UNITED STATES PATENT AND TRADEMARK OFFICE
`
`____________________
`
`
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`
`____________________
`
`US ENDODONTICS, LLC,
`Petitioner
`
`v.
`
`GOLD STANDARD INSTRUMENTS, LLC
`Patent Owner
`____________________
`
`Case: PGR2015-00019
`U.S. Patent No. 8,876,991
`____________________
`
`
`
`DECLARATION OF A. JON GOLDBERG
`
`
`
`
`
`PGR2015-00019 – Ex. 1002
`US Endodontics, LLC,
` Petitioner
`1
`
`
`
`
`
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`
`
`

`
`
`
`EXHIBIT LIST
`
`
`
`Exhibit #
`1001
`
`Exhibit Description
`U.S. Patent No. 8,876,991
`
`1002
`
`1003
`
`1004
`
`1005
`
`1006
`
`1007
`
`1008
`
`1009
`
`1010
`
`1011
`
`1012
`
`1013
`
`1014
`
`1015
`
`Declaration of A. Jon Goldberg
`
`Prosecution history of U.S. Patent No. 8,876,991
`Fujio Miura et al., The super-elastic property of the Japanese NiTi
`alloy wire for use in orthodontics, 90 AM. J. ORTHODONTICS &
`DENTOFACIAL ORTHOPEDICS 1 (1986)
`
`transformation
`investigation of phase
`Satish B. Alapati, “An
`mechanisms for nickel-titanium rotary endodontic instruments,” PhD
`thesis, 2006
`Alan R. Pelton et al., Optimisation of Processing and Properties of
`Medical-Grade Nitinol Wire, MINIMALLY INVASIVE THERAPIES &
`ALLIED TECHS. 107 (2000)
`
`U.S. Patent No. 5,697,906 to Ariola et al.
`
`Prosecution history of U.S. Patent No. 8,727,773
`
`Prosecution history of U.S. Patent No. 8,083,873
`
`Prosecution history of U.S. Patent No. 8,062,033
`
`U.S. Patent No. 8,727,773
`
`Prosecution history of European Patent Application No. 05756629.1
`Excerpts of Transcript of Motion Hearing, Nov. 25, 2014, Dentsply
`International, Inc. v. US Endodontics, LLC, Docket No. CV-2-14-196
`(E.D. Tenn.)
`International Standard ISO 3630-1, 2nd ed. (2008)
`Declaration of Walter Zanes
`
`
`
`
`
`2
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`

`
`
`
`Exhibit #
`1016
`
`1017
`
`1018
`
`1019
`
`1020
`
`1021
`
`1022
`
`1023
`
`1024
`
`1025
`
`1026
`
`1027
`
`1028
`
`Exhibit Description
`Edgar Schäfer et al., Bending Properties of Rotary Nickel-Titanium
`Instruments, 96 ORAL SURGERY ORAL MEDICINE ORAL PATHOLOGY
`757 (2003)
`Luca Testarelli et al., Bending Properties of a New Nickel-Titanium
`Alloy with a Lower Percent by Weight of Nickel, 37 J. ENDODONTICS
`1293 (2011)
`
`Declaration of Adam Kozak
`Excerpts of Expert Report of Robert Sinclair, Ph.D., Dentsply
`International, Inc. v. US Endodontics, LLC, Docket No. CV-2-14-196
`(E.D. Tenn.)
`Alan R. Pelton et al., The Physical Metallurgy of Nitinol for Medical
`Applications, 55 J. METALS 33-37 (May 2003)
`S. Miyazaki et al., Characteristics of Deformation and
`Transformation Pseudoelasticity in Ti-Ti Alloys, 43 J. PHYSIQUE
`COLLOQUES C4-255 (1982)
`
`U.S. Patent App. Pub. No. 2008/0032260 A1 to Luebke
`
`International Standard ISO 3630-1, 1st ed. (1992)
`
`U.S. Patent No. 5,628,674 to Heath et al.
`
`U.S. Patent Application Publication No. US 2006/0115786 A1 to
`Matsutani et al.
`
`Japanese Unexamined Patent Application Publication Number
`2006-149675 to Matsutani et al.
