PTO/SB/16 (1 0-05)
`Approved for use through 07/31/2006. OMB 0651-0032
`U.S. Patent and Trademark Office; U.S. DEPARTMENT OF COMMERCE
`Under the Paperwork Reduction Act of 1995, no persons are required to respond to a collection of information unless it displays a valid OMB control number.
`PROVISIONAL APPLICATION FOR PATENT COVER SHEET- Page 1 of 2
`This is a request for filing a PROVISIONAL APPLICATION FOR PATENT under 37 CFR 1.53(c).
`Express Mail Label No
`
`Given Name (first and middle [if any])
`
`INVENTOR(S)
`Family Name or Surname
`
`Yong
`
`Randall
`
`Gao
`
`Maxwell
`
`Residence
`(City and either State or Foreign Country)
`
`Broken Arrow, OK 74012
`
`Broken Arrow, OK 74011
`
`separately numbered sheets attached hereto
`Additional inventors are being named on the
`TITLE OF THE INVENTION (500 characters max):
`
`ENDODONTIC ROTARY INSTRUMENTS MADE OF SHAPE MEMORY ALLOYS IN THEIR
`MARTENSITIC STATE AND MANUFACTURING METHODS
`
`Direct all correspondence to:
`
`CORRESPONDENCE ADDRESS
`
`D The address corresponding to Customer Number:
`I
`OR
`lZl ~~~i~~al Name David A. Zdurne, DENTSPL Y International Inc.
`
`I
`
`Address 570 West College Aveunue
`P.O. Box 872
`
`City
`York
`Country us
`
`[{]Application Data Sheet. See 37 CFR 1.76
`
`[{] Specification Number of Pages 25
`
`Zip 17 405-0872
`
`State PA
`Telephone 717-849-4461
`Email
`david.zdurne@dentsolv.com
`ENCLOSED APPLICATION PARTS (check all that apply)
`D CD(s), Number of COs
`D Other (specify)
`
`D Drawing(s) Number of Sheets
`Fees Due: Filing Fee of $200 ($1 00 for small entity). If the specification and drawings exceed 100 sheets of paper, an application size fee is
`also due, which is $250 ($125 for small entity) for each additional 50 sheets or fraction thereof. See 35 U.S.C. 41(a)(1)(G) and 37 CFR 1.16(s).
`
`METHOD OF PAYMENT OF THE FILING FEE AND APPLICATION SIZE FEE FOR THIS PROVISIONAL APPLICATION FOR PATENT
`
`Applicant claims small entity status. See 37 CFR 1.27.
`
`D
`D A check or money order is enclosed to cover the filing fee and application size fee (if applicable).
`D Payment by credit card. Form PT0-2038 is attached
`lZl The Director is hereby authorized to charge the filing fee and application size fee (if applicable) or credit any overpayment to Deposit
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`I
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`$220.00
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`I
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`TOTAL FEE AMOUNT($)
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`A duplicative copy of this form is enclosed for fee processing.
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`USE ONLY FOR FILING A PROVISIONAL APPLICATION FOR PATENT
`This collection of information is required by 37 CFR 1.51. The information is required to obtain or retain a benefit by the public which is to file (and by the USPTO
`to process) an application. Confidentiality is governed by 35 U.S.C. 122 and 37 CFR 1.11 and 1.14. This collection is estimated to take 8 hours to complete,
`including gathertng, preparing, and submitting the completed application form to the USPTO. Time will vary depending upon the individual case. Any comments
`on the amount of time you require to complete this form and/or suggestions for reducing this burden, should be sent to the Chief Information Officer, U.S. Patent
`and Trademark Office, U.S. Department of Commerce, P.O. Box 1450, Alexandria, VA 22313-1450. DO NOT SEND FEES OR COMPLETED FORMS TO THIS
`ADDRESS. SEND TO: Commissioner for Patents, P.O. Box 1450, Alexandria, VA 22313-1450.
`If you need assistance in completing the form, ca/11-800-PT0-9199 and select option 2.
