(19) United States
`(12) Patent Application Publication (10) Pub. No.: US 2008/0032260 A1
`Luebke
`(43) Pub. Date:
`Feb. 7 2008
`
`9
`
`US 20080032260A1
`
`(54) DENTAL AND MEDICAL INSTRUMENTS
`COMPRISING TITANIUM
`
`Publication Classi?cation
`
`(76) Inventor: Neill Hamilton Luebke, Brook?eld, WI
`(US)
`
`(51) Int. Cl.
`(2006.01)
`A61C 5/02
`(52) US. Cl. .......................................... .. 433/102; 433/224
`
`Correspondence Address:
`QUARLES & BRADY LLP
`411 E. WISCONSIN AVENUE
`SUITE 2040
`MILWAUKEE’ WI 53202-4497 (Us)
`_
`(21) Appl' NO"
`.
`_
`(22) PCT Flled'
`_
`86 PCTN ..
`O
`(
`)
`§ 371(c)(1)
`(2) (4) Dat’e:
`’
`
`11/628’933
`
`Jun' 7’ 2005
`
`PCT/US05/19947
`
`Dec_ 7, 2006
`
`Related U_s_ Application Data
`
`(60) Provisional application No. 60/578,091, ?led on Jun.
`8, 2004.
`
`(57)
`
`ABSTRACT
`
`Endodontic instruments for use in performing root canal
`therapy on a tooth are disclosed. In one form, the instru
`ments include an elongate shank having a cutting edge
`extending from a distal end of the shank along an axial
`length of the shank. The shank comprises a titanium alloy,
`and the shank is prepared by heat-treating the shank at a
`temperature above 250 C. in an atmosphere consisting
`essentially of a gas unreactive With the shank. In another
`form, the endodontic instruments have an elongate shank
`having a cutting edge extending from a distal end of the
`shank along an axial length of the shank. The shank consists
`essentially of a titanium alloy selected from alpha-titanium
`alloys, beta-titanium alloys, and alpha-beta-titanium alloys.
`The instruments Solve the problems encountered When
`cleaning and enlarging a curved root canal.
`
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`Patent Application Publication Feb. 7, 2008 Sheet 1 0f 7
`
`US 2008/0032260 A1
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`B F
`
`F162
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`Patent Application Publication Feb. 7, 2008 Sheet 2 0f 7
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`US 2008/0032260 A1
`
`Fig. 1b
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`Patent Application Publication Feb. 7, 2008 Sheet 3 0f 7
`
`US 2008/0032260 A1
`
`Figure 3
`
`MEAN of‘l'l'
`
`= +7%
`
`EMEAH?TqYl?W“;
`
`_____ WV
`
`L ... _
`
`250
`
`200 ——
`
`ICOntrQI
`
`ETTIN
`
`150 —
`
`Mt (gcm)
`
`100 —
`
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`Patent Application Publication Feb. 7, 2008 Sheet 4 0f 7
`
`US 2008/0032260 A1
`
`Figure 4
`
`[5 Control
`
`MEAN of TF
`
`= +25%
`
`1 000
`
`800 ——
`
`700 A—
`
`600 -—
`
`At (°)
`
`500 —
`
`400 —
`
`300 J~
`
`200 —
`
`100 W
`
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`Patent Application Publication Feb. 7, 2008 Sheet 5 0f 7
`
`US 2008/0032260 A1
`
`Figure 5
`
`lilControl
`'3“
`
`MEAN OfTI' -
`= -39%
`Me'mmij
`
`180
`
`160 ——
`
`140 i
`
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`Patent Application Publication Feb. 7, 2008 Sheet 6 0f 7
`
`US 2008/0032260 A1
`
`Figure 6
`
`+780 %
`
`+1350%
`
`+1260%
`
`+880%
`
`+1010%
`
`+1041%
`
`_I_T5@7/JE
`lar er SD’ WW.
`g
`‘
`
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`.I.
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`“mm/L;
`
`_B
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`
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`
`+610% &
`
`larger SD
`
`' M‘“
`
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`
`j
`
`51 Control
`DTP
`ElTl-N
`
`1
`
`1 My
`
`=;+a50%
`
`"lama-ML?
`
`~
`
`35
`
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`
`25 __
`
`20 ——
`
`5
`
`E;
`
`15 ~
`
`10 -
`
`5 __
`
`._;‘____7
`
`,
`
`._
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`__
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`‘
`
`_¥_4____.._
`
`_ WV“
`
`= +1050 % = 11 time's- higher angle '%
`MEAN ofTT
`1.
