
`
`metals, oxides, and semiconductors via sputtering, including Aluminum, Tungsten,
`
`Tungsten Silicide, Titanium, Titanium Nitride, and Silicon Dioxide.
`
`6.
`
`After completing my Ph.D.,
`
`I held multiple appointments
`
`simultaneously between 1998 and 2000. I served as a Consulting Assistant
`
`Professor in the Electrical Engineering Department of Stanford University. I also
`
`served as a Visiting Research Engineer in the Department of Electrical Engineering
`
`
`
`
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`2
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`U.S. Patent No. 7,381,657
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`and Computer Sciences at the University of California, Berkeley, where my
`
`research focused on 25nm metal oxide semiconductor field effect transistor
`
`(MOSFET) design and fabrication.
`
` I worked on technologies for high-
`
`performance transistor processes, and I published several papers as a direct
`
`outcome of this technology development. As part of my research work both at
`
`Berkeley and at Stanford during this period, I performed research on the use of
`
`sputtering and reactive sputtering.
`
`7.
`
`During the same period, I also served as a founder and member of
`
`technical staff of Matrix Semiconductor, a startup company that developed high-
`
`density nonvolatile memories. At Matrix, I led much of the process development
`
`effort to develop a new type of memory. We made extensive use of sputtering and
`
`reactive sputtering in this work, and I led much of the process development in this
`
`regard. Matrix was subsequently acquired by Sandisk.
`
`8.
`
`In 2000, I became an assistant professor at the University of
`
`California, Berkeley in the Department of Electrical Engineering & Computer
`
`Sciences. In 2005, I was promoted to the position of tenured Associate Professor,
`
`and in 2011, I was promoted to full Professor. In 2018, I became a full Professor
`
`of Microtechnology at EPFL in Switzerland, where I lead the Laboratory for
`
`Advanced Fabrication Technologies (LAFT). The lab focuses on the development
`
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`U.S. Patent No. 7,381,657
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`and application of advanced additive fabrication techniques for realizing precision
`
`microelectronic and electromechanical systems. As of 2020, I have completed my
`
`move to EPFL and have therefore converted to an adjunct appointment at
`
`Berkeley.
`
`9.
`
`Starting in 2004, I was a founding technical advisor for Kovio. Under
`
`my leadership, Kovio re-focused on RFID and RF anti-theft systems. I led the
`
`development of Kovio’s first commercial RFID tag product, including the design
`
`of both the tag and the reader. My involvement with Kovio ended with Kovio’s
`
`acquisition by Thin Film Electronics ASA, but Kovio continues to focus on this
`
`area.
`
`10.
`
`I co-founded Locix Inc. in 2014. Locix develops and sells a range of
`
`wireless-enabled products, including proprietary Wi-Fi-based RF localization
`
`systems and sub-GHz low-power wireless sensor networks. As CTO of Locix, I
`
`led the development of the entire Locix RF product portfolio. I continue to be
`
`involved with Locix on a regular basis.
`
`11.
`
`I have authored or co-authored over 200 technical papers in
`
`international journals and conferences and have been named an inventor or co-
`
`inventor on more than 50 patents, many of which cover aspects of thin film
`
`
`
`
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`4
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`U.S. Patent No. 7,381,657
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`deposition and devices based on the same, including use of sputtering and reactive
`
`sputtering in this regard.
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`
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`U.S. Patent No. 7,381,657
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`III. MATERIALS REVIEWED
`
`13. The opinions contained in this Declaration are based on the
`
`documents I reviewed, my professional judgment, as well as my education,
`
`experience, and knowledge regarding systems and processes for sputtering-based
`
`deposition of films on substrates.
`
`14.
`
`In forming my opinions expressed in this Declaration, I reviewed the
`
`following materials:
`
`Ex. 1001
`
`U.S. Patent No. 7,381,657
`
`Ex. 1004
`
`Prosecution History of U.S. Patent No. 7,381,657
`
`Ex. 1005
`
`U.S. Patent No. 6,342,134 to Barber et al.