`
`1 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`PROVISIONAL APPLICATION COVER SHEET
`Page 2 of2
`
`PTO/SB/16 (10-05)
`Approved for use through 07/31/2006. OMB 0651-0032
`U.S. Patent and Trademark Office; U.S. DEPARTMENT OF COMMERCE
`Under the Paperwork Reduction Act of 1995, no persons are required to respond to a collection of information unless it displays a valid OMB control number.
`
`The invention was made by an agency of the United States Government or under a contract with an agency of the United States Government.
`[{]
`D No.
`
`Yes, the name of the U.S. Government agency and the Government contract number a re : - - - - - - - - - - - - - -
`
`WARNING:
`Petitioner/applicant is cautioned to avoid submitting personal information in documents filed in a patent application that may
`contribute to identity theft. Personal information such as social security numbers, bank account numbers, or credit card
`numbers (other than a check or credit card authorization form PT0-2038 submitted for payment purposes) is never required by
`the USPTO to support a petition or an application. If this type of personal information is included in documents submitted to
`the USPTO, petitioners/applicants should consider redacting such personal information from the documents before submitting
`them to the USPTO. Petitioner/applicant is advised that the record of a patent application is available to the public after
`ublication request in compliance with 37 CFR 1.213(a) is made in the application)
`publication ofthe application (unless a no
`or issuance of a patent. Furthermore,
`record from an abandoned application may also be available to the public if the
`·
`li
`application is referenc
`application or an issued patent (see 37 CFR 1.14). Checks and credit card
`authorization for
`T0-2038 su
`d for payment purposes are not retained in the application file and therefore are not
`publicly av ·
`
`SIGN
`
`Date May 10, 2010
`
`TYPEDorPRINTEDNAME~D~av~i~d~A~.Z=d~u~r~ne~--------------- REGISTRATION NO. 5""8""6_,30::...._ ____ _
`(if appropriate)
`
`TELEPHONE 717-849-4461
`
`Docket Number: ...!T..=U~L~-2=2""9A~----------
`
`2 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket No: DPD-7336-2
`
`IN THE UNITED STATES PATENT AND TRADEMARK OFFICE
`
`In re application of: Y ong Gao et al.
`
`Application No:
`
`Filed: HEREWITH
`
`Group Art Unit:
`
`Examiner:
`
`For: ENDODONTIC ROTARY INSTRUMENTS MADE OF SHAPE MEMORY ALLOYS
`IN THEIR MARTENSITIC STATE AND MANUFACTURING METHODS
`
`Commissioner for Patents
`P.O. Box 1450
`Alexandria, VA 22313-1450
`
`1. Applicant Information
`
`APPLICATION DATA SHEET
`
`First Applicant:
`Mailing Address:
`
`Residence:
`Citizenship:
`
`Second Applicant:
`Mailing Address:
`
`Residence:
`Citizenship:
`
`YongGao
`323 N. Butternut Avenue
`Broken Arrow, OK 74012
`us
`Same
`P.R. China
`
`Randall Maxwell
`12945 S. 124 E Avenue
`Broken Arrow, OK 74011
`us
`Same
`us
`
`2. Correspondence Information
`
`CoiTespondence for this application should be addressed to:
`IZI Name: David A. Zdume
`
`Address:
`
`DENTSPL Y International Inc.
`570 West College A venue
`P.O. Box 872
`York, PA 17405-0872
`
`- 1 -
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`US ENDODONTICS, LLC., Petitioner
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`

`

`Attorney Docket No: DPD-7336-2
`
`rg] Customer No: 23439
`
`3. Application Information
`
`Title of Invention: ENDODONTIC ROTARY INSTRUMENTS MADE OF SHAPE
`MEMORY ALLOYS IN THEIR MARTENSITIC STATE AND
`MANUFACTURING METHODS
`
`Docket number assigned to this application: TUL-229A
`Suggested Classification:
`C l a s s : - - - - - - - - - - - - - - - (cid:173)
`Technology Center:
`Total number of drawing sheets: 0 - - -
`0 Suggested drawing figure for publication:
`0 Application is not being published.