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`I,‘ |. LWMMJ I"
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`{MEAN of Tl-N =+710% = 8 times higher angle v
`
`SX
`
`S1
`
`S2
`
`F1
`
`F2
`
`F3
`
`ISO size
`
`7 of 14
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`Patent Application Publication Feb. 7, 2008 Sheet 7 0f 7
`
`US 2008/0032260 A1
`
`3500
`
`Figure 7
`
`I Contro'
`EHN
`
`MEAN OUT
`= +300% = 4 times higher resistance
`MEAN Qm-N = +200%_=w3.times higher resistarice
`
`1
`
`3000 -
`
`—-~~———~~—-~WMWW * " ~ " '~
`
`"'4
`
`+450% &
`larger SD
`
`‘I
`
`<
`
`7 ~
`
`7‘
`
`NZSOOA'SS‘
`ar er
`'~—g—~~——
`
`4.480% &
`
`larger SD
`
`2500 --
`
`2000 __
`
`1500 -—
`
`
`
`Fatigue (cycles)
`
`+23o% s.
`
`larger SD
`+180% &
`
`{larger SD
`
`+25% &
`1000 -- 'argefso W
`1+21o% &1
`ilarger SD }
`
`500 —~
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`‘ar er SD 1
`_E.
`
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`F130% a}
`larger SD 1
`+70% 8;’
`M
`
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`dunnglestmg
`
`2622:
`“1
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`b
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`IargerSD
`,Mwaaa
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`:
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`:
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`
`sx
`
`s1
`
`82
`
`F1
`
`ISO size
`
`F2
`
`F3
`
`8 of 14
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`IPR2015-00632 - Ex. 1012
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`

`US 2008/0032260 A1
`
`Feb. 7, 2008
`
`DENTAL AND MEDICAL INSTRUMENTS
`COMPRISING TITANIUM
`
`CROSS-REFERENCES TO RELATED
`APPLICATIONS
`
`[0001] This application claims priority from US. Provi
`sional Patent Application No. 60/578,091 ?led Jun. 8, 2004.
`
`STATEMENT REGARDING FEDERALLY
`SPONSORED RESEARCH
`
`[0002] Not Applicable.
`
`BACKGROUND OF THE INVENTION
`
`1. Field of the Invention
`
`[0003]
`[0004] The invention relates to instruments used in medi
`cine and dentistry. More particularly, the invention relates to
`medical and dental instruments such as drills, burs and ?les,
`and to endodontic instruments such as drills, burs and ?les
`used by dentists.
`[0005] 2. Description of the Related Art
`
`[0006] Endodontics or root canal therapy is the branch of
`dentistry that deals With diseases of the dental pulp and
`associated tissues. One aspect of endodontics comprises the
`treatment of infected root canals by removal of diseased
`pulp tissues and subsequent ?lling.
`
`[0007] FIG. 1 shoWs a representation of a tooth to provide
`background. Root canal therapy is generally indicated for
`teeth having sound external structures but having diseased,
`dead or dying pulp tissues. Such teeth Will generally possess
`intact enamel 10 and dentin 12, and Will be satisfactorily
`engaged With the bony tissue 20, by among other things,
`healthy periodontal ligaments 18. In such teeth, the pulp
`tissue 14, and excised portions of the root 16, should be
`replaced by a biocompatible substitute. FIG. 1 also shoWs
`the apical foramen 22 through Which blood and nerves pass
`to support the pulp tissues.
`
`[0008] One method for the preparation of a root canal for
`?lling is represented by FIGS. 2a-2e. A tooth having a
`basically sound outer structure 24 but diseased pulp 26, is
`cut With conventional or coated dental drill 28 creating a
`coronal access opening 30. A broach is used for gross
`removal of pulp material 26 from the root canal through the
`coronal access opening 30. The void 32 formed is enlarged
`as in FIG. 2d With ?le 34, to result in a fully excavated cavity
`36. Debris is removed from this cavity by ?ushing and the
`cavity cleansed to remove all diseased tissue. The excavated
`canal is then ready for ?lling.
`[0009] During this procedure, small endodontic instru
`ments (e.g., ?le 34) are utiliZed to clean and enlarge the long
`narroW tapered root canals. While most ?les perform
`entirely satisfactorily When cleaning and enlarging a straight
`root canal, problems have been encountered When using
`certain ?les to clean and enlarge a curved root canal. As Will
`be understood by those skilled in the art, a very large portion
`of the root canals encountered by a practicing dentist and/or
`endodontist are of the curved variety, and thus this problem
`is a signi?cant one for the profession.
`
`[0010] When performing an operation on a curved root
`canal With a smaller diameter ?le, the ?le can easily be
`
`inserted into the curved canal and Will easily bend to ?t the
`curved shape of the canal due to the ?exibility of the small
`diameter ?le. In FIG. 1a, there is shoWn the ?le 34 of FIG.