`
`Ex. 1006
`
`U.S. Patent No. 6,485,602 to Hirose
`
`Ex. 1007
`
`U.S. Patent No. 5,651,865 to Sellers
`
`Ex. 1008
`
`A. Belkind et al., Pulsed-DC reactive sputtering of
`dielectrics: Pulsing parameter effects (2000)
`
`Ex. 1009
`
`U.S. Patent No. 4,464,223 to Gorin
`
`Ex. 1010
`
`U.S. Patent No. 6,132,564 to Licata
`
`Ex. 1011
`
`U.S. Patent No. 5,942,089 to Sproul
`
`Ex. 1012
`
`U.S. Patent No. 6,352,629 to Wang
`
`Ex. 1013
`
`S. Gibilisco, Handbook of Radio & Wireless Technology
`(1999)
`
`
`
`
`
`6
`
`
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`U.S. Patent No. 7,381,657
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`Ex. 1014
`
`J. Joo, Low-temperature polysilicon deposition by ionized
`magnetron sputtering (2000)
`
`Ex. 1016
`
`U.S. Patent No. 4,579,618 to Celestino
`
`Ex. 1017
`
`International Publication No. WO 02/23588 to Quon
`
`Ex. 1018
`
`International Publication No. WO 01/6300 to Johnson
`
`Ex. 1019
`
`U.S. Patent No. 6,695,954 to Hong
`
`Ex. 1020
`
`U.S. Patent No. 6,153,068 to Ohmi
`
`Ex. 1021
`
`U.S. Patent No. 4,846,920 to Keller
`
`Ex. 1023
`
`U.S. Patent No. 5,302,882 to Miller
`
`Ex. 1024
`
`Ex. 1025
`
`Ex. 1026
`
`Ex. 1029
`
`Ex. 1030
`
`Ex. 1031
`
`Ex. 1032
`
`Ex. 1033
`
`Pinnacle Plus+ 10KW (325-650 Vdc) Master/Slave AE Bus,
`DeviceNet, MDXL User, UHF Output User Manual (March
`2005)
`The Advanced Energy MDX Magnetron Drive, Advanced
`Energy Industries, Inc. (March 1993)
`Pinnacle 10x6 kW DeviceNet, MDXL User 5702063-C, User
`Manual, (May 2000)
`E. Dogheche, Growth and optical characterization of
`aluminum nitride thin films deposited on silicon by radio-
`frequency sputtering, Applied Physics Letters (1999)
`U.S. Patent No. 6,506,686 to Masuda
`
`K. Nam, A study on the high rate deposition of CrN films with
`x controlled microstructure by magnetron sputtering, Surface
`& Coatings Technology (2000)
`D. Mattox, Handbook of Physical Vapor Deposition (PVD)
`Processing – Film Formation, Adhesion, Surface Preparation
`and Contamination Control (1998)
`U.S. Patent No. 5,830,327 to Kolenkow
`
`Ex. 1034
`
`U.S. Patent Publication No. 2001/0041252 to Laird
`
`
`
`
`
`7
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`Declaration of Dr. Vivek Subramanian
`U.S. Patent No. 7,381,657
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`
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`Ex. 1035 M. Ruske, Properties of SiO2 and Si3N4 layers deposited by
`MF twin magnetron sputtering using different target
`materials, Thin Solid Films (1999)
`Ex. 1036 W. Sproul, High-rate reactive DC magnetron sputtering of
`oxide and nitride superlattice coatings (1998)
`U.S. Patent Publication No. 2003/0029563 to Kaushal
`
`Ex. 1037
`
`Ex. 1038
`
`U.S. Patent No. 6,627,323 to Nagaraj
`
`Ex. 1040
`
`U.S. Patent No. 6,001,227 to Pavate
`
`Ex. 1041
`
`Ex. 1043
`Ex. 1044
`
`S. Wolf et al., Silicon Processing for the VLSI Era, Vol. 1
`(2000)
`
`U.S. Patent Publication No. 2001/0031383 to Sakawaki
`U.S. Patent No. 4,895,631 to Wirz
`
`Ex. 1045
`
`U.S. Patent No. 7,041,391 to Ando
`
`Ex. 1046
`
`U.S. Patent No. 6,984,550 to Yamazaki
`
`Ex. 1047
`
`Ex. 1048
`
`Ex. 1049
`
`A. Billard, Low-frequency modulation of pulsed d.c. or r.f.
