`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: IPR2015-00632
`U.S. Patent No. 8,727,773
`____________________
`
`
`DECLARATION OF A. JON GOLDBERG
`
`
`
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`
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`
`
`
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`
`
`
`IPR2015-00632 – Ex. 1002
`US Endodontics, LLC, Petitioner
`1
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`

`

`EXHIBIT LIST
`
`
`Exhibit #
`1001
`
`Exhibit Description
`U.S. Patent No. 8,727,773 B2 (the “’773 patent”)
`
`1002
`
`1003
`
`1004
`
`1005
`
`1006
`
`1007
`
`1008
`
`1009
`
`1010
`
`1011
`
`1012
`
`1013
`
`1014
`
`Declaration of A. Jon Goldberg
`Harmeet Walia et al., An Initial Investigation of the Bending and Tor-
`sional Properties of Nitinol Root Canal Files, 14 J. ENDODONTICS
`346 (1988) (“Walia”)
`Fujio Miura et al., The super-elastic property of the Japanese NiTi alloy
`wire for use in orthodontics, 90 AM. J. ORTHODONTICS & DENTOFA-
`CIAL ORTHOPEDICS 1 (1986) (“Miura”)
`
`Satish B. Alapati, “An investigation of phase transformation
`mechanisms for nickel-titanium rotary endodontic instruments,”
`PhD thesis, 2006. (“Alapati”)
`
`Alan R. Pelton et al., Optimisation of Processing and Properties
`of Medical-Grade Nitinol Wire, 9 Minimally Invasive Therapies
`& Allied Techs. 107 (2000) (“Pelton”);
`
`U.S. Patent No. 5,697,906 to Ariola et al.
`
`Prosecution history of the ’773 patent
`
`Prosecution history of U.S. Patent No. 8,062,033
`
`Prosecution history of U.S. Patent No. 8,562,341
`
`US. Provisional Patent Application No. 60/578,091
`
`U.S. Patent Application Publication No. 2008/0032260 A1,
`Luebke (“Luebke 2008”)
`
`Prosecution history of U.S. Patent No. 8,083,873
`
`U.S. Patent Application Publication No. 2011/0271529 A1, Gao
`et al. (“Gao”)
`
`
`
`
`
`2
`
`

`

`1015
`
`1016
`
`1017
`
`1018
`
`1019
`
`1020
`
`1021
`
`1022
`
`1023
`
`1024
`
`1025
`
`1026
`
`1027
`
`U.S. Provisional Patent Application No. 61/332,954
`International Standard ISO 3630-1, 1st ed. (1992)
`International Standard ISO 3630-1, 2nd ed. (2008)
`Salwa E. Khier et al., Bending properties of superelastic and nonsupere-
`lastic nickel-titanium orthodontic wires, 99 AM. J. ORTHODONTICS &
`DENTOFACIAL ORTHOPEDICS 310 (1991) (“Khier”)
`Grégoire Kuhn & Laurence Jordan, Fatigue and Mechanical Proper-
`ties of Nickel-Titanium Endodontic Instruments, 28 J. ENDODONTICS
`716 (2002) (“Kuhn”)
`
`U.S. Patent No. 5,628,674 to Heath et al.
`Edgar Schäfer et al., Bending properties of rotary nickel-titanium in-
`struments, 96 ORAL SURGERY ORAL MEDICINE ORAL PATHOLO-
`GY 757 (2003)
`
`U.S. Patent App. Pub. No. 2002/0137008 A1, McSpadden et al.
`(“McSpadden”)
`
`U.S. Patent No. 7,713,815 B2 to Matsutani et al. (“Matsutani”)
`S. Miyazaki et al., Characteristics of Deformation and Transformation
`Pseudoelasticity in Ti-Ti Alloys, 43 J. PHYSIQUE COLLOQUES C4-
`255 (1982) (“Miyazaki”)
`
`Franklin S. Weine, ENDODONTIC THERAPY, 6th Ed., 2004,
`Chapter 5 (“Weine”)
`
`Japanese Unexamined Patent Application Publication No. 2006-
`149675, Matsutani et al.
`
`English translation of Japanese Unexamined Patent Application
`Publication No. 2006-149675, Matsutani et al.
`
`
`
`
`3
`
`
`
`
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`