`2d in a bent position. The ?le 34 has a shank 42 mounted at
`its proximate end 47 to a handle 43. The shank 42 may
`include calibrated depth markings 45 and further includes a
`distal end 48. The shank 42 includes tWo continuous helical
`?utes 51 as shoWn in FIG. 1b that extend along its loWer
`portion. The ?utes 51 de?ne a cutting edge. Ahelical land 53
`is positioned betWeen axially adjacent ?utes as shoWn in
`FIG. 1b.
`
`[0011] While ?le 34 can easily bend to ?t the curved shape
`of a canal due to the ?exibility of the small diameter shank
`42, With increasingly larger siZes of ?les, the ?le becomes
`signi?cantly less ?exible and becomes more and more
`di?icult to insert through the curved portion of the canal. In
`some cases, the relatively in?exible ?le Will cut only on the
`inside of the curve and Will not cut on the outside of the
`curvature of the root canal. Thus, the problems, Which occur
`during the therapy of a root canal, are often the result of the
`basic stiffness of the ?les, particularly With the respect to the
`instruments of larger diameter.
`
`[0012] Various solutions have been proposed to limit the
`problems encountered When cleaning and enlarging a curved
`root canal With a ?le. For example, US. Pat. No. 4,443,193
`describes a shaped endodontic instrument that is said to
`solve this problem. US. Pat. No. 5,380,200 describes an
`endodontic instrument having an inner core and an outer
`shell Wherein one of the cores or shell is a nickel-titanium
`alloy and the other core or shell is selected from stainless
`steel, titanium alpha alloy, titanium beta alloy, and titanium
`alpha beta alloy. (For background on beta-titanium, see US.
`Pat. Nos. 4,197,643; 4,892,479; 4,952,236; 5,156,807;
`5,232,361; 5,264,055; 5,358,586; 5,947,723; 6,132,209; and
`6,258,182.) US. Pat. No. 5,464,362 describes an endodontic
`instrument of a titanium alloy that is machined under certain
`speci?c operating parameters to produce an instrument
`having high ?exibility, high resistance to torsion breakage,
`and sharp cutting edges. US. Pat. No. 6,315,558 proposes
`the use of superelastic alloys such as nickel-titanium that can
`Withstand several times more strain than conventional mate
`rials Without becoming plastically deformed. This property
`is termed shape memory, Which alloWs the superelastic alloy
`to revert back to a straight con?guration even after clinical
`use, testing or fracture (separation).
`
`[0013] In spite of the aforementioned advances, there
`remains a need for medical and dental instruments, and
`particularly endodontic instruments, such as drills, burs and
`?les, that have high ?exibility, have high resistance to
`torsion breakage, maintain shape upon fracture, can With
`stand increased strain, and can hold sharp cutting edges.
`
`SUMMARY OF THE INVENTION
`
`[0014] The present invention overcomes the problems
`encountered When cleaning and enlarging a curved root
`canal. In one aspect, the invention provides an endodontic
`instrument for use in performing root canal therapy on a
`tooth. The instrument includes an elongate shank having a
`cutting edge extending from a distal end of the shank along
`an axial length of the shank. The shank comprises a titanium
`alloy, and the shank is prepared by heat-treating the shank at
`a temperature above 250 C. in an atmosphere consisting
`
`9 of 14
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`IPR2015-00632 - Ex. 1012
`US ENDODONTICS, LLC., Petitioner
`
`

`

`US 2008/0032260 A1
`
`Feb. 7, 2008
`
`essentially of a gas unreactive With the shank. The shank has
`high ?exibility, high resistance to torsion breakage, main
`tains shape upon fracture, can Withstand increased strain,
`and can hold sharp cutting edges. Thus, it solves the prob
`lems encountered When cleaning and enlarging a curved root
`canal.
`
`[0015] In another aspect, the invention provides an endo
`dontic instrument for use in performing root canal therapy
`on a tooth. The instrument has an elongate shank having a
`cutting edge extending from a distal end of the shank along
`an axial length of the shank. The shank consists essentially
`of a titanium alloy selected from alpha-titanium alloys,
`beta-titanium alloys, and alpha-beta-titanium alloys. The
`shank avoids the use of complex tWo material systems that
`are expensive to produce and are prone to delamination of
`the materials. This version of the invention also solves the
`problems encountered When cleaning and enlarging a curved
`root canal.
`
`[0016] These and other features, aspects, and advantages
`of the present invention Will become better understood upon
`consideration of the folloWing detailed description, draW
`ings, and appended claims.
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`
`[0017] FIG. 1 is a cross-sectional vieW of a tooth.