`discharges for controlling the reactive magnetron sputtering
`process, Surface & Coatings Technology (1996)
`P. Kelly, The deposition of aluminum oxide coatings by
`reactive unbalanced magnetron sputtering (1996)
`U.S. Patent No. 7,247,227 to Hanson
`
`Ex. 1051
`
`International Publication No. WO 96/06203 to O’Brien
`
`Ex. 1057
`
`Ex. 1058
`
`Ex. 1059
`
`
`U.S. Patent No. 6,284,110 to Sill
`
`U.S. Patent No. 5,148,133 to Zennamo
`
`P. Kelly et al., Reactive pulsed magnetron sputtering
`process for alumina films (2000)
`
`
`
`
`
`
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`U.S. Patent No. 7,381,657
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`
`Ex. 1062
`
`Ex. 1065
`
`Ex. 1067
`
`Ex. 1068
`
`Ex. 1069
`
`Ex. 1070
`Ex. 1071
`Ex. 1072
`Ex. 1073
`Ex. 1074
`
`Pinnacle 20 kW DeviceNet, MDXL User 5702199-A, User
`Manual, (April 2001)
`Pinnacle Plus Pulsed DC Power Supply Data Sheet (April
`1999)
`Pinnacle Plus 10kW User 5702269-B, User Manual, (June
`2002)
`Japanese Patent Publication No. JPH10102247A to Aokura
`and certified English translation of JPH10102247A
`
`U.S. Patent Application Publication US 2001/0047838 to
`Segal
`U.S. Patent No. 5,527,605 to Doessel
`U.S. Patent No. 6,077,384 to Collins et al.
`U.S. Patent No. 5,130,005 to Hurwitt
`U.S. Patent No. 4,006,070 to King
`Sellers, Asymmetric bipolar pulsed DC: the enabling
`technology for reactive PVD (1998)
`
` I
`
` also considered any other documents and materials I refer to in this Declaration.
`
`15. My opinions contained in this declaration are based on the documents
`
`I reviewed and my knowledge and professional judgment. My opinions have also
`
`been guided by my appreciation of how a person of ordinary skill in the art would
`
`have understood the state of the art, the prior art, and the claims and the
`
`specification of the ’657 patent at the time of the alleged invention, which I discuss
`
`below.
`
`16.
`
`I have been asked to initially consider that the time of the alleged
`
`invention of the ’657 patent was around 2002 (including and up to March 16,
`
`
`
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`Declaration of Dr. Vivek Subramanian
`U.S. Patent No. 7,381,657
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`2002), which corresponds to the filing date of the parent application for ‘657
`
`patent. (Ex. 1001, Cover.)
`
`17. Based on my experience and expertise, it is my opinion that certain
`
`references disclose and/or suggest all the features recited in challenged claims of
`
`the ’657 patent, as I discuss in detail below.
`
`
`
`
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`
`
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`Declaration of Dr. Vivek Subramanian
`U.S. Patent No. 7,381,657
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`IV. PERSON OF ORDINARY SKILL IN THE ART AND THE TIME OF
`THE ALLEGED INVENTION
`
`18.
`
`I am familiar with the level of ordinary skill in the art regarding the
`
`’657 patent as of what I understand to be around the claimed priority date of March
`
`16, 2002. Considering the ’657 patent, the technology, the educational level and
`
`experience of workers in the field relating to the patent, and problems and
`
`solutions in that field (e.g., processes and related systems for sputtering deposition
`
`of films on substrates), and drawing on my own experience, I believe a person of
`
`ordinary skill in the art at the time of the alleged invention (around March 16,
`
`2002) would have had a Master’s degree in Electrical Engineering or Material
`
`Science (or an equivalent subject) and at least two years of relevant experience, or
`
`a Bachelor’s degree in Electrical Engineering or Material Science (or an equivalent
`
`subject) and at least four years of relevant experience. Relevant experience in the
`
`context of the ’657 patent refers to experience with sputtering deposition of films
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`on substrates, as referenced in the ’657 patent. (See ’657 patent (Ex. 1001) at 1:10-
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`14, 2:45-47.)