`
`English translation of Japanese Unexamined Patent Application
`Publication Number 2006-149675 to Matsutani et al.
`
`Transmittal from prosecution history of U.S. Patent Application Serial
`No. 11/287,771, enclosing Japanese Patent Application No. 2004-
`344717 to Matsutani et al.
`
`
`
`
`
`3
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`

`
`
`
`Exhibit #
`1029
`
`1030
`
`1031
`
`1032
`
`1033
`
`1034
`
`1035
`
`1036
`
`Exhibit Description
`Transmittal from prosecution history of U.S. Patent Application Serial
`No. 11/287,771, with English translation of enclosed Japanese Patent
`Application No. 2004-344717 to Matsutani et al.
`Grégoire Kuhn & Laurence Jordan, Fatigue and Mechanical
`Properties of Nickel-Titanium Endodontic Instruments, 28 J.
`ENDODONTICS 716 (2002)
`
`U.S. Patent App. Pub. No. 2002/0137008 A1, McSpadden et al.
`
`Teresa Roberta Tripi et al., “Fabrication of Hard Coatings on NiTi
`Instruments,” 29 J. ENDODONTICS 132 (2003)
`Harmeet Walia et al., An Initial Investigation of the Bending and
`Torsional Properties of Nitinol Root Canal Files, 14 J. ENDODONTICS
`346 (1988)
`M. G. A. Bahia, Fatigue Behaviour of Nickel–Titanium Superelastic
`Wires and Endodontic Instruments, FATIGUE & FRACTURE OF ENG’G
`MATS. & STRUCTURES 29, 518–523 (2006)
`
`Printout of the webpage:
`http://www.tulsadentalspecialties.com/default/endodontics/RotaryFile
`s/ProFileISO.aspx, accessed on July 22, 2015, and Safety Data Sheet
`for Nickel Titanium Wire: NITINOL 55, linked on that webpage
`Masao J. Drexel et al., The Effects of Cold Work and Heat Treatment
`on the Properties of Nitinol Wire, Proc. Int’l Conference on Shape
`Memory & Superelastic Techs., SMST-2006, pp. 447-454 (2008)
`
`Prosecution history of U.S. Patent No. 8,562,341
`1037
`1038 W.A. Brantley et al., Differential Scanning Calorimetric Studies of
`Nickel Titanium Rotary Endodontic Instruments, 28 J. ENDODONTICS
`567 (2002)
`
`
`
`Prosecution history exhibits are cited using page numbers added by Petitioner.
`Other exhibits are cited by their original page or paragraph numbers.
`
`
`
`
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`4
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`
`Table of Contents
`
`
`
`D. 
`
`E. 
`
`
`I. 
`Background and Qualifications ....................................................................... 8 
`Assignment and Materials Reviewed ............................................................ 10 
`II. 
`III.  Overview of the ’991 Patent .......................................................................... 12 
`IV.  Claims of the ’991 Patent .............................................................................. 14 
`V. 
`Scientific and Technological Background ..................................................... 15 
`VI.  Claim Construction ........................................................................................ 22 
`A. 
`“heat-treating the entire shank” ................................................................ 22 
`B. 
`“wherein the heat treated shank has an angle greater than 10
`degrees of permanent deformation after torque at 45 degrees
`of flexion when tested in accordance with ISO Standard
`3630-1” ..................................................................................................... 23 
`“permanent deformation” ......................................................................... 23 
`C. 
`“diameter” ................................................................................................. 23 
`D. 
`VII.  Written Description in Prior Applications ..................................................... 24 
`A. 
`Standard Applied ...................................................................................... 24 
`B. 
`Applications in the Priority Chain of the ’991 Patent .............................. 25 
`C. 