`
`[0018] FIG. 1a is a side elevational vieW of an endodontic
`instrument.
`
`[0019] FIG. 1b is a partial detailed vieW of the shank of the
`endodontic instrument shoWn in FIG. 1a.
`
`[0020] FIGS. 2a-2e represent a prior art procedure for
`preparing a tooth for endodontic restoration.
`
`[0021] FIG. 3 is a graph shoWing the results of a study of
`torsion (Mt) reported in g~cm performed in accordance With
`“ISO Standard 3630-1 DentistryiRoot-canal instru
`mentsiPart 1: General requirements” and “ANSI/ADA
`Speci?cation No. 28, Endodontic ?les and reamers” for
`untreated (Control) ?les, heat-treated ?les (TT), and tita
`nium nitride coated ?les (TiiN).
`
`[0022] FIG. 4 is a graph shoWing the results of a study of
`torsion (At) reported in degrees of de?ection performed in
`accordance With “ISO Standard 3630-1 DentistryiRoot
`canal instrumentsiPart 1: General requirements” and
`“ANSI/ADA Speci?cation No. 28, Endodontic ?les and
`reamers” for untreated (Control) ?les, heat-treated ?les
`(TT), and titanium nitride coated ?les (TiiN).
`
`[0023] FIG. 5 is a graph shoWing the results of a study of
`maximum torque at 45° of ?exion (Mf) reported in g-cm
`performed in accordance With “ISO Standard 3630-1 Den
`tistryiRoot-canal instrumentsiPart 1: General require
`ments” and “ANSI/ADA Speci?cation No. 28, Endodontic
`?les and reamers” for untreated (Control) ?les, heat-treated
`?les (TT), and titanium nitride coated ?les (TiiN).
`
`[0024] FIG. 6 is a graph shoWing the results of a study of
`angle of permanent deformation after the ?exion test (ADP)
`reported in degrees of de?ection performed in accordance
`With “ISO Standard 3630-1 DentistryiRoot-canal instru
`mentsiPart 1: General requirements” and “ANSI/ADA
`Speci?cation No. 28, Endodontic ?les and reamers” for
`
`untreated (Control) ?les, heat-treated ?les (TT), and tita
`nium nitride coated ?les (TiiN).
`
`[0025] FIG. 7 is a graph shoWing the results of a study of
`fatigue reported in cycles (revolutions) to failure for
`untreated (Control) ?les, heat-treated ?les (TT), and tita
`nium nitride coated ?les (TiiN). This study Was performed
`in accordance With the “ISO Standard 3630-2 Dental root
`canal instrumentsiPar‘t 2: Enlargers” and “ANSI/ADA
`Speci?cation No. 95, for Root canal enlargers”.
`
`DETAILED DESCRIPTION OF THE
`INVENTION
`
`[0026] One embodiment of the invention provides an
`improved endodontic instrument for use in performing root
`canal therapy on a tooth. This embodiment of the invention
`is an endodontic instrument as shoWn in FIG. 111 that
`includes an elongate shank 42 mounted at its proximate end
`47 to a handle 43. The shank 42 may be about 30 millimeters
`long. The proximate end 47 may have a diameter of about
`0.5 to about 1.6 millimeters. The shank 42 may include
`calibrated depth markings 45 and further includes a distal
`end 48. The shank 42 includes tWo continuous helical ?utes
`51 as shoWn in FIG. 1b that extend along its loWer portion.
`The ?utes 51 de?ne a cutting edge. A helical land 53 is
`positioned betWeen axially adjacent ?utes as shoWn in FIG.
`1b.
`
`[0027] The shank 42 comprises a titanium alloy, and is
`prepared by heat-treating the shank at a temperature above
`250 C. in an atmosphere consisting essentially of a gas
`unreactive With the shank. Preferably, the temperature is
`from 4000 C. up to but not equal to the melting point of the
`titanium alloy, and most preferably, the temperature is from
`4750 C. to 525° C. Preferably, the gas is selected from the
`group consisting of helium, neon, argon, krypton, xenon,
`and radon. Most preferably, the gas is argon. In one example
`embodiment, the shank is heat-treated for approximately 1
`to 2 hours. In another example embodiment, the shank is
`heat-treated at 500° C. for 75 minutes. HoWever, other
`temperatures are suitable as they are dependent on the time
`period selected for heat exposure.