`

`Table of Contents
`
`B.
`
`
`I.
`Background and Qualifications ................................................................................. 7
`Assignment and Materials Reviewed ........................................................................ 8
`II.
`III. Overview of the ’773 Patent .................................................................................... 11
`IV. Claims of the ’773 Patent ......................................................................................... 13
`V.
`Scientific and Technological Background .............................................................. 16
`VI. Claim Construction ................................................................................................... 21
`A.
`“heat-treating the entire shank” / “heat-treating the entire
`instrument shank” ............................................................................................... 21
`“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” ................................................................................................. 21
`“permanent deformation” .................................................................................. 22
`C.
`“diameter” ............................................................................................................ 22
`D.
`VII. Written Description in Prior Applications............................................................. 22
`A.
`Standard Applied ................................................................................................. 23
`B.
`Applications in the Priority Chain of the ’773 Patent..................................... 23
`C.
`Earlier Applications Do Not Support Heat Treatment in an
`Unreactive Atmosphere ...................................................................................... 24
`VIII. Standards Applied ..................................................................................................... 30
`IX. Patentability Analysis ................................................................................................ 32
`A.
`Level of Skill in the Art ...................................................................................... 32
`B.
`Scope and Content of the Prior Art ................................................................. 32
`i. Overview of Gao ................................................................................................. 34
`ii.
`Overview of ISO 3630-1 .............................................................................. 34
`iii. Overview of Khier ........................................................................................ 34
`iv. Overview of Luebke 2008 ............................................................................ 35
`v.
`Overview of Kuhn ........................................................................................ 35
`vi. Overview of McSpadden .............................................................................. 35
`
`
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`4
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`

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`C.
`
`D.
`
`vii. Overview of Pelton ....................................................................................... 36
`viii. Overview of Weine ....................................................................................... 38
`ix. Overview of Walia ......................................................................................... 38
`x.
`Overview of Miyazaki ................................................................................... 39
`xi. Overview of Matsutani ................................................................................. 43
`Anticipation by Luebke 2008 ............................................................................. 45
`i. Anticipation of claim 1 ....................................................................................... 45
`ii.
`Anticipation of claim 13 ............................................................................... 47
`iii.
`Anticipation of claims 2, 9-11, and 15 ........................................................ 48
`iv.
`Anticipation of claims 3 and 14 ................................................................... 48
`v.
`Anticipation of claims 4, 5, and 16 .............................................................. 48
`vi.
`Anticipation of claim 8 ................................................................................. 49
`vii. Anticipation of claims 12 and 17 ................................................................. 49
`viii. Anticipation of claims 6 and 7 ..................................................................... 49
`Anticipation by Gao; Obviousness in View of Gao and ISO
`3630-1 ................................................................................................................... 50
`i. Anticipation of claim 1 ....................................................................................... 50
`ii.
`Obviousness of claim 13 .............................................................................. 54
`iii.
`Anticipation of claims 2 and 9-11; obviousness of claim 15.................... 55
`iv.
`Anticipation of claim 3; obviousness of claim 14 ..................................... 55
`v.
`Anticipation of claims 4 and 5; obviousness of claim 16 ......................... 56
`vi. Obviousness of claim 8 ................................................................................ 56
`vii. Anticipation of claim 12; obviousness of claim 17 ................................... 57
`viii. Anticipation of claims 6 and 7 ..................................................................... 57
`E. Obviousness in View of Gao, ISO 3630-1, and Khier ................................... 58
`F.
`Anticipation by Kuhn; Obviousness in View of Kuhn and ISO
`3630-1 ................................................................................................................... 59
`i. Anticipation of claim 1 ....................................................................................... 59
`ii.
`Obviousness of Claim 13 ............................................................................. 64
`iii. Obviousness of claim 8 ................................................................................ 65
`iv.
`Anticipation of claims 4 and 5; obviousness of claim 16 ......................... 66
`
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`5
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`I.
`
`v.
`Anticipation of claims 2 and 9-11; obviousness of claim 15.................... 66
`Anticipation of Claim 12; Obviousness of Claim 17 ................................ 67
`vi.
`G. Obviousness in View of Kuhn, ISO 3630-1, McSpadden, and
`Pelton .................................................................................................................... 68
`i. Obviousness of claims 1-17 ............................................................................... 68
`H. Obviousness in View of Kuhn, ISO 3630-1, and Khier; and/or
`Kuhn, ISO 3630-1, McSpadden, Pelton, and Khier ....................................... 76
`Obviousness in View of McSpadden, Miyazaki, and ISO 3630-
`1 ............................................................................................................................. 77
`i. Obviousness of claim 1 ...................................................................................... 77
`ii.
`Obviousness of claim 13 .............................................................................. 84
`iii. Obviousness of claims 2, 9-11, and 15 ....................................................... 85
`iv. Obviousness of claims 3 and 14 .................................................................. 85
`v.
`Obviousness of claims 4, 5, and 16 ............................................................. 86
`vi. Obviousness of claim 8 ................................................................................ 86
`vii. Obviousness of claims 12 and 17 ................................................................ 87
`viii. Obviousness of claims 6 and 7 .................................................................... 87
`Obviousness in View of Matsutani, Pelton, and ISO 3630-1 ........................ 88
`i. Obviousness of claim 1 ...................................................................................... 88
`ii.
`Obviousness of claim 13 .............................................................................. 95
`iii. Obviousness of claims 2, 9-11, and 15 ....................................................... 96
`iv. Obviousness of claims 3 and 14 .................................................................. 96
`v.
`Obviousness of claims 4, 5, and 16 ............................................................. 97
`vi. Obviousness of claim 8 ................................................................................ 97
`vii. Obviousness of claims 12 and 17 ................................................................ 98
`viii. Obviousness of claims 6 and 7 .................................................................... 98
`K. Obviousness in View of Matsutani, Pelton, ISO 3630-1, and
`Khier ..................................................................................................................... 99
`
`J.
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`6
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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 Den-
`
`tal 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 Dentis-
`
`try, School of Dental Medicine. Since 1995, I have served as the Director of the Cen-
`
`ter for Biomaterials at the University of Connecticut Health Center. I am a founding
`
`member of the Board of Directors of 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 Craniofacial Re-
`
`
`
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`
`7
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`