`
`- - -
`
`Subclass: - - - - - - - - -
`
`Type of Application:
`0 Utility Application
`0 Design Application
`rg] Provisional Application
`0 Reissue Application
`0 Plant Application
`
`Genus: ----------------
`Denomination:-------------
`0 This Application discloses a significant part of the subject matter of an application
`which is under a secrecy order pursuant to §37 CFR 5.2.
`
`Species: -----------
`
`4. Representative Information
`
`The following have a power of attorney or authorization of agent in this Application
`
`0 Name of attorney ( ag en t ) : - - - - - - - - - - - - - - - - - - - - -
`
`rg] Customer No: 23439
`
`-2-
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`4 of 39
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`US ENDODONTICS, LLC., Petitioner
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`Attorney Docket No: DPD-7336-2
`
`5. Domestic Priority Information
`
`Domestic priority for this application is claimed as
`IZI No domestic priority is claimed.
`0
`
`35 U.S.C. §119(e)
`
`Application No: -----------------------------------------------------
`Filed: ----------------------------------------------------------
`Starns: ----------------------------------------------------------(cid:173)
`Relmionship:-------------------------------------------------------
`D 35 u.s. c. §120
`Application No: -------------------------------------------------
`Filed: - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
`Starns: ----------------------------------------------------------
`Relationship: -------------------------------------------------------
`
`U.S. Application
`Number
`
`Date of Filing
`(day, month, year)
`
`Status
`(patented, pending, abandoned)
`
`D 35 U.S.C. §121
`Application No: -------------------------------------------------(cid:173)
`Filed: ------------------------------------------------------------
`Starns:. _________________________________________________________ __
`Relationship: -----------------------------------------------------
`0
`35 U.S.C. §365(c)
`Application No: --------------------------------------------------
`Filed:
`-----------------------------------------------------~---
`Starns:. ____________________________________________________ __
`Relationship: --------------------------------------------------
`
`" - .) -
`
`5 of 39
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`US ENDODONTICS, LLC., Petitioner
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`Attorney Docket No: DPD-7336-2
`
`6. Foreign Priority Information
`I:8J No foreign priority is claimed.
`0 Foreign priority is claimed for this application from:
`
`Application No::...._ _________________________ _
`
`Filing D a t e : - - - - - - - - - - - - - - - - - - - - - - - - - - - (cid:173)
`Country:------------------------------------
`0 Foreign application( s) having a filing date before that of the above application for
`which priority is claimed.
`
`Application No: -----------------------------
`Filing D a t e : - - - - - - - - - - - - - - - - - - - - - - - , - - - - - - - - - -
`Coun t ry : - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
`
`7. Assignee Information
`
`The assignee(s) of this application based on filed Assignment papers:
`Name of assignee:
`
`Extent of interest of assignee in application: ----------+r-----------
`Dated: May 10, 2010
`
`Phone: (717)849-4461
`Fax: (717)849-4360
`
`-4-
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`6 of 39
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`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`Endodontic Rotary Instruments made of shape memory alloys in their martensitic state
`
`and manufacturing methods thereof
`
`Field of Invention
`
`The present invention is directed to a method for treating a dental instrument, and specifically to
`
`a rotary file useful for shaping and cleaning root canals with severe curvature.
`
`Description of Invention:
`
`Superelastic materials are typically metal alloys which return to their original shape after
`
`substantial deformation. Examples of efforts in the art towards superelastic materials are found
`
`in US 6,149,501, which is herein incorporated by reference for all purposes.
`
`The endodontic rotary instrument made of shape memory alloys (e.g., NiTi based, Cu based, Fe
`
`based, or combinations thereof) in their martensitic state of the present invention may provide
`
`more flexibility and increase fatigue resistance by optimized microstructure, which is particularly
`effective in shaping and cleaning canals with severe curvatures. Superelastic alloys such as
`
`nickel titanium (NiTi) or otherwise can withstand several times more strain than conventional
`
`materials, such as stainless steel, without becoming plastically deformed.
