(12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT)
`
`(19) World Intellectual Property
`Organization
`International Bureau
`
`
`
`(43) International Publication Date
`29 December 2005 (29.12.2005)
`
`(10) International Publication Number
`
`PCT
`
`WO 2005/122942 A1
`
`(51) International Patent Classification7:
`
`A61C 5/02
`
`(21) International Application Number:
`PCT/US2005/019947
`
`(22) International Filing Date:
`
`7 June 2005 (07.06.2005)
`
`(25) Filing Language:
`
`(26) Publication Language:
`
`(30) Priority Data:
`60/578,091
`
`English
`
`English
`
`(84)
`
`8 June 2004 (08.06.2004)
`
`US
`
`(71) Applicant and
`(72) Inventor: LUEBKE, Neil, Hamilton [US/US]; 18010
`Continental Drive, Brookfield, WI 53045—1204 (US).
`
`(74) Agent: ROCHE, Richard, T.; Quarles & Brady LLP, 411
`East Wisconsin Avenue, Milwaukee, WI 53202 (US).
`
`AT, AU, AZ, BA, BB, BG, BR, BW, BY, BZ, CA, CH, CN,
`CO, CR, CU, CZ, DE, DK, DM, DZ, EC, EE, EG, ES, FI,
`GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE,
`KG, KM, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA,
`MD, MG, MK, MN, MW, MX, MZ, NA, NG, NI, NO, NZ,
`OM, PG, PH, PL, PT, RO, RU, SC, SD, SE, SG, SK, SL,
`SM, SY, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC,
`VN, YU, ZA, ZM, ZW.
`
`Designated States (unless otherwise indicated, for every
`kind of regional protection available): ARIPO (BW, GH,
`GM, KE, LS, MW, MZ, NA, SD, SL, SZ, TZ, UG, ZM,
`ZW), Eurasian (AM, AZ, BY, KG, KZ, MD, RU, TJ, TM),
`European (AT, BE, BG, CH, CY, CZ, DE, DK, EE, ES, FI,
`FR, GB, GR, HU, IE, IS, IT, LT, LU, MC, NL, PL, PT, RO,
`SE, SI, SK, TR), OAPI (BF, BJ, CF, CG, CI, CM, GA, GN,
`GQ, GW, ML, MR, NE, SN, TD, TG).
`
`(81) Designated States (unless otherwise indicated, for every
`kind of national protection available): AE, AG, AL, AM,
`
`Published:
`
`with international search report
`
`[Continued on next page]
`
`(54) Title: DENTAL AND MEDICAL INSTRUMENTS COMPRISING TITANIUM
`
`instruments
`Endodontic
`(57) Abstract:
`for use in performing root canal
`therapy
`on a tooth are disclosed.
`In one form,
`the
`instruments 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 25 °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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`|||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||
`
`— before the expiration of the time limit for amending the
`claims and to be republished in the event of receipt of
`amendments
`
`For two—letter codes and other abbreviations, refer to the ”Guid—
`ance Notes on Codes andAbbreviations” appearing at the begin—
`ning of each regular issue of the PCT Gazette.
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`WO 2005/122942
`
`PCT/US2005/019947
`
`Dental and Medical Instruments Comprising Titanium
`
`CROSS-REFERENCES TO RELATED APPLICATIONS
`
`[0001]
`
`This application claims priority from United States Provisional Patent
`
`Application NO. 60/578,091 filed June 8, 2004.
`
`STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
`
`[0002]
`
`Not Applicable.
`
`'
`
`BACKGROUND OF THE INVENTION
`
`1. Field of the Invention
`
`[0003]
`
`The invention relates to instruments used in medicine and dentistry.
`
`More particularly, the invention relates to medical and dental instruments such as
`
`10
`
`drills, burs and files, and to endodontic instruments such as drills, burs and files
`
`used by dentists.
`
`2. Description of the Related Art
`
`15
`
`20
`
`[0004]
`
`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 filling.
`
`[0005]
`
`Figure 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. Figure 1 also shows the apical foramen 22 through
`
`which blood and nerves pass to support the pulp tissues.
`
`25
`
`[0006]
`
`One method for the preparation of a root canal for filling is represented
`
`by Figures 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
`
`30
`
`formed is enlarged as in Figure 2d with file 34, to result in a fully excavated cavity
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`
`36. Debris is removed from this cavity by flushing and the cavity cleansed to
`
`remove all diseased tissue. The excavated canal is then ready for filling.
`
`[0007]
`
`During this procedure, small endodontic instruments (e.g., file 34) are
`
`utilized to clean and enlarge the long narrow tapered root canals. While most files
`
`perform entirely satisfactorily when cleaning and enlarging a straight root canal,
`
`problems have been encountered when using certain files 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 significant one for the
`
`10
`
`profession.