`Earlier Applications Do Not Support Heat-Treatment in the
`Range of 25°C to the Melting Point of the Alloy for
`Producing Permanent Deformation .......................................................... 26 
`Earlier Applications Do Not Support Heat-Treatment in a
`Range of 300°C to the Melting Point of the Alloy ................................... 28 
`Earlier Applications Do Not Support Heat-Treatment in an
`Unreactive Atmosphere ............................................................................ 30 
`The ’933 Application Does Not Describe Heat-Treatment
`in an Atmosphere Other Than One Consisting Essentially
`of a Gas Unreactive with the Instrument ............................................. 30 
`The Prosecution History of the ’933 Application
`Confirms That It Is Limited to Unreactive-Gas
`Atmospheres ........................................................................................ 34 
`iii.  Applications Filed After the ’933 Application Also Do
`Not Describe Heat-Treatment in Reactive Atmospheres .................... 36 
`
`i. 
`
`ii. 
`
`
`
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`
`5
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`

`
`
`
`VIII.  Standards Applied in Analyzing Patentability Issues .................................... 36 
`IX.  Patentability Analysis .................................................................................... 39 
`A. 
`Level of Skill in the Art ............................................................................ 39 
`B. 
`Scope and Content of the Prior Art .......................................................... 40 
`Overview of ISO 3630-1 ..................................................................... 41 
`i. 
`Overview of Luebke 2008 ................................................................... 41 
`ii. 
`iii.  Overview of Kuhn ............................................................................... 41 
`iv.  Overview of McSpadden ..................................................................... 42 
`v. 
`Overview of Pelton .............................................................................. 43 
`vi.  Overview of Walia .............................................................................. 45 
`vii.  Overview of Miyazaki ......................................................................... 46 
`viii.  Overview of Matsutani ........................................................................ 50 
`ix.  Overview of Tripi ................................................................................ 53 
`Ground 1: Lack of Enablement (Claims 12-16) ....................................... 53 
`Heat Treatment At or Near 25°C and Up to 300°C to
`Achieve the Claimed Permanent Deformation is Not
`Enabled ................................................................................................ 54 
`Undue Experimentation Is Necessary to Practice the Full
`Scope of the Challenged Claims ......................................................... 60 
`D.  Ground 2: Lack of Written Description (Claims 12-16) .......................... 67 
`E. 
`Ground 3: Anticipation of Claims 12-16 by Luebke 2008 ...................... 71 
`Anticipation of claim 12 ...................................................................... 71 
`i. 
`Anticipation of claim 13 ...................................................................... 75 
`ii. 
`iii.  Anticipation of claim 14 ...................................................................... 75 
`iv.  Anticipation of claim 15 ...................................................................... 76 
`v. 
`Anticipation of claim 16 ...................................................................... 76 
`Ground 4: Obviousness of Claim 15 over Luebke 2008
`Alone or in View of Heath or ISO 3630-1 ............................................... 77 
`G.  Ground 5: Anticipation of Claims 12-16 by Matsutani .......................... 78 
`i. 
`Anticipation of claim 12 ...................................................................... 78 
`ii. 
`Anticipation of claim 13 ...................................................................... 81 
`
`i. 
`
`ii. 
`
`C. 
`
`F. 
`
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`6
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`

`
`I. 
`
`J. 
`
`iii.  Anticipation of claim 14 ...................................................................... 81 
`iv.  Anticipation of claim 15 ...................................................................... 82 
`v. 
`Anticipation of claim 16 ...................................................................... 83 
`H.  Ground 6: Anticipation of Claims 12-14 and 16 by Kuhn ....................... 83 
`i. 
`Anticipation of claim 12 ...................................................................... 83 
`ii. 
`Anticipation of claim 13 ...................................................................... 90 
`iii.  Anticipation of claim 14 ...................................................................... 90 
`iv.  Anticipation of claim 16 ...................................................................... 90 
`Ground 7: Obviousness of Claim 15 over Kuhn Either Alone
`or in View of Heath or ISO 3630-1 .......................................................... 91 
`Ground 8: Obviousness of Claims 12-16 over Kuhn Either
`Alone or in View of Heath or ISO 3630-1 ............................................... 92 
`K.  Ground 9: Obviousness of Claims, 12-14 and 16 in View of
`McSpadden and Pelton in View of Kuhn ................................................. 93 
`Obviousness of claim 12 ..................................................................... 97 
`i. 
`Obviousness of claim 13 ................................................................... 101 
`ii. 