`
`This invention relates to dental instruments in general. Specifically, this invention relates to
`
`endodontic rotary instruments for use in root canal cleaning and shaping procedures. The
`
`present invention provides an innovation of endodontic instrument that is made of shape
`
`memory alloys (SMA) such as Nickel-Titanium (NiTi) based systems, Cu based systems Fe
`
`based systems, or any combination thereof (e.g., materials selected from a group consisting of
`
`near-equiatomic Ni-Ti, Ni-Ti-Nb alloys, Ni-Ti-Fe alloys, Ni-Ti-Cu alloys, beta-phase titanium and
`
`combinations thereof).
`
`The present invention comprises rotary instruments made of NiTi Shape Memory Alloys, which
`
`provide one or more of the following novel aspects:
`1) Primary metallurgical phase in microstructure: martensite is the primary metallurgical
`
`phase in the present invention instrument, which is different from standard NiTi rotary
`
`instruments with predominant austenite structure at ambient temperature;
`
`1
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`US ENDODONTICS, LLC., Petitioner
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`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/1 0/1 0
`
`2) Higher austenite finish temperature (the final A.sub.f temperature measured by
`
`Differential Scanning Calorimetry): the austenite finish temperature is preferably higher
`
`(e.g., at least about 3°C) than the ambient temperature (25°C); in contrast, most
`standard superelastic NiTi rotary instruments have austenite finish temperatures lower
`
`than ambient temperature;
`
`3) Due to higher austenite finish temperature, the present invention instrument would not
`
`return to the original complete straight state after being bent or deflected; in contrast,
`most standard superelastic NiTi rotary instruments can return to the original straight form
`
`via reverse phase transformation (martensite-to-austenite) upon unloading.
`
`4) Endodontic instruments made of NiTi shape memory alloys in their martensitic state
`
`have significantly improved overall performance than their austenitic counterparts
`
`(regular superelastic NiTi instruments), especially on flexibility and resistance against
`
`cyclic fatigue.
`
`5) The strength and cutting efficiency of endodontic instruments can also be improved by
`
`using ternary shape memory alloys NiTiX (X: Co, Cr, Fe, Nb, etc) based on the
`
`mechanism of alloy strengthening.
`
`Specifically, the present invention instrument has essential and most desired characteristics for'
`
`improved
`lower stiffness,
`including higher flexibility and
`successful root canal surgery,
`resistance to cyclic fatigue, higher degree of rotation against torsional fracture, more conforming
`
`to the shape of highly curved canals (less likely for !edging or perforation), and minimum
`
`possibility of instrument separation in comparison against conventional endodontic instruments
`
`made of NiTi shape memory alloy in superelastic condition with fully austenitic phase in
`
`microstructure.
`
`Methods of Manufacturing Martensitic Endodontic Instruments
`
`Endodontic instruments made of NiTi shape memory alloys in their martensitic state in the
`
`present invention can be fabricated by the following methods:
`1) Method 1: Post heat treatment after file flutes have been manufactured according to
`
`mechanical design (i.e., after flute grinding process in a typical file manufacturing
`
`This process includes a post heat treatment including a heating step at
`process).
`temperature of at least 300°C. Preferably the heating step includes a temperature
`ranging from about 300°C to about 600°C, and more preferably from about 370°C to
`
`about 51 0°C. The heat treatment step may be present for a time period of at least 5
`
`2
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`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`minutes. Preferably, the heating step may be present for a time period that ranges from
`about 5 minutes to about 120 minutes, and more preferably from about 10 minutes to
`
`about 60 minutes (typically under a controlled atmosphere).
`Similar to the traditional NiTi rotary file manufacturing process using regular superelastic
`
`NiTi wires; however, in another embodiment, an additional thermal process- (e.g., post
`heat treatment at the temperature range of 370 - 510 oc for a period of time (typically
`10-60 min) depending on file size, taper, file design requirement) will be performed after
`flute grinding process. Essentially, Nickel-rich precipitates may form during this post
`
`heat treatment process. Correspondingly, the ratio of Ti/Ni will increase and a desired
`
`austenite finish temperature (the final At temperature) will be achieved. After post heat
`
`treatment, brass or steel handle will be installed.