`

`search, National Institutes of Health. I am an inventor or co-inventor of six U.S. pa-
`
`tents 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 var-
`
`ious dental/endodontic procedures (U.S. Pat. No. 4,894,012).
`
`4.
`
`I teach a variety of courses on materials engineering and materials sci-
`
`ence 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 appli-
`
`cations, biocatalyzed mineralization and use of high performance polyphenylene pol-
`
`ymers in orthodontics.
`
`5.
`
`I have supervised the research of engineering and dental graduate stu-
`
`dents. 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).
`
`II. ASSIGNMENT AND MATERIALS REVIEWED
`
`8.
`
`I submit this declaration in support of US Endodontics, LLC’s (“US
`
`Endo’s”) petition for inter partes review of U.S. Patent No. 8,727,773 (“the ’773 pa-
`
`tent”).
`
`
`
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`
`8
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`

`

`9.
`
`10.
`
`I am not an employee of US Endo or any affiliate or subsidiary thereof.
`
`I am being compensated for my work in connection with this case 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 US Endo’s petition for inter partes re-
`
`view (or the outcome of the inter partes review, if trial is instituted).
`
`12.
`
`I have been asked to provide certain opinions relating to the patentability
`
`of the ’773 patent. Specifically, I have been asked to provide my opinion regarding
`
`(i) the level of ordinary skill in the art to which the ’773 patent pertains; (ii) whether
`
`the claims are entitled to a priority date earlier than the filing date of the ’773 patent;
`
`and (iii) whether claims 1-17 are anticipated by, or would have been obvious over, cer-
`
`tain prior art references.
`
`13. The opinions expressed in this declaration are not exhaustive of my
`
`opinions on the patentability of claims 1-17. Therefore, the fact that I do not address
`
`a particular point should not be understood to indicate any opinion on my part that
`
`any claim otherwise complies with the patentability requirements.
`
`14.
`
`In forming my opinions, I have reviewed the ’773 patent, its prosecution
`
`history, and certain prior art to the ’773 patent including:
`
`a) S. Miyazaki et al., Characteristics of Deformation and Transformation Pseudoelas-
`
`ticity in Ti-Ti Alloys, 43 J. PHYSIQUE COLLOQUES C4-255 (1982) (“Miya-
`
`zaki”)
`
`
`
`
`
`9
`
`