`iii.  Obviousness of claim 14 ................................................................... 101 
`iv.  Obviousness of claim 16 ................................................................... 101 
`Ground 10: Obviousness of Claim 15 over McSpadden and
`Pelton in View of Kuhn and in Further View of Heath or
`ISO 3630-1 ............................................................................................. 102 
`M.  Ground 11: Obviousness of Claims 12-14 and 16 over Tripi
`in view of McSpadden ............................................................................ 103 
`N.  Ground 12: Obviousness of Claim 15 Over Tripi in View of
`McSpadden and in Further View of Heath or ISO 3630-1 .................... 104 
`
`L. 
`
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`7
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`
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`I, A. Jon Goldberg, do hereby declare and state as follows:
`
`I.
`
`BACKGROUND AND QUALIFICATIONS
`
`1. My business address is University of Connecticut Health Center,
`
`Center for Biomaterials, Department of Reconstructive Sciences, 263 Farmington
`
`Avenue, Farmington, Connecticut. I hold a B.S. in Metallurgical Engineering
`
`(1970) from Drexel University, an M.S.E. in Metallurgical Engineering (1971) and
`
`a Ph.D. in Dental Materials-Metallurgical Engineering (1977), both from the
`
`University of Michigan. My doctoral degree was a combined degree from the
`
`School of Engineering and the School of Dentistry.
`
`2.
`
`Since 1975, I have been employed at the University of Connecticut in
`
`the following positions: Assistant Professor (1975-1980), Associate Professor
`
`(1980-1986), and Professor (1986 to Present), all in the Department of Restorative
`
`Dentistry, School of Dental Medicine. Since 1995, I have served as the Director of
`
`the Center for Biomaterials at the University of Connecticut Health Center. I am
`
`also a member of the Advisory Board of the Institute of Material Science at the
`
`University of Connecticut.
`
`3.
`
`I have authored 70 scientific research articles, 100 abstracts, and eight
`
`books and book chapters. I have presented the results of my research at numerous
`
`national and international meetings, and have given several invited lectures. I am
`
`co-director of a training grant from the National Institute of Dental and
`
`
`
`
`
`8
`
`

`
`
`
`Craniofacial Research, National Institutes of Health. I am an inventor or co-
`
`inventor of six U.S. patents concerning the use of materials in dentistry, including
`
`titanium alloys for use in orthodontic appliances (U.S. Pat. No. 4,197,643) and
`
`composite materials used in various dental/endodontic procedures (U.S. Pat. No.
`
`4,894,012).
`
`4.
`
`I teach a variety of courses on materials engineering and materials
`
`science at the University of Connecticut, including courses on dental materials
`
`such as titanium alloys. My research activities have covered a broad range of
`
`dental materials including titanium alloys, fiber-reinforced composites for various
`
`dental clinical applications, biocatalyzed mineralization and use of high
`
`performance polyphenylene polymers in orthodontics.
`
`5.
`
`I have supervised the research of engineering and dental graduate
`
`students. I have held primary academic appointments in clinical departments where
`
`I have integrated materials science into clinical teaching and research.
`
`6.
`
`Based on my education and experience, I believe I am qualified to
`
`render opinions in the field of nickel titanium alloys, including mechanical
`
`properties and phase transformations associated with these alloys, particularly as
`
`applied in dentistry.
`
`7.
`
`A copy of my curriculum vitae is attached hereto (Ex. A).
`
`
`
`
`
`9
`
`

`
`
`
`II. ASSIGNMENT AND MATERIALS REVIEWED
`
`8.
`
`I submit this declaration in support of US Endodontics, LLC’s
`
`(“Petitioner”) petition for post-grant review of U.S. Patent No. 8,876,991 (“the
`
`’991 patent”).
`
`9.
`
`I am not an employee of Petitioner or any affiliate thereof.
`
`10.
`
`I am being compensated for my work in connection with this
`
`proceeding at a rate of $400 per hour, plus expenses.
`
`11. My compensation is in no way dependent upon the substance of the
`
`opinions I offer below, or upon the outcome of the petition for post-grant review
`
`(or the outcome of the post-grant review, if trial is instituted).
`
`12.