`
`2) Method 2: Apply heat during grinding process to ensure the temperature on the NiTi
`
`materials is higher than their austenite finish temperatures.
`
`In this method, grinding process will be directly applied to martensitic SMA (e.g., NiTi)
`
`wires. However, martensitic SMA (e.g., NiTi) wires will be heated to a temperature
`
`higher than their austenite finish temperatures during grinding process. Therefore,
`martensitic SMA (e.g., NiTi) wires will temporarily transform to superelastic wires (a
`
`stiffer structure in the austenitic state) to facilitate the grinding process during the
`instrument manufacturing process. The instruments will transform back to martensitic
`
`state at ambient temperature after flute grinding process.
`
`-
`For example, in one embodiment, the method may include a non-superelastic wire; The
`
`non-superelastic wire may provided in a manufacturing environment with temperature
`
`higher than its austenite finish temperature (at least 25 degree C; The non-superelastic
`
`wire may transform to superelastic at this higher temperature); then forming flutes and
`
`grooves to form the (semi finished) rotary file; then, remove the (semi-finished) rotary file
`
`from the manufacturing environment with higher (warmer) temperature. The non(cid:173)
`
`superelastic wire will form non-superelastic rotary file at room temperature about 25°C.
`
`Description of Known Prior Art:
`
`3
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`US ENDODONTICS, LLC., Petitioner
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`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/1 0/1 0
`
`The endodontic instruments (including files and reamers) are used for cleaning and shaping the
`root canals of infected teeth as shown in Fig. 1 and 2. They are in mode of either rotation or
`reciprocation in the canal by dentists, either manually or with the aid of dental handpieces onto
`which the instruments are mounted. Instruments are generally used in sequence (depending on
`different root canal surgery techniques) in order to achieve the desired outcome of cleaning and
`
`shaping. The endodontic instrument is subjected to substantial cyclic bending and torsional
`stresses as it is used in the process of cleaning and shaping a root canal. Because of the
`complex curvature of root canals, a variety of unwanted procedural accidents such as ledging,
`
`transportation, perforation, or instrument separation, can be encountered in the practice of
`endodontics.
`
`Currently, endodontic rotary instruments made of Shape Memory Alloys (SMA) have shown
`better overall performance than stainless steel counterparts. However, the occurrence of
`unwanted procedural accidents mentioned above has not been drastically reduced. Therefore,
`it necessitates new endodontic instruments with improved overall properties, especially flexibility
`
`and resistance to fracture either due to cyclic fatigue and torsional overload.
`
`4
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`US ENDODONTICS, LLC., Petitioner
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`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`10--...._
`
`I
`
`I ;I
`
`i
`
`1
`
`Fig.2
`
`18·
`Fig.l
`
`Fig. 1 &2 Fig. 1 is an elevation a I view of a typical endodontic instrument showing the lower
`portion thereof, that is, the stem of the instrument having circumferential grooves formed on the
`outer surface to form circumferential cutting/scraping edges. Fig. 2 is an elevational cross(cid:173)
`sectional view of a molar human tooth showing the root system and the coronal area penetrated
`by a hole to expose the root canal system. Shown positioned within one of the root canals is
`the endodontic instrument as illustrated in Fig. 1. The endodontic instrument is subjected to
`substantial cyclic bending and torsional stresses as it is used in the process of cleaning and
`shaping a root canal.
`Shape memory alloy like NiTi alloy has two primary crystallographic structures, which are
`temperature dependent, i.e. austenite at higher temperatures and martensite at
`lower
`
`5
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`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`temperatures. This
`
`temperature-dependent diffusionless phase
`
`transformation
`
`is
`
`from
`
`martensite to austenite (M ~A) during heating, while the reverse transformation from austenite
`
`to martensite (A ~ M) starts upon cooing. Sometimes, R-phase as an intermediate phase
`between austenite and martensite could appear during phase transformations i.e., either M ~ R
`
`~ A during heating or A~ R ~ M during cooling. The phase transformation temperatures can
`
`be determined using Differential Scanning Calorimetry (DSC) curve as shown in the Fig. 3. For
`
`example, Af (austenite finish temperature) can be obtained from the graphical intersection of the
`baseline with the extension of the line of maximum inclination of the peak of the heating curve.