`

`b) Fujio Miura et al., The super-elastic property of the Japanese NiTi alloy wire for
`
`use in orthodontics, 90 AM. J. ORTHODONTICS & DENTOFACIAL ORTHOPE-
`
`DICS 1 (1986) (“Miura”);
`
`c) Salwa E. Khier et al., Bending properties of superelastic and nonsuperelastic nickel-
`
`titanium orthodontic wires, 99 AM. J. ORTHODONTICS & DENTOFACIAL OR-
`
`THOPEDICS 310 (1991) (“Khier”);
`
`d) Harmeet Walia et al., An Initial Investigation of the Bending and Torsional Prop-
`
`erties of Nitinol Root Canal Files, 14 J. ENDODONTICS 346 (1988) (“Walia”);
`
`e) International Standard ISO 3630-1, 1st ed. (1992) and 2nd ed. (2008);
`
`f) F.X. Gil et al., Relevant aspects in the clinical applications of NiTi shape memory
`
`alloys, 7 J. MATERIALS SCI.: MATERIALS MED. 403 (1996) (“Gil”);
`
`g) U.S. Patent No. 5,628,674 to Heath et al.;
`
`h) Alan R. Pelton et al., Optimisation of Processing and Properties of Medical-Grade
`
`Nitinol Wire, MINIMALLY INVASIVE THERAPIES & ALLIED TECHS. 107
`
`(2000) (“Pelton”);
`
`i) Grégoire Kuhn & Laurence Jordan, Fatigue and Mechanical Properties of
`
`Nickel-Titanium Endodontic Instruments, 28 J. ENDODONTICS 716 (2002)
`
`(“Kuhn”);
`
`j) U.S. Patent App. Pub. No. 2002/0137008 A1, McSpadden et al.
`
`(“McSpadden”);
`
`
`
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`10
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`

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`k) Franklin S. Weine, ENDODONTIC THERAPY, 6th Ed., 2004, Chapter 5
`
`(“Weine”);
`
`l) Satish B. Alapati, “An investigation of phase transformation mechanisms
`
`for nickel-titanium rotary endodontic instruments,” PhD thesis, 2006.
`
`(“Alapati”).
`
`m) Japanese Unexamined Patent Application No. 2006-149675, Matsutani
`
`et al. (English translation);
`
`n) U.S. Patent No. 7,713,815 B2 to Matsutani et al.;
`
`o) U.S. Patent App. Pub. No. 2008/0032260 A1, Luebke (“Luebke 2008”);
`
`p) U.S. Provisional Patent App. No. 61/332,954; and
`
`q) U.S. Patent App. Pub. No. 2011/0271529 A1, Gao et al. (“Gao”);
`
`I have also reviewed and am familiar with any other patents and publications dis-
`
`cussed below.
`
`III. OVERVIEW OF THE ’773 PATENT
`
`15. The ’773 patent is entitled “Dental and Medical Instruments Comprising
`
`Titanium” and names Neill Hamilton Luebke as its sole inventor. On its face, the pa-
`
`tent issued May 20, 2014 from an application filed April 25, 2012. It claims priority to
`
`numerous applications, the earliest of which is provisional application number
`
`60/578,091, filed June 8, 2004.
`
`16. The specification of the ’773 patent broadly describes the use of titanium
`
`alloys to make endodontic instruments. It broadly, and briefly, covers numerous top-
`
`
`
`
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`11
`
`

`

`ics, such as the shape of the instrument (a ubiquitous one), a host of different titani-
`
`um alloys that may be used, heat treatment very generally, and (in most detail) coating
`
`of the instruments. Little emphasis is given to heat treatment of endodontic files apart
`
`from five “Examples.”
`
`17. Each of the five Examples set forth in the specification involves samples
`
`of nickel titanium endodontic files, in six sizes. One group of nickel titanium 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 un-
`
`treated. In this sense, each example is identical. The only difference is that each exam-
`
`ple involves performing a different test on the three groups of instruments: two tor-
`
`sion (twisting) tests, two bending tests, and a fatigue test. According to the ’773 pa-
`
`tent, the heat treated group showed the best performance in all five 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 at 9:19-23.
`
`18. The claims of the ’773 patent are generally directed to one of these ex-
`
`amples, but include a range of temperatures and atmospheric conditions for the heat
`
`treatment, not just the one temperature and atmosphere disclosed in the example. In
`
`particular, the claims are methods that include providing endodontic files made from
`
`a superelastic nickel titanium alloy and heat treating them at a temperature of at least
`
`400°C, but below the melting point of the alloy. Per the claims, the result is supposed
`
`
`
`
`
`12
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`

`

`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 ’773 PATENT
`
`19. The ’773 patent includes 17 claims. Claims 1 and 13 are independent,
`
`and the rest dependent.
`
`20.
`
`I understand that US Endo is challenging all 17 claims of the ’773 patent.
`
`They are reproduced below for reference:
`
`1. 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 from 400° 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 torque at
`45 degrees of flexion when tested in accordance with
`ISO Standard 3630-1.
`
`2. The method of claim 1 wherein:
`the temperature is from 475° C. to 525° C.
`
`3. The method of claim 1 wherein:
`the shank is heat-treated for 1 to 2 hours.
`
`4. The method of claim 1 wherein:
`step (b) is performed in any atmosphere.
`
`
`
`
`
`13
`
`