`
`I have been asked to provide certain opinions relating to the
`
`patentability of the ’991 patent. Specifically, I have been asked to provide my
`
`opinion regarding (i) the level of ordinary skill in the art to which the ’991 patent
`
`pertains; (ii) whether claims 12-16 are entitled to a priority date earlier than the
`
`filing date of the ’991 patent; (iii) whether claims 12-16 are adequately described
`
`and enabled by the application leading to the ’991 patent; and (iv) whether claims
`
`12-16 are anticipated by, and/or would have been obvious over, certain prior art
`
`references.
`
`13.
`
`In forming my opinions, I have reviewed the ’991 patent, its
`
`prosecution history, and certain prior art to the ’991 patent including:
`
`
`
`
`
`10
`
`

`
`
`
`
`
`a) S. Miyazaki
`
`et
`
`al., Characteristics of Deformation and
`
`Transformation Pseudoelasticity in Ti-Ti Alloys, 43 J. PHYSIQUE
`
`COLLOQUES C4-255 (1982) (“Miyazaki”);
`
`b) Fujio Miura et al., The super-elastic property of the Japanese NiTi
`
`alloy wire for use in orthodontics, 90 AM. J. ORTHODONTICS &
`
`DENTOFACIAL ORTHOPEDICS 1 (1986) (“Miura”);
`
`c) Harmeet Walia et al., An Initial Investigation of the Bending and
`
`Torsional Properties of Nitinol Root Canal Files, 14 J. ENDODONTICS
`
`346 (1988) (“Walia”);
`
`d) International Standard ISO 3630-1, 1st ed. (1992) and 2nd ed. (2008)
`
`(“ISO 3630-1”);
`
`e) U.S. Patent No. 5,628,674 to Heath et al. (“Heath”);
`
`f) Alan R. Pelton et al., Optimisation of Processing and Properties of
`
`Medical-Grade Nitinol Wire, MINIMALLY INVASIVE THERAPIES &
`
`ALLIED TECHS. 107 (2000) (“Pelton”);
`
`g) Alan R. Pelton et al., The Physical Metallurgy of Nitinol for Medical
`
`Applications, 55 J. METALS 33-37 (May 2003);
`
`h) Grégoire Kuhn & Laurence Jordan, Fatigue and Mechanical
`
`Properties of Nickel-Titanium Endodontic
`
`Instruments, 28 J.
`
`ENDODONTICS 716 (2002) (“Kuhn”);
`
`
`
`11
`
`

`
`
`
`i) U.S. Patent App. Pub. No. 2002/0137008 A1, McSpadden et al.
`
`(“McSpadden”);
`
`j) U.S. Patent Application Publication No. US 2006/0115786 A1 to
`
`Matsutani et al. (“Matsutani”), and English translations of related
`
`Japanese Unexamined Patent Application Publication No. 2006-
`
`149675 (P2006-149675A) and Japanese Patent Application 2004-
`
`344717 (P2004-344717);
`
`k) U.S. Patent App. Pub. No. 2008/0032260 A1, Luebke (“Luebke
`
`2008”); and
`
`l) Teresa Roberta Tripi et al., “Fabrication of Hard Coatings on NiTi
`
`Instruments,” 29 J. ENDODONTICS 132 (2003) (“Tripi”).
`
`I have also reviewed and am familiar with any other patents, publications, and
`
`other materials discussed below.
`
`III. OVERVIEW OF THE ’991 PATENT
`
`14. The ’991 patent is entitled “Dental and Medical Instruments
`
`Comprising Titanium” and names Neill Hamilton Luebke as its sole inventor. On
`
`its face, the patent issued November 4, 2014 from an application filed January 29,
`
`2014. It claims priority to numerous applications, the earliest of which is
`
`provisional application number 60/578,091, filed June 8, 2004.
`
`
`
`
`
`12
`
`

`
`
`
`15. The specification of the ’991 patent broadly describes the use of
`
`titanium alloys to make endodontic instruments. It broadly, and briefly, covers
`
`numerous topics, such as the shape of the instrument (a ubiquitous one), a host of
`
`different titanium alloys that may be used, heat-treatment very generally, and
`
`coating of the instruments.