`
`[0008] When performing an operation on a curved root canal with a smaller
`
`diameter file, the file can easily be inserted into the curved canal and will easily
`
`bend to fit the curved shape of the canal due to the flexibility of the small diameter
`file.
`In Figure 1a, there is shown the file 34 of Figure 2d in a bent position. The
`
`15
`
`file 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 flutes 51 as shown in Figure 1b that
`
`extend along its lower portion. The flutes 51 define a cutting edge. A helical land
`
`53 is positioned between axially adjacent flutes as shown in Figure 1b.
`
`20
`
`[0009] While file 34 can easily bend to fit the curved shape of a canal due to
`
`the flexibility of the small diameter shank 42, with increasingly larger sizes of files,
`
`the file becomes significantly less flexible and becomes more and more difficult to
`
`insert through the curved portion of the canal.
`
`In some cases, the relatively
`
`inflexible file will out only on the inside of the curve and will not cut on the outside
`
`25
`
`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 files,
`
`particularly with the respect to the instruments of larger diameter.
`
`[0010]
`
`Various solutions have been proposed to limit the problems
`
`encountered when cleaning and enlarging a curved root canal with a file. For
`
`30
`
`example, U.S. Patent No. 4,443,193 describes a shaped endodontic instrument
`
`that is said to solve this problem. US. Patent No. 5,380,200 describes an
`
`endodontic instrument having an inner core and an outer shell wherein one of the
`
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`PCT/US2005/019947
`
`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. Patent 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. Patent No. 5,464,362 describes an endodontic
`
`instrument of a titanium alloy that is machined under certain specific operating
`
`parameters to produce an instrument having high flexibility, high resistance to
`
`torsion breakage, and sharp cutting edges. US. Patent No. 6,315,558 proposes
`
`10
`
`the use of superelastic alloys such as nickel-titanium that can withstand several
`times more strain than conventional materials without becoming plastically
`
`deformed. This property is termed shape memory, which allows the superelastic
`
`alloy to revert back to a straight configuration even after clinical use, testing or
`
`fracture (separation).
`
`[0011]
`
`In spite of the aforementioned advances, there remains a need for
`
`15
`
`medical and dental instruments, and particularly endodontic instruments, such as
`
`drills, burs and files, that have high flexibility, have high resistance to torsion
`
`breakage, maintain shape upon fracture, can withstand increased strain, and can
`
`hold sharp cutting edges.
`
`SUMMARY OF THE INVENTION
`
`20
`
`[0012]
`
`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
`
`25
`
`titanium alloy, and the shank is prepared by heat-treating the shank at a
`
`temperature above 25°C in an atmosphere consisting essentially of a gas
`
`unreactive with the shank. The shank has high flexibility, high resistance to
`
`torsion breakage, maintains shape upon fracture, can withstand increased strain,
`
`and can hold sharp cutting edges. Thus, it solves the problems encountered
`
`30
`
`when cleaning and enlarging a curved root canal.
`
`[0013]
`
`In another aspect, the invention provides an endodontic instrument for
`
`use in performing root canal therapy on a tooth. The instrument has an elongate
`
`-3-
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`
`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.
`
`[0014]
`
`These and other features, aspects, and advantages of the present
`
`invention will become better understood upon consideration of the following
`
`10
`
`detailed description, drawings, and appended claims.
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`
`[0015]
`
`Figure 1 is a cross-sectional view of a tooth.
`
`[0016]
`
`Figure 1a is a side elevational view of an endodontic instrument.
`
`[0017]
`
`Figure 1b is a partial detailed view of the shank of the endodontic
`
`15
`
`instrument shown in Figure 1a.
`
`[0018]
`
`Figures 2a-2e represent a prior art procedure for preparing a tooth for
`
`endodontic restoration.
`
`[0019]
`
`Figure 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 Dentistry -
`
`20
`
`Root-canal instruments - Part 1: General requirements" and “ANSI/ADA
`
`Specification No. 28, Endodontic files and reamers" for untreated (Control) files,
`
`heat-treated files (TT), and titanium nitride coated files (Ti-N).
`
`[0020]
`
`Figure 4 is a graph showing the results of a study of torsion (At)
`
`reported in degrees of deflection performed in accordance with “lSO Standard
`
`25
`
`3630-1 Dentistry - Root-canal instruments - Part 1: General requirements" and
`
`“ANSI/ADA Specification No. 28, Endodontic files and reamers" for untreated
`
`(Control) files, heat-treated files (TT), and titanium nitride coated files (Ti-N).