`

`5. The method of claim 4 wherein:
`the atmosphere is unreactive, ambient or any other
`acceptable heat treatment process.
`
`6. The method of claim 4 wherein:
`the atmosphere is unreactive, ambient or any other
`acceptable heat treatment process,
`the temperature is from 475° C. to 525° C., and
`the shank is heat-treated for 1 to 2 hours.
`
`7. The method of claim 4 wherein:
`the instrument shank consists essentially of a superelastic
`nickel titanium alloy comprising 54-57 weight percent
`nickel and 43-46 weight percent titanium,
`the temperature is 500° C., and
`the shank is heat-treated for 1 to 2 hours.
`
`8. The method of claim 1 wherein:
`the instrument shank has a diameter of 0.5 to 1.6
`millimeters.
`
`9. The method of claim 1 wherein:
`the instrument shank is heat-treated in step (b) at a single
`temperature.
`
`10. The method of claim 9 wherein:
`the single temperature is from 400° C. to 525° C.
`
`11. The method of claim 10 wherein:
`the single temperature is from 475° C. to 525° C.
`
`12. The method of claim 1 wherein:
`the superelastic nickel titanium alloy comprises 54-57
`weight percent nickel and 43-46 weight percent
`titanium.
`
`
`
`
`
`14
`
`

`

`13. 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 helical flutes
`defining a cutting edge extending from a distal end of
`the shank along an axial length of the shank, the
`instrument being in accordance with ISO Standard
`3630-1, the shank consisting essentially of a
`superelastic nickel titanium alloy; and
`(b) after step (a), heat-treating the entire instrument
`shank at a temperature from 475° C. to 525° C.,
`wherein the heat-treated shank has an angle greater than
`10 degrees of permanent deformation after torque at
`45° of flexion tested in accordance with ISO Standard
`3630-1.
`
`14. The method of claim 13 wherein:
`the shank is heat-treated for 1 to 2 hours.
`
`15. The method of claim 13 wherein:
`the instrument shank is heat-treated in step (b) at a single
`temperature.
`
`16. The method of claim 13 wherein:
`step (b) is performed in an atmosphere that is unreactive,
`ambient or any other acceptable heat treatment
`process.
`
`17. The method of claim 13 wherein:
`the superelastic nickel titanium alloy comprises 54-57
`weight percent nickel and 43-46 weight percent
`titanium.
`
`
`
`
`
`
`
`15
`
`