`
`16. Each of the five examples described in the specification involves
`
`samples of nickel titanium endodontic files, in six sizes. Each example describes
`
`three groups of files. One group of nickel titanium (“Ni-Ti”) files was heat-treated
`
`at 500°C for 75 minutes in a furnace in an argon atmosphere, and slowly cooled.
`
`Another group was coated in titanium nitride. And, the third group was untreated.
`
`According to the ’991 patent, the heat-treated group showed the best performance
`
`based on various tests. As a result of heat-treatment, the instruments allegedly
`
`“exhibit higher resistance to torsion breakage, can withstand increased strain, have
`
`higher flexibility, have increased fatigue life and maintain any acquired shape upon
`
`fracture better,” Ex. 1001 (’991 patent) at 9:22-26.
`
`17. The claims of the ’991 patent are generally directed to heat-treating
`
`dental or endodontic instruments, but include a range of temperatures and
`
`atmospheric conditions for the heat-treatment, not just the one temperature and
`
`atmosphere disclosed in the examples. In particular, the claims are methods that
`
`include providing dental or endodontic instruments made from a superelastic Ni-Ti
`
`
`
`
`
`13
`
`

`
`
`
`alloy and heat-treating them at a temperature of at least 25°C, but below the
`
`melting point of the alloy, which is about 1300°C. Per the claims, the result is
`
`supposed to show at least 10 degrees of permanent deformation after 45 degrees of
`
`flexion when tested in accordance with ISO 3630-1.
`
`IV. CLAIMS OF THE ’991 PATENT
`
`18. The ’991 patent includes 16 claims. Claims 1, 6, and 12 are
`
`independent, and the rest dependent.
`
`19.
`
`I understand that Petitioner is challenging claims 12-16 of the ’991
`
`patent (the “Challenged Claims”). They are reproduced below for reference:
`
`12. A method for manufacturing or modifying an
`endodontic instrument for use in performing root
`canal therapy on a tooth, the method comprising:
`
`(a) providing an elongate shank having a cutting edge
`extending from a distal end of the shank along an
`axial length of the shank, the shank comprising a
`superelastic nickel titanium alloy, and
`
`(b) after step (a), heat-treating the entire shank at a
`temperature above 25° C. up to but not equal to the
`melting point of the superelastic nickel titanium
`alloy,
`
`wherein the heat treated shank has an angle greater
`than 10 degrees of permanent deformation after
`
`
`
`
`
`14
`
`

`
`
`
`torque at 45 degrees of flexion when tested in
`accordance with ISO Standard 3630-1.
`
`13. The method of claim 12 wherein:
`
`step (b) is performed in an atmosphere that is
`unreactive, ambient or any other acceptable heat
`treatment process.
`
`14. The method of claim 12 wherein:
`
`the temperature is from 300° C. up to but not equal to
`the melting point of the superelastic nickel titanium
`alloy.
`
`15. The method of claim 12 wherein:
`
`the instrument shank has a diameter of 0.5 to 1.6
`millimeters.
`
`16. The method of claim 12 wherein:
`
`the instrument shank consists essentially of a titanium
`alloy comprising 54-57 weight percent nickel.
`
`
`SCIENTIFIC AND TECHNOLOGICAL BACKGROUND
`
`V.
`
`20.
`
`I have been asked to provide a brief scientific and technological
`
`background regarding Ni-Ti and its use in endodontic instruments.
`
`
`
`
`
`15
`
`

`
`
`
`21. Endodontic therapy is commonly known as a “root canal” procedure,
`
`and it involves drilling through the hard outer portion of a tooth and removing
`
`diseased tissue (pulp) from the inside of the tooth. A small-diameter file is needed
`
`to remove the tissue from the tooth’s root(s), i.e., the parts that anchor the tooth in
`
`the bone. This thin file is the endodontic instrument to which the ’991 patent
`
`pertains.
`
`22. For many years, endodontic instruments were typically made of steel,
`
`usually stainless steel.