`
`[0028] The titanium alloy may be selected from alpha
`titanium alloys, beta-titanium alloys, alpha-beta-titanium
`alloys, and nickel-titanium alloys. Non-limiting examples of
`alpha-titanium alloys, beta-titanium alloys, alpha-beta-tita
`nium alloys for use in this embodiment of the invention are:
`Ti-5Al-2.5Sn alpha alloy; Ti-5Al-2.5Sn-ELI (loW O2) alpha
`alloy; Ti-3Al-2.5V alpha alloy; Ti-5Al-5Zr-5Sn alpha alloy;
`Ti-6Al-2Cb-1Ta-0.8Mo alpha alloy; Ti-5Al-5Sn-2Zr-2Mo
`0.25Si near alpha alloy; Ti-6Al-2Nb-1Ta-1Mo near alpha
`alloy; Ti-8Al-1Mo-1V near alpha alloy; Ti-6Al-2Sn-4Zr
`2Mo near alpha alloy; Ti-6Al-2Sn-1.5Zr-1Mo-0.35Bi-0.1Si
`near alpha alloy; Ti-2.25-Al-11Sn-5Zr-1Mo-0.2Si near
`alpha alloy; Ti-3Al-2.5V alpha-beta alloy; Ti-10V-2Fe-3Al
`alpha-beta alloy; Ti-5Al-2Sn-2Zr-4Mo-4Cr alpha-beta
`alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta alloy; Ti-4Al-4Mn
`alpha-beta alloy; Ti-6Al-2Sn-2Zr-2Mo-2Cr-0.25Si alpha
`beta alloy; Ti-4Al-3Mo-1V alpha-beta alloy; Ti-6Al-2Sn
`4Zr-6Mo alpha-beta alloy; Ti-11Sn-5Zr-2Al-1Mo alpha
`beta alloy; Ti-6Al-4V alpha-beta alloy; Ti-6Al-4V-ELI (loW
`O2) alpha-beta alloy; Ti-6Al-6V-2Sn-0.75Cu alpha-beta
`alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-6Al-2Sn-4Zr-2Mo
`alpha-beta alloy; Ti-5Al-1.5Fe-1.5Cr-1.5Mo alpha-beta
`
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`

`US 2008/0032260 A1
`
`Feb. 7, 2008
`
`alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3Al beta
`alloy; Ti-11.5Mo-6Zr-4.5Sn beta alloy; Ti-3Al-8V-6Cr
`4Mo-4Zr beta alloy; and Ti-3Al-13V-11Cr beta alloy (the
`numbers being percent by Weight). An example, nickel
`titanium alloy includes 54-57 Weight percent nickel and
`43-46 Weight percent titanium. Preferably, the titanium alloy
`used for the shank includes 54-57 Weight percent nickel and
`43-46 Weight percent titanium and is commercially available
`as Nitinol 55. Thus, most preferably, the shank consists
`essentially of 54-57 Weight percent nickel and 43-46 Weight
`percent titanium thereby avoiding the inclusion of elements
`that affect the superelastic properties of the alloy.
`[0029] Another embodiment of the invention provides an
`improved endodontic instrument for use in performing root
`canal therapy on a tooth. This embodiment of the invention
`is an endodontic instrument as shoWn in FIG. 111 that
`includes an elongate shank 42 mounted at its proximate end
`47 to a handle 43. The shank 42 may be about 30 millimeters
`long. The proximate end 47 may have a diameter of about
`0.5 to about 1.6 millimeters. The shank 42 may include
`calibrated depth markings 45 and further includes a distal
`end 48. The shank 42 includes tWo continuous helical ?utes
`51 as shoWn in FIG. 1b, Which extend along its loWer
`portion. The ?utes 51 de?ne a cutting edge. Ahelical land 53
`is positioned betWeen axially adjacent ?utes as shoWn in
`FIG. 1b. The endodontic instrument is fabricated solely from
`an alpha-titanium alloy, a beta-titanium alloy, or an alpha
`beta-titanium alloy to avoid the problems associated With
`multiple alloy systems.