`
`The final A.sub.f temperature of endodontic instrument made of shape memory alloys was
`
`measured in DSC test with general accordance with ASTM Standard F2004-05 "Standard Test
`
`Method for Transformation Temperature of Nickel-Titanium Alloys by Thermal Analysis", such
`
`as using heating or cooling rates of 1 0±0.5°C/min with purge gas of either helium or nitrogen,
`
`except that the fluted segment' cut from rotary instrument sample does not need any further
`
`thermal annealing process (i.e., 850°C for 30 min in vacuum), which is typically used for
`
`measuring ingot transition temperatures at fully austenitic condition.
`
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`US ENDODONTICS, LLC., Petitioner
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`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/1 0
`
`iOO ·.-----------------------------~
`
`Cooling
`+-
`
`•As
`Af i
`.......... _:.:..· ___ .,._ ..... ___ ..... _________ :·"':':---~..:.~'\.---------~----:..:.:"7·-.~---,..,;.--"':'-.;J .... ;;.;· _____ ...;..;., ___ _
`' '·.
`
`''---to(cid:173)
`Heating
`
`50
`
`Fig. 3 Schematic differential scanning calorimetry (DSC) curve of a shape memory alloy (nickel(cid:173)
`
`titanium) in both heating and cooling cycle. Af (austenite finish temperature), As (austenite start
`
`temperature), Mf (martensite finish temperature), Ms (martensite start temperature) are obtained
`from the graphical intersection of the baseline with the extension of the line of maximum
`
`inclination of the appropriate peak of the curve. Martensite start temperature (Ms): the
`
`temperature at which the transformation from austenite to martensite begins on cooling;
`
`Martensite finish temperature (Mf): the temperature at which the transformation from austenite
`
`to martensite finishes on cooling; Austenite start temperature (As): the temperature at which the
`
`transformation
`
`from
`
`martensite
`
`to
`
`austenite
`
`begins
`
`on
`
`heating;
`
`Austenite finish temperature; (Af): the temperature at which the transformation from martensite
`
`to austenite finishes on heating.
`
`Description of How Problems.are Solved by Present Invention and Other Advantages:
`
`7
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`13 of 39
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`US ENDODONTICS, LLC., Petitioner
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`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/1 0/1 0
`
`Based on the experimental results, the endodontic instruments made of NiTi shape memory
`
`alloys in their martensitic state will possess the following most desired characteristics for root
`canal surgery: (1) higher flexibility and lower stiffness; (2) improved resistance to cyclic fatigue;
`
`(3) higher degree of rotation against torsional fracture; and (4) more conforming to the curved
`
`canal profile, especially for the root canals with considerable curvature and complex profile.
`
`In order to compare the impact of different metallurgical structures (austenite vs. martensite),
`two different instrument samples have made through different thermal processing in order to
`
`represent two distinct structures: (1) superelastic instruments with fully austenitic microstructure,
`
`(2) instrument with martensitic microstructure. Based on the DSC measurements, the final
`A.sub.f temperatures for these two instruments with distinct microstructures are 17 and 37 oc,
`respectively. All instrument samples have the same geometric design. All tests were performed
`at ambient temperature -23 oc.
`
`(1) Stiffness test showing higher flexibility and lower stiffness on endodontic instruments
`\
`
`made of NiTi shape memory alloys in their martensitic state
`
`The stiffness of all sample instruments has been determined by twisting the root canal
`instrument through 45° using the testing apparatus as shown in Fig. 4. As shown in the testing
`
`results in Fig. 5, the rotary instruments with martensitic microstructure at ambient temperature
`In
`exhibit higher flexibility and lower stiffness (as indicated by lower peak torque on bending).