`
`23. The Ni-Ti alloys described and claimed by the ’991 patent were first
`
`discovered in the 1960’s, and their use in endodontics was first disclosed as early
`
`as 1988 by Walia. Properties including flexibility, superelasticity, shape memory
`
`properties, and resistance to fatigue have made Ni-Ti a desirable material for
`
`endodontic files ever since it was first used for that purpose.
`
`24. The ’991 patent does not describe the superelastic or shape memory
`
`properties, or microscopic structure of Ni-Ti, in any detail. However, the applicant
`
`did rely on such characteristics during prosecution to distinguish the prior art.
`
`Therefore, I will provide a basic overview.
`
`25. When appropriately processed, Ni-Ti can exhibit superelasticity (also
`
`known as pseudoelasticity) and shape memory in a temperature-dependent fashion.
`
`Superelasticity means that the material is relatively rigid until a threshold stress is
`
`
`
`
`
`16
`
`

`
`
`
`applied to it; above that threshold, the material becomes considerably more
`
`flexible. When the stress is removed, the material reverts to its original shape. A
`
`shape memory material is one that is flexible and does not revert to its original
`
`shape immediately after it is deformed. However, when the material is heated past
`
`a certain temperature, it then reverts to its pre-deformation shape, even though it
`
`held its deformed shape prior to heating. In other words, it “remembers” its
`
`original shape.
`
`26. These properties result from the microscopic structure of Ni-Ti. Ni-Ti
`
`alloys are crystalline, meaning the material’s atoms have a well-defined crystal
`
`structure. Changes in temperature or stress can impact the crystal structure,
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`resulting in different “phases.” Various properties of Ni-Ti depend in part on the
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`crystalline phases that are present in the material. In general, at higher
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`temperatures, Ni-Ti will be in a phase referred to as austenite and, at lower
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`temperatures, in a phase referred to as martensite. In the austenite phase, the Ni-Ti
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`atomic arrangement results in a more rigid material, whereas in the martensite
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`phase, the crystal lattice structure results in a more flexible material. The
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`transformation between austenite and martensite depends principally on
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`temperature, with martensite occurring below
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`the alloy’s
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`transformation
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`temperatures and austenite occurring above them.
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`27. These transformation temperatures include:
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` martensite start (Ms): the temperature at which a transformation to
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`martensite begins during cooling
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` martensite finish (Mf): the temperature at which the transformation to
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`martensite is complete
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` austenite start (As): the temperature at which a transformation to
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`austenite begins during heating
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` austenite finish (Af): the temperature at which the transformation to
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`austenite is complete
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`28. When Ni-Ti is in the martensite phase at ambient temperatures, it
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`exhibits shape memory. That is, it can be deformed and will retain its deformed
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`shape, rather than springing back to its original state. To a point, this deformation
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`will result from small shifts of the atoms within the crystal lattice rather than the
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`slippage over longer distances associated with permanent (or plastic) deformation.
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`Heating the Ni-Ti above its transformation temperature will cause the martensite to
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`become austenite, and return to its original shape.
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`29. When ambient
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`temperature
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`is higher
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`than
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`the material’s
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`transformation temperature, Ni-Ti is stable as austenite rather than martensite.
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`However, a sufficient applied stress will transform the austenite phase into a more
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`18
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`flexible but meta-stable martensite phase despite being above its transformation
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`temperature, allowing considerable recoverable deformation. When the stress is
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`released, the Ni-Ti reverts quickly to the austenite phase, returning the object to its
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`previous shape. This is superelasticity.
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`30. By 2004, it was well known in the art that heat-treating Ni-Ti alloys
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`(that is, subjecting them to a controlled high temperature for a controlled time in
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`order to alter their properties) could change their transformation temperatures.
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`Pelton, for example, showed that heat-treating a particular Ni-Ti alloy with an Af
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`temperature of 11°C would change the Af to anywhere within a range of about 3°C
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`to 61°C, depending on the time and temperature used. See Ex. 1006 (Pelton) at
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`112-15. Ariola also disclosed a method of selectively altering the Af temperature of
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`different portions of a Ni-Ti catheter tube by subjecting them to a 450-550°C salt
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`bath for different amounts of time. See Ex. 1007 (Ariola) at 4:64-5:35.