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`19. My opinions in this Declaration regarding the ’657 patent and the
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`prior art (including the state of the art) are from the perspective of one of ordinary
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`skill in the art as I defined above, during the relevant timeframe (e.g., the time of
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`the alleged invention), which I discussed above as being around March 16, 2002.
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`V. TECHNICAL BACKGROUND
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`20. Below, I present a brief overview of certain aspects of systems and
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`processes relating to the sputtering deposition of films on substrates prior to and at
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`the time of the alleged invention for the ’657 patent. The functionalities and
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`concepts I describe below in this technical background section reflect the state of
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`the art that a person of ordinary skill in the art would have had knowledge of and
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`understood prior to and at the time of the alleged invention of the ’657 patent. I
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`rely on, and incorporate as applicable (even if not expressly mentioned below in
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`Section IX), the following disclosures and opinions to support my opinions in this
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`Declaration, including those opinions relating to how the prior art discloses and/or
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`suggests the challenged claims of the ’657 and how and why a person of ordinary
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`skill in the art would have been motivated to consider and combined the
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`disclosures and suggestions from that prior art as I explain below in Section IX.
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`The concepts below would have been within the knowledge and mindset of a
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`person of ordinary skill in the art at the time.
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`A.
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`Sputter Deposition
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`21. Sputter deposition, which was also often known as just “sputtering,” is
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`a film deposition technique that takes place in a plasma process chamber, where a
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`target is bombarded with gas ions, such as noble/inert gas (e.g., argon) ions. (Ex.
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`1007, 1:19-21; see also Ex. 1032, 6; Ex. 1041, 5-10 (discussions regarding the
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`physics of sputtering).) Those of ordinary skill in the art understood that ionized
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`gas was (and is) also known as a plasma. (Ex. 1041, 3-4 (disclosing that a plasma
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`is a “partially ionized gas”).) In a sputtering process, the gas ion bombardment
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`mechanically frees atoms of the target material, and the target material is then
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`deposited, forming a film on a substrate placed in the plasma chamber. (Ex. 1007,
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`1:21-23.) Argon was known generally as the gas of choice for sputtering processes
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`because “it is easily available (hence low in cost), and its mass is a good match to
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`those of the elements most frequently sputtered (Al, Cu, Si, and Ti).” (Ex. 1041, 8;
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`see also Ex. 1032, 7 (“typically argon…is used for inert gas sputtering since it is a
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`relatively inexpensive inert gas”).)
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`22. Many types of target materials (e.g., element, alloy, or compound)
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`were known and available for sputter deposition processes, which allowed for
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`diverse fields of applications. (Ex. 1032, 18 (disclosing that one of the advantages
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`of sputtering deposition is that the method is capable of sputtering “element, alloy,
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`or compound” materials); see also id., 19-20 (disclosing a list of exemplary target
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`materials available for sputtering for various fields of applications, e.g.,
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`semiconductor devices, optical coatings, and wear/erosion-resistant coatings …
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`etc.); Ex. 1011, 3:58-60). For example, single element targets made of aluminum
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`or silicon were well known before March 2002. (See e.g., Ex. 1005, 6:42-50.) It
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`was also well known that a target may be made of an alloy, which contained, for
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`example, both aluminum and silicon. (See e.g., Ex. 1034, ¶[0027].) It was also
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`known that an alloy target may also include rare-earth ions, such as yttrium. (Ex.
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`1036, 6; Ex. 1069, ¶¶[0041]-[0048].) Furthermore, oxides of yttrium-containing
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`alloy such, as yttria-stabilized zirconia (YSZ), were known to be widely used as a
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`thermal-barrier coating for its high-temperature capability. (Ex. 1038, 1:30-35.)
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`Also, a person of ordinary skill in the art would have appreciated and known that
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`an aluminum oxynitride layer (AlNxOy), deposited using a “reactive” sputtering
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`technique (which I discuss in the next section below), was used in manufacturing
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`displays, particularly useful for “blocking moisture and oxygen” and “to prevent
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`impurity…from entering” semiconductor devices in the displays and the film also
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`has other useful properties including “a high thermal conductivity, a heat radiation
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`effect, and a very high light transmitting property.” (Ex. 1046, 19:34-39.)
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`23. Typical sputtering systems were also known to include a substrate
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`holder, upon which a substrate is positioned to face the target for film deposition.