`comparison with the regular superelastic instrument with the final A.sub.f temperature 17 oc, the
`instruments with the martensitic microstructure (the final A.sub.f temperature - 37 oC) have
`shown 23% reduction in bending torque. The lower stiffness of martensitic instruments can be
`
`attributed to the lower Young's modulus of martensite (about 30-40 GPa) whereas austenite is
`
`about 80-90 GPa at ambient temperature.
`
`8
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`14 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`3
`
`Key
`
`1
`2
`3
`4
`
`reversible gear motor
`stop
`torque ... measunng dev1ce
`catch pin
`
`Apparatus for bending test
`
`Fig. 4 Diagrammatic representation of bending test apparatus to measure stiffness or root canal
`instruments. (Picture was copied from ISO 3630-1:2008, Dentistry - Root-canal instrument(cid:173)
`Part 1: General requirements and test methods)
`
`Flexibility (Stiffness)
`
`1
`
`0.6
`
`-;::; 0.8
`0 g
`~
`... e 0.4
`:J c;
`.:.r. "' ~ a.
`
`0.2
`
`0
`
`Regular SuperEiastic (Af=17''C)
`
`Martensitic {Af=37""C}
`
`Fig. 5 Schematic graph of the relationship between different NiTi microstructures (regular
`superelastic or austenic vs. martensitic) and average peak torque of endodontic rotary
`instruments made of NiTi shape memory alloy in bending test, showing that lower peak torque
`
`9
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`15 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/1 0
`
`(less stiff or more flexible) can be achieved by martensitic microstructure, which is indicated by
`
`the higher austenite finish temperatures.
`
`In one embodiement, the ratio of peak torque
`
`(flexibility/stiffness) of the non-superelastic rotary file to the superelastic rotary file may be less
`than about 1:0.9 (e.g., less than about 1:0.85, and preferably less than about 1 :0.8) at about
`
`25°C.
`
`(2) Bending rotation fatigue test showing higher fatigue life on endodontic instruments made
`of NiTi shape memory alloys in their martensitic state
`
`The fatigue resistance of all sample instruments has been measured by bending rotation fatigue
`
`tester as shown in Fig. 6. According to the testing results shown in Fig. 7, the average cyclic
`
`fatigue life of instruments in the martensitic state (A.sub.f temperature 37 °C) is about 3 times of
`
`its austenitic counterpart (A.sub.f temperature 17 °C).
`
`WARM·WATER
`OR
`COMPRESSED AIR
`
`10
`~-,
`106
`
`94
`
`118
`
`92
`·"" ""!~__,.......,... 88
`
`92
`
`Fig. 6 Diagrammatic representation of a test apparatus used to test the bending-rotation fatigue
`
`resistance of endodontic instruments. The endodontic rotary instrument sample is rotating
`
`freely within a simulated stainless steel canal with controlled radius and curvature.
`
`10
`
`16 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/1 0
`
`Q) ... 1400
`....
`:::;
`'-' ro 1200
`0 .....
`"' 1000
`Q) v
`>
`800
`
`Resistance against cyclic fatigue
`
`1201
`
`389
`
`,_ -
`'-' -0 ,_
`200 -{:?.
`
`600
`
`400
`
`Q)
`.a
`E
`::1
`t:
`75
`
`0
`
`Regular SuperEiastic (Af=1 7*C}
`
`Martensitic (Af=37*C}
`
`Fig. 7 Schematic graph of the relationship between different NiTi microstructures (austenic vs.
`
`martensitic) and average cyclic fatigue life of endodontic rotary instruments made of NiTi shape
`
`memory alloy, showing that longer cyclic fatigue
`
`life can be achieved by martensitic
`
`microstructure at ambient temperature, which is indicated by the higher austenite finish
`
`temperature. In another embodiement, the ratio of total number of cycles to fatigue (resistance
`
`against cyclic fatigue) of the non-superelastic rotary file to the superelastic rotary file may be at
`
`least about 1.25:1 (e.g., at least about 1.5:1, preferably at least about 2:1) at about 25°C ..