`[0030] Non-limiting examples of alpha-titanium alloys,
`beta-titanium alloys, alpha-beta-titanium alloys for use in
`this embodiment of the invention are: Ti-5Al-2.5Sn alpha
`alloy; Ti-5Al-2.5Sn-ELI (low 02) alpha alloy; Ti-3Al-2.5V
`alpha alloy; Ti-5Al-5Zr-5Sn alpha alloy; Ti-6Al-2Cb-1Ta
`0.8Mo alpha alloy; Ti-5Al-5Sn-2Zr-2Mo-0.25Si near alpha
`alloy; Ti-6Al-2Nb-1Ta-1Mo near alpha alloy; Ti-8Al-1Mo
`1V near alpha alloy; Ti-6Al-2Sn-4Zr-2Mo near alpha alloy;
`Ti-6Al-2Sn-1.5Zr-1Mo-0.35Bi-0.1Si near alpha alloy;
`Ti-2.25-Al-11Sn-5Zr-1Mo-0.2Si near alpha alloy; Ti-3Al
`2.5V alpha-beta alloy; Ti-10V-2Fe-3Al alpha-beta alloy;
`Ti-5Al-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6Al-2Sn
`4Zr-6Mo alpha-beta alloy; Ti-4Al-4Mn alpha-beta alloy;
`Ti-6Al-2Sn-2Zr-2Mo-2Cr-025Si alpha-beta alloy; Ti-4Al
`3Mo-1V alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta
`alloy; Ti-11Sn-5Zr-2A-1Mo alpha-beta alloy; Ti-6Al-4V
`alpha-beta alloy; Ti-6Al-4V-ELI (low 02) alpha-beta alloy;
`Ti-6Al-6V-2Sn-0.75Cu alpha-beta alloy; Ti-7Al-4Mo alpha
`beta alloy; Ti-6Al-2Sn-4Zr-2Mo alpha-beta alloy; Ti-5Al
`1.5Fe-1.5Cr-1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta
`alloy; Ti-8Mo-8V-2Fe-3Al beta alloy; Ti-11.5Mo-6Zr-4.5Sn
`beta alloy; Ti-3Al-8V-6Cr-4Mo-4Zr beta alloy; and Ti-3Al
`13V-11Cr beta alloy (the numbers being percent by Weight).
`These alloys of titanium include phase stabiliZing amounts
`of a metal selected from molybdenum, tin, bismuth, tanta
`lum, vanadium, Zirconium, niobium, chromium, cobalt,
`nickel, manganese, iron, aluminum and lanthanum. An
`endodontic instrument according to this embodiment of the
`invention has improved sharpness, cutting ability, and
`instrument longevity compared to instruments fabricated
`from untreated nickel-titanium. Alpha-titanium, beta-tita
`nium and alpha-beta-titanium are superior because they are
`harder and hence Will hold an edge better and still maintain
`near the ?exibility of nickel-titanium to negotiate curved
`canals. These alpha-titanium, beta-titanium and alpha-beta
`
`titanium instruments may include medical, dental and endo
`dontic instruments (both hand and engine driven), cutting
`burs (drills), and enlarging instruments including hand,
`mechanical and rotary.
`[0031] Present medical and dental practice entails cutting
`of hard tissues such as bone or teeth With instruments
`manufactured of carbide steel, stainless steel and nickel
`titanium. Present endodontic practice entails the preparation,
`cleaning, and shaping of root canals in teeth utiliZing carbide
`steel, stainless steel and nickel-titanium instruments for
`hand, mechanical and rotary applications. This version of
`the invention Would use an alpha-titanium alloy, a beta
`titanium alloy, or an alpha-beta-titanium alloy to fabricate
`these instruments. It may be coated (as described beloW) or
`uncoated. Today a groWing number of physicians and den
`tists (endodontists) are utiliZing engine driven drills and ?les
`With various names and applications. This aspect of the
`present invention pertains to the fabrication of these cutting
`instruments such as drills and ?les solely from an alpha
`titanium alloy, a beta-titanium alloy, or an alpha-beta-tita
`nium alloy to produce a sharper cutting edge that should
`provide for better cutting or a smooth ?nished surface. This
`includes instrumentation that Will facilitate the cleaning and
`sealing of the root canal system. In addition, a coating or
`heat-treatment may relieve stress in the instrument to alloW
`it to Withstand more torque, rotate through a larger angle of
`de?ection, change the handling properties, or visually
`exhibit a near failure of the instrument. This aspect of the
`invention relates to all drills, burs, ?les, and instruments
`used in medicine and dentistry.
`[0032] In another aspect, the present invention provides
`for coating and optionally thereafter heat-treating dental and
`medical instruments including the coatings to maintain
`and/or improve their sharpness, cutting ability, and/ or instru
`ment longevity. Such an instrument may be manufactured
`from nickel-titanium, an alpha-titanium alloy, a beta-tita
`nium alloy, or an alpha-beta-titanium alloy, stainless steel,
`carbide steel, as Well as other materials. These instruments
`may be electropolished before or after coating or heat
`treating. These instruments Will include medical, dental and
`endodontic instruments (both hand and engine driven),
`cutting burs (drills), and enlarging instruments including
`hand, mechanical and rotary.