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`(See, e.g., Ex. 1005, FIG. 2 (disclosing a substrate platen 115, upon which a
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`U.S. Patent No. 7,381,657
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`substrate 110 is positioned).) A wide range of substrate materials were known to
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`be used, including, for example, silicon, quartz, sapphire, aluminum oxide (id.,
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`3:63-65), or a piece of steel (Ex. 1011, 3:56-58). Additionally, those of ordinary
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`skill in the art were aware, would have appreciated, and understood the benefits of
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`monitoring and controlling the temperature of the substrate (via for example
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`temperature control circuits or the like) to obtain a high-quality sputter deposited
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`film (Ex. 1029, 2) and that the temperature can be controlled with a high accuracy
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`(Ex. 1030, 1:33-40 (disclosing temperature control within a plasma environment
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`with an “accuracy of ± 5 °C), 1:60-67 (disclosing temperature control within a
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`plasma environment with “a high accuracy of ± 2 °C).)
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`B. Reactive Sputter Deposition
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`24. A reactive sputtering process differs from the above discussed
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`sputtering process as it introduces one or more reactive gases (e.g., oxygen or
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`nitrogen) in addition to the noble/inert gas (e.g., argon). (Ex. 1005, 2:5-7.)
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`Typically, the reactive gases were known to have low atomic masses and known to
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`be not as effective in sputtering. Therefore, a heavier noble/inert gas, such as
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`argon, was known to be used in the reactive sputtering process to sputter the target
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`material. (Ex. 1032, 8.)
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`25. The reactive gas reacts with the target material to produce a film that
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`is sputtered onto the substrate. (Ex. 1005, 2:5-8; see also Ex. 1007, 1:7-11.)
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`Reactive sputtering can be used for forming insulating layers, such as oxides or
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`nitrides of a metal, by using a metallic or conductive target and an oxygen or
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`nitrogen-containing reactive gas. (Ex. 1007, 1:11-14.) For example, a layer of
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`aluminum oxide film may be formed by using an aluminum target and an oxygen-
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`containing reactive gas. (Id., 1:27-29; see also id., 1:29-37 (describing that other
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`types of target materials and reactive gases may be used).)
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`26. One issue associated with reactive sputtering that those of ordinary
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`skill in the art would have understood and appreciated was the buildup of
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`insulating materials on the target surface, which was also known as “poisoning” of
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`the target that may significantly reduce the sputtering rate and causes arcing on the
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`target. (Ex. 1007, 1:45-47; see also Ex. 1005, 2:37-43; Ex. 1048, Abstract.) It was
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`therefore known to use a pulsed DC power supply (discussed further below) to
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`reduce such arcing.
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`C.
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`27.
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`Power Supplies Used for Reactive Sputtering
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`It was known by those of ordinary skill in the art prior to March 2002
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`to use in such reactive sputtering systems a power supply connected to the target to
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`apply a bias in order to create a plasma and to facilitate sputtering. (See, e.g., Ex.
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`1005, 6:6-8, FIG. 2; Ex. 1007, 9:32-37, FIG. 12.) Such skilled persons would have
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`understood that a continuous (i.e., non-pulsed) DC power supply was typically not
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`suitable for reactive sputtering because, once the target surface reacts with the
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`reactive gas and forms an insulating layer (a “poisoned” target), charges buildup on
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`the insulated target surface lead to arcing and also prevent bombardment/sputtering
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`of the surface (e.g., ceasing or significantly hindering the sputter deposition
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`process). (Ex. 1008, 1; see also Ex. 1007, 6:2-5 (discussing arcing’s deleterious
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`effects on the target); Ex. 1032, 3.) Those of ordinary skill in the art at the time
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`understood that such issues can be resolved through the use of a pulsed DC power
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`supply, which reverses its negative bias to the positive bias periodically in order to
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`discharge poisoned/insulated target surface, preventing arcing and allowing the ion
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`bombardment to continue (once the pulse flips back to the negative bias). (Ex.
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`1008, 1.) For example, a typical waveform of a pulsed DC power supply is
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`shown in Figure 1 of Belkin, which I annotate below.
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`U.S. Patent No. 7,381,657
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`(Ex. 1008, FIG. 1 (annotat