`
`(3) Torque test showing higher degree of rotation against torsional fracture on endodontic
`
`instruments made of NiTi shape memory alloys in their martensitic state
`
`The test of resistance to fracture of root canal instruments is performed to measure the average
`
`maximum degree of rotation against torsional fracture using the testing apparatus as shown in
`
`Fig. 8. According to the testing results in Fig. 9 and 10, the instruments with martensitic
`
`microstructure exhibit higher degree of rotation and peak torque against torsional fracture than
`
`their austenitic counterparts.
`
`Most instrument separation was caused by either cyclic fatigue or torsional fracture; therefore,
`
`the separation of instruments made of shape memory alloys with martensitic microstructure can
`be significantly reduced according to the testing results in (2) bending rotation fatigue test and
`(3) torque test.
`
`11
`
`17 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/10
`
`1
`
`2
`
`4
`
`1
`
`2
`
`3
`
`1
`2
`3
`4
`5
`
`reversible gear motor
`chuck with hardened steel jaws
`,chuckwithsoftbrassjaws
`torque measuring device
`.Uriear ball~bearing
`
`K~y
`
`1
`2
`
`chuck with hardened steel jaws
`soft brass jaws
`
`Details oftest chuck
`
`Apparatus for torque test
`
`Fig. 8 Diagrammatic representation of torque test apparatus to measure the resistance to
`
`fracture by twisting and angular deflection (Pictures were copied from ISO 3630-1 :2008,
`Dentistry- Root-canal instrument- Part 1: General requirements and test methods)
`
`500
`
`... :;)
`(!) 520
`..... u
`....
`r\'!
`f-t.
`0 .....
`I:
`0
`+.;:::
`....
`ro
`0
`
`480
`
`0:: 460 -0
`
`Torsional Property
`
`503
`
`440
`
`(!)
`(!)
`
`,_
`
`440
`
`tl.l)
`(!)
`0
`E 420
`E
`·;;:
`r\'! 400
`~
`
`:;)
`
`Regular SuperElastic (Af=l7°C)
`
`Martensitic (Af::::37~C)
`
`·-···--·-··------·····-·····--·-····-··--··-·····-··-············-·······-··-··-···-----·-··········--·············-············----·-···---···-··-····-······'
`Fig. 9 Schematic graph of the relationship between different metallurgical structures and
`average "maximum degree of rotation to fracture" of endodontic rotary instruments made of NiTi
`
`shape memory alloy, showing that higher degree of rotation can be achieved by martensitic
`
`12
`
`18 of 39
`
`IPR2015-00632 - Ex. 1015
`US ENDODONTICS, LLC., Petitioner
`
`

`

`Attorney Docket: TUL-229A
`Provisional Application filed electronically on 05/10/1 0
`
`microstructure.
`
`In another embodiement, the ratio of maximum degree of rotation to fracture
`
`(torsional property) of the non-superelastic rotary file to the superelastic rotary file may be at
`
`least about 1.05:1 (e.g., at least about 1.075:1, preferably at least about 1.1:1) at about 25°C.
`
`Torsional Resistance
`
`1.8
`
`1.75
`
`1.7
`
`-....
`0 ,s
`Q>
`::;
`... 0
`0' 1.65
`l-
`.:;e.
`Q
`Q>
`0..
`
`1.6
`
`1.55
`
`15
`
`Regular SuperEiastk (Af=1 TC}
`
`Martensitic (Af=37*C}
`
`Fig. 10 Schematic graph of the relationship between different metallurgical structures and
`
`average "peak torque" of endodontic rotary instruments made of NiTi shape memory alloy,
`In
`showing that higher torque resistance can be achieved by martensitic microstructure.
`
`another embodiement, the ratio of peak torque (torsional resistance) of the non-superelastic
`rotary file to the superelastic rotary file may be at least about 1.05:1 (e.g., at least about 1.075:1,
`
`preferably at least about 1.09:1) at about 25°C.
`
`(4) Endodontic instruments made of NiTi sha