`

`21. As can be seen, each claim has the same “wherein” clause, either directly
`
`or by dependency. Dependent claims recite limitations directed to alloy composition,
`
`treatment temperature, treatment time, and treatment atmosphere.
`
`V.
`
`SCIENTIFIC AND TECHNOLOGICAL BACKGROUND
`
`22.
`
`I have been asked to provide a brief scientific and technological back-
`
`ground regarding nickel titanium and its use in endodontic instruments.
`
`23. Endodontic therapy is commonly known as a “root canal” procedure,
`
`and it involves drilling through the hard outer portion of a tooth and removing dis-
`
`eased tissue (pulp) from the inside of the tooth. A small-diameter file is needed to re-
`
`move the tissue from the tooth’s root(s), i.e., the parts that anchor the tooth in the
`
`gums. This thin file is the endodontic instrument to which the ’773 patent pertains.
`
`24.
`
`For many years, endodontic instruments were typically made of steel,
`
`usually stainless steel.
`
`25. The nickel titanium alloys (which I will refer to as “Ni-Ti”) described
`
`and claimed by the ’773 patent were first discovered in the 1960’s, and their use in en-
`
`dodontics was first disclosed as early as 1988 by Walia et al. Properties including flexi-
`
`bility, 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 pur-
`
`pose.
`
`26. The ’773 patent does not describe the superelastic or shape memory
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`properties, or microscopic structure of Ni-Ti, in any detail. However, the applicant
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`did rely on such characteristics during prosecution to distinguish the prior art. There-
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`fore, I will provide a basic overview.
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`27. When appropriately processed, Ni-Ti can exhibit both superelasticity (al-
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`so known as pseudoelasticity) and shape memory. Superelasticity means that the mate-
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`rial is relatively rigid until a threshold stress is applied to it; above that threshold, the
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`material becomes considerably more flexible. When the stress is removed, the material
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`reverts to its original shape. A shape memory material is one that is flexible and does
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`not revert to its original shape immediately after it is deformed. However, when the
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`material is heated past a certain temperature, it then reverts to its pre-deformation
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`shape, even though it held its deformed shape prior to heating. In other words, it
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`“remembers” its original shape.
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`28. These properties result from the microscopic structure of Ni-Ti. Nickel
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`titanium alloys are crystalline, meaning the material’s atoms have a well-defined crystal
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`structure. Changes in temperature or stress can impact the crystal structure, resulting
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`in different “phases.” Various properties of nickel titanium depend in part on the
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`crystalline phases that are present in the material. In general, at higher temperatures,
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`nickel titanium will be in a phase referred to as austenite and, at lower temperatures, in
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`a phase referred to as martensite. In the austenite phase, the nickel titanium atomic
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`arrangement results in a more rigid material, whereas in the martensite phase, the crys-
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`tal lattice structure results in a more flexible material. The transformation between
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`austenite and martensite depends principally on temperature, with martensite occur-
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`ring below the alloy’s transformation temperatures and austenite occurring above
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`them.
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`29. These transformation temperatures include:
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`• martensite start (Ms): the temperature at which a transformation to mar-
`tensite begins during cooling
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`• martensite finish (Mf): the temperature at which the transformation to
`martensite is complete
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`• austenite start (As): the temperature at which a transformation to austen-
`ite begins during heating
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`• austenite finish (Af): the temperature at which the transformation to
`austenite is complete
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`30. When Ni-Ti is in the martensite phase at ambient temperatures, it exhib-
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`its shape memory. That is, it can be deformed and will retain its deformed shape, ra-
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`ther than springing back to its original state. To a point, this deformation will result
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`from small shifts of the atoms within the crystal lattice rather than the slippage over
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`longer distances associated with permanent (or plastic) deformation. Heating the Ni-
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`Ti above its transformation temperature will cause the martensite to become austen-
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`ite, and return to its original shape.
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`31. When ambient temperature is higher than the material’s transformation
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`temperature, Ni-Ti is stable as austenite rather than martensite. However, a sufficient
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`applied stress will transform the austenite phase into a more flexible but meta-stable
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`martensite phase despite being above its transformation temperature, allowing consid-
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`erably more deformation. When the stress is released, the Ni-Ti reverts quickly to the
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`austenite phase, returning the object to its previous shape. This is superelasticity.
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`32. By 2004, it was well known in the art that heat-treating nickel titanium
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`alloys (that is, subjecting them to a controlled high temperature for a controlled time
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`in order to alter their properties) could change their transformation temperatures. Pel-
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`ton et al., 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 to
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`61°C, depending on the time and temperature used. See Ex. 1006 (Pelton) at 112-14.
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`Ariola et al. also disclosed a method of selectively altering the Af temperature of dif-
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`ferent portions of a nickel titanium catheter tube by subjecting them to a 450-550°C
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`salt bath for different amounts of time. See Ex. 1007 (Ariola) at 4:64-5:35.
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`33. As briefly mentioned above, the applicant relied on these characteristics
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`of Ni-Ti to distinguish his invention during prosecution. In particular, the applicant
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`submitted sixteen pages of notes, the purpose of which was to distinguish U.S. Patent
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`Application Publication No. 2005/0090844 A1 (Patel et al.). See Ex. 1008 (’773 patent
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`prosecution history) at 144-60. Per the applicant, “Applicant has provided evidence
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`and can provide further evidence that the subject matter of Patel does not possess the
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`flexion test properties recited in claim 1.” Id. at 145. The applicant agreed that the
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`flexion test itself “is only referred to inferentially,” that is, it does not need to be ex-
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`pressly disclosed by the prior art reference. Id. Therefore, the question was whether
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`Patel’s 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. at
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`146.
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`34.
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` A major focus of the applicant’s notes was the difference between aus-
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`tenite and martensite, and the temperature(s) at which Ni-Ti transforms from one to
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`the other. According to Dr. Luebke, the applicant, the essence of his invention was
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`that 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., Ex. 1008 (’773 patent prosecution his-
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`tory) at 147, 151-52, 159. As a result, the material would exhibit non-superelastic
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`properties during clinical use. He thereby distinguished the superelastic characteristic
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`of Patel’s wire, which preferably had an austenite finish tempe