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`31. The applicant relied on these characteristics of Ni-Ti to distinguish his
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`invention during prosecution. For example, in response to an enablement rejection,
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`applicant Luebke submitted a declaration in which he “conducted a study to show
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`that endodontic instruments heat treated at 375°C will have an angle greater than
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`10 degrees of permanent deformation after torque at 45° of flexion when tested in
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`accordance with ISO Standard 3630-1.” Ex. 1003 (’991 patent prosecution history)
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`at 126. This did not involve actually performing a flexion test under ISO 3630-1.
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`Instead, the applicant “used differential scanning calorimetry (DSC) on [the] heat-
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`treated endodontic instruments to determine the phase of [the] heat treated
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`endodontic instruments.” Id. DSC is a technique for measuring the amount of heat
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`absorbed (or released) by a material as its temperature increases (or decreases).
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`This can be used to determine the transformation temperatures of nickel-titanium
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`alloys. Here, the DSC tests upon which applicant relied showed that “the
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`endodontic instruments were in the martensitic phase.” Id. at 127. In particular, the
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`DSC tests showed an Af temperature above 37°C, as evidenced by the right
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`edge/tangent of the peaks being to the right of that temperature on the x-axis. Id. at
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`130-32. Luebke distinguished his invention from superelastic orthodontic wire,
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`stating, “The Af temperature of the orthodontic wire is usually in the range of 25°C
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`and hence the activation of the SMA [shape memory alloy] movement or force. In
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`the instance of the present patent application, I am attempting to create a
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`martensitic alloy (instrument or device) that is not activated … at mouth
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`temperature (37°C) but still displays permanent deformation at 37°C.” Id. at 129.
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`In other words, applicant’s invention is intended to create a Ni-Ti instrument with
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`an Af temperature above 37°C.
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`32.
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` The applicant also relied on the microcrystalline properties of Ni-Ti
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`during prosecution of a patent in the same family of the ’991 patent, U.S. Patent
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`No. 8,727,773 (“the ’773 patent”). The applicant submitted sixteen pages of notes
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`20
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`in an attempt to distinguish his invention from U.S. Patent Application Publication
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`No. 2005/0090844 A1 (Patel). See Ex. 1008 (’773 patent prosecution history) at
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`144-60. Per the applicant, “Applicant has provided evidence and can provide
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`further evidence that the subject matter of Patel does not possess the flexion test
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`properties recited in claim 1.” Id. at 145. The applicant agreed that the flexion test
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`itself “is only referred to inferentially,” that is, it does not need to be expressly
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`disclosed by the prior art reference. Id. Therefore, the question was whether Patel’s
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`material would possess the property described by the “wherein” clause. The
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`applicant asserted that Patel’s material did not, because it was superelastic. See id.
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`at 146.
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`33.
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` A major focus of the applicant’s notes was the difference between
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`austenite and martensite, and the temperature(s) at which Ni-Ti transforms from
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`one to the other. According to the applicant, the essence of his invention was that
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`the file resulting from heat-treatment had an austenite finish temperature greater
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`than body temperature, which is 37°C. See, e.g., id. at 147, 151-52, 159. As a
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`result, the material would exhibit non-superelastic properties during clinical use.
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`He thereby distinguished the superelastic characteristic of Patel’s wire, which
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`preferably had an austenite finish temperature lower than body temperature, about
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`26-36°C. See id. at 147. These notes demonstrate Luebke’s understanding that, if
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`the austenite finish temperature of the endodontic instrument is raised above 37°C,
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`21
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`the instrument will possess the property embodied by the “wherein” clause of the
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`claims of the ’991 patent.
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`34. The alleged invention of the ’991 patent is to increase the
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`transformation temperature (Af temperature) so that a Ni-Ti endodontic file, under
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`conditions of use (i.e., at mouth temperature), is in the martensite phase rather than
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`the austenite phase so that the file can be permanently deformed in use.
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`35. The specification of the ’991 patent seems to confound the term
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`“shape memory” with superelasticity. E.g., Ex. 1001 (’991 patent) at 8:59-62.
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`However, where “shape memory” is used in the prosecution history, it ge