`[0033] The coating processes may include but not limited
`to the folloWing processes: composite electroless plating
`(see, e.g., U.S. Pat. Nos. 4,820,547; 4,997,686; 5,145,517;
`5,300,330; 5,863,616; and 6,306,466); chemical vapor depo
`sition (see, e.g., U.S. Pat. No. 4,814,294); microWave depo
`sition (see, e.g., U.S. Pat. No. 4,859,493); laser ablation
`process (see, e.g., U.S. Pat. No. 5,299,937); ion beam
`assisted deposition (see, e.g., U.S. Pat. No. 5,725,573);
`physical vapor deposition (see, e.g., U.S. Pat. Nos. 4,670,
`024, 4,776,863, 4,984,940, and 5,545,490); Molybdenum
`Disul?de Coating (MoS2) (see, e.g., U.S. Pat. No. 5,037,516
`or SAE Standard AMS2526); electropolishing; coatings
`including titanium nitride and titanium aluminum nitride
`commercially available under the trademark FirexTM; coat
`ings such as titanium nitride (TiN), titanium carbonitride
`(TiCN), titanium aluminum nitride (TiAlN), aluminum tita
`nium nitride (AlTiN); or multiple coatings or combinations
`of coatings.
`[0034] As detailed above, present medical and dental
`practice entails cutting of hard tissues such as bone or teeth
`
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`
`IPR2015-00632 - Ex. 1012
`US ENDODONTICS, LLC., Petitioner
`
`

`

`US 2008/0032260 A1
`
`Feb. 7, 2008
`
`With instruments manufactured of carbide steel, stainless
`steel and nickel-titanium. Present endodontic practice entails
`the preparation, cleaning, and shaping of root canals in teeth
`utilizing carbide steel, stainless steel and nickel-titanium.
`These can be manufactured as hand, mechanical and rotary
`instruments. Today a groWing number of physicians and
`dentists (endodontists) are utiliZing engine driven drills and
`?les With various names and applications. This aspect of the
`present invention pertains to the application of coatings and
`optionally heat-treatment to cutting instruments such as
`drills and ?les to produce a sharper cutting edge and a higher
`resistance to heat degradation that should provide for better
`cutting, a smooth surface and/or different metallurgical
`properties than the material from Which it Was manufac
`tured. This includes instrumentation that Will facilitate the
`cleaning and sealing of the root canal system. In addition, a
`heat-treatment separately applied or as utiliZed in the coating
`process may relieve stress in the instrument Which should
`alloW for more instrument longevity by the ability to With
`stand more torque, rotate through a larger angle of de?ec
`tion, change the handling properties, remove shape memory
`or visually exhibit a near failure of the instrument. This
`aspect of the invention relates to all drills, burs, ?les, and
`instruments used in medicine and dentistry.
`
`[0035] One example process of this aspect of the present
`invention for such instruments is a titanium nitride coating.
`This coating process is done With physical vapor deposition
`With an inherent heat-treatment. Another process is a mul
`tilayer process utilizing a titanium nitride coating and then
`a titanium aluminum nitride coating. This last coating pro
`cess is commercially available under the trademark
`FIREXTM.
`
`[0036] Another example process of this aspect of the
`present invention for such instruments is a metal or metal
`alloy coating incorporating particulate matter. One process
`to produce such a coating to an instrument includes con
`tacting the surface of the instrument With a stable electroless
`metalliZing bath comprising a metal salt, an electroless
`reducing agent, a complexing agent, an electroless plating
`stabiliZer, a quantity of particulate matter Which is essen
`tially insoluble or sparingly soluble in the metalliZing bath,
`and a particulate matter stabiliZer, and maintaining the
`particulate matter in suspension in the metalliZing bath
`during the metalliZing of the instrument for a time suf?cient
`to produce a metallic coating With the particulate matter
`dispersed.
`
`EXAMPLES
`
`[0037] The folloWing Examples have been presented in
`order to further illustrate the invention and are not intended
`to limit the invention in any Way.
`
`Example 1
`
`[0038] Thirty ISO siZe SX ?les, thirty ISO siZe S1 ?les,
`thirty ISO siZe S2 ?les, thirty ISO siZe F1 ?les, thirty ISO
`siZe F2 ?les and thirty ISO siZe F3 ?les Were used in a study
`of torsion (Mt) reported in g~cm performed in accordance
`With “ISO Standard 3630-1 DentistryiRoot-canal instru
`mentsiPart 1: General requirements” and “ANSI/ADA
`Speci?cation No. 28, Endodontic ?les and reamers”. The
`results are shoWn in FIG. 3. The ?les Were made from a
`titanium alloy comprising 54-57 Weight percent nickel and
`
`43-46 Weight percent titanium, and included an elongate
`shank having a cutting edge extending from a distal end of
`the shank along an axial length of the shank. Ten of each ISO
`siZe Were untreated (Control) ?les. Ten of each ISO siZe
`Were heat-treated in a furnace in an argon atmosphere at
`5000 C. for 75 minutes. These are labeled “TT” in FIG. 3.
`Ten of each ISO siZe Were coated With titanium nitride using
`physical vapor deposition With an inherent heat-treatment.
`These are labeled “TiiN” in FIG. 3. Mt Was determined for
`each of the thirty ?les in each siZe, and the mean and
`standard deviation for each group (Control, TT, TiiN) of
`ten ?les Were calculated. The ten ?les in all but one siZe that
`Were heat-treated in a furnace in an argon atmosphere at
`5000 C. for 75 minutes shoWed the best result With the
`highest Mt.
`
`Example 2
`
`[0039] Thirty ISO siZe SX ?les, thirty ISO siZe S1 ?les,
`thirty ISO siZe S2 ?les, thirty ISO siZe F1 ?les, thirty ISO
`siZe F2 ?les and thirty ISO siZe F3 ?les Were used in a study
`of torsion (At) reported in degrees of de?ection performed in
`accordance With “ISO Standard 3630-1 DentistryiRoot
`canal instrumentsiPart 1: General requirements” and
`“ANSI/ADA Speci?cation No. 28, Endodontic ?les and
`reamers”. The results are shoWn in FIG. 4. The ?les Were
`made from a titanium alloy comprising 54-57 Weight percent
`nickel and 43-46 Weight percent titanium, and included an
`elongate shank having a cutting edge extending from a distal
`end of the shank along an axial length of the shank. Ten of
`each ISO siZe Were untreated (Control) ?les. Ten of each
`ISO siZe Were heat-treated in a furnace in an argon atmo
`sphere at 5000 C. for 75 minutes. These are labeled “TT” in
`FIG. 4. Ten of each ISO siZe Were coated With titanium
`nitride using physical vapor deposition With an inherent
`heat-treatment. These are labeled “TiiN” in FIG. 4. At Was
`determined for each of the thirty ?les in each siZe, and the
`mean and standard deviation for each group (Control, TT,
`TiiN) of ten ?les Were calculated. The ten ?les in each siZe
`that Were heat-treated in a furnace in an argon atmosphere at
`5000 C. for 75 minutes shoWed the best results With the
`highest At.
`
`Example 3
`
`[0040] Thirty ISO siZe SX ?les, thirty ISO siZe S1 ?les,
`thirty ISO siZe S2 ?les, thirty ISO siZe F1 ?les, thirty ISO
`siZe F2 ?les and thirty ISO siZe F3 ?les Were used in a study
`of maximum torque at 450 of ?exion (Mf) reported in g~cm
`performed in accordance With “ISO Standard 3630-1 Den
`tistryiRoot-canal instrumentsiPart 1: General require
`ments” and “ANSI/ADA Speci?cation No. 28, Endodontic
`?les and reamers”. The shank is held in a torque meter,
`?exed at an angle of 45°, and then torque is measured. The
`results are shoWn in FIG. 5. The ?les Were made from a
`titanium alloy comprising 54-57 Weight percent nickel and
`43-46 Weight percent titanium, and included an elongate
`shank having a cutting edge extending from a distal end of
`the shank along an axial length of the shank. Ten of each ISO
`siZe Were untreated (Control) ?les. Ten of each ISO siZe
`Were heat-treated in a furnace in an argon atmosphere at
`5000 C. for 75 minutes. These are labeled “TT” in FIG. 5.
`Ten of each ISO siZe Were coated With titanium nitride using
`physical vapor deposition With an inherent heat-treatment.
`These are labeled “TiiN” in FIG. 5. MfWas determined for
`
`12 of 14
`
`IPR2015-00632 - Ex. 1012
`US ENDODONTICS, LLC., Petitioner
`
`

`

`US 2008/0032260 A1
`
`Feb. 7, 2008
`
`each of the thirty ?les in each size, and the mean and
`standard deviation for each group (Control, TT, TiiN) of
`ten ?les Were calculated. It can be seen that the heat-treated
`?les in each siZe impart less torque When bent and appear to
`have higher ?exibility than untreated (control) ?les.
`
`Example 4
`[0041] Thirty ISO siZe SX ?les, thirty ISO siZe Sl ?les,
`thirty ISO siZe S2 ?les, thirty ISO siZe Fl ?les, thirty ISO
`siZe F2 ?les and thirty ISO siZe F3 ?les Were used in a study
`of angle of permanent deformation after the ?exion test
`(ADP) reported in degrees of de?ection performed in accor
`dance With “ISO Standard 3630-1 DentistryiRoot-canal
`instrumentsiPart 1: General requirements” and “ANSI/
`ADA Speci?cation No. 28, Endodontic ?les and reamers”.
`The results are shoWn in FIG. 6. The ?les Were made from
`a titanium alloy comprising 54-57 Weight percent nickel and
`43-46 Weight percent titanium, and included an elongate
`shan