`
`[0021]
`
`Figure 5 is a graph showing the results of a study of maximum torque at
`
`45° of flexion (Mf) reported in g-cm performed in accordance with “ISO Standard
`
`30
`
`3630-1 Dentistry - Root-canal instruments - Part 1: General requirements" and
`
`“ANSI/ADA Specification No. 28, Endodontic files and reamers" for untreated
`
`(Control) files, heat—treated files (TT), and titanium nitride coated files (Ti—N).-
`
`-4-
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`
`[0022]
`
`Figure 6 is a graph showing the results of a study of angle of permanent
`
`deformation after the flexion test (ADP) reported in degrees of deflection
`
`performed in accordance with “ISO Standard 3630-1 Dentistry - Root—canal
`
`instruments - Part 1: General requirements" and “ANSI/ADA Specification No. 28,
`
`Endodontic files and reamers" for untreated (Control) files, heat-treated files (TT),
`
`and titanium nitride coated files (Ti-N).
`
`[0023]
`
`Figure 7 is a graph showing the results of a study of fatigue reported in
`
`cycles (revolutions) to failure for untreated (Control) files, heat-treated files (TT),
`
`and titanium nitride coated files (Ti-N). This study was performed in accordance
`
`10
`
`with the “ISO Standard 3630-2 Dental root-canal instruments - Part 2: Enlargers"
`
`and “ANSI/ADA Specification No. 95, for Root canal enlargers".
`
`DETAILED DESCRIPTION OF THE INVENTION
`
`[0024]
`
`One embodiment of the invention provides an improved endodontic
`
`instrument for use in performing root canal therapy on a tooth. This embodiment
`
`15
`
`of the invention is an endodontic instrument as shown in Figure 1a 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
`
`20
`
`continuous helical flutes 51 as shown in Figure 1b that extend along its lower
`
`portion. The flutes 51 define a cutting edge. A helical land 53 is positioned
`
`between axially adjacent flutes as shown in Figure 1b.
`
`[0025]
`
`The shank 42 comprises a titanium alloy, and is prepared by heat-
`
`treating the shank at a temperature above 25°C in an atmosphere consisting
`
`25
`
`essentially of a gas unreactive with the shank. Preferably, the temperature is from
`
`400°C up to but not equal to the melting point of the titanium alloy, and most
`preferably, the temperature is from 475°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
`
`30
`
`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.
`
`-5-
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`PCT/US2005/019947
`
`[0026]
`
`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-titanium alloys
`
`for use in this embodiment of the invention are: Ti-5Al-2.58n alpha alloy; Ti-5Al-
`
`2.58n-ELI (low 02) alpha alloy; Ti-3Al-2.5V alpha alloy; Ti-5Al-5Zr—58n alpha
`
`alloy; Ti—6Al-ZCb-1Ta-0.8Mo alpha alloy; Ti-5Al-5Sn-2Zr—2Mo-0.258i near alpha
`
`alloy; Ti-6Al—2Nb-1Ta-1Mo near alpha alloy; Ti-8Al-1Mo-1V near alpha alloy; Ti-
`
`6Al-28n-4Zr—2Mo near alpha alloy; Ti-6Al-28n-1.5Zr-1Mo-O.3SBi-O.1Si near alpha
`
`alloy; Ti-2.25-Al-11Sn-5Zr—1Mo-O.2$i near alpha alloy; Ti-3Al-2.5V alpha-beta
`
`alloy; Ti-10V—2Fe-3Al alpha-beta alloy; Ti—5Al-23n-22r-4Mo-4Cr alpha-beta alloy;
`
`Ti-6Al-28n-4Zr-6Mo alpha-beta alloy; Ti-4AI-4Mn alpha-beta alloy; Ti-6Al-28n-
`
`2Zr-2Mo—ZCr-O.25Si alpha-beta alloy; Ti-4Al-3Mo-1V alpha-beta alloy; Ti-6Al-28n-
`
`4Zr—6Mo alpha—beta alloy; Ti-11Sn-5Zr-2Al-1Mo alpha-beta alloy; Ti-6Al-4V alpha-
`
`beta alloy; Ti-6Al-4V-ELI (low 02) alpha-beta alloy; Ti-6Al-6V-28n-0.7SCu alpha-
`
`beta alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-6AI-28n-4Zr-2Mo alpha-beta alloy; Ti-
`
`5Al-1.5Fe-1.5Cr—1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-
`
`3Al beta alloy; Ti-11.5Mo-6Zr-4.5$n 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
`
`1O
`
`15
`
`20
`
`25
`
`the alloy.
`
`[0027]
`
`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 Figure 1a that includes
`
`an elongate shank 42 mounted at its proximate end 47 to a handle 43. The shank
`
`30
`
`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
`
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`v PCT/U82005/019947
`
`continuous helical flutes 51 as shown in Figure 1b, which extend along its lower
`
`portion. The flutes 51 define a cutting edge. A helical land 53 is positioned
`
`between axially adjacent flutes as shown in Figure 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.
`
`[0028]
`
`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-
`
`2.58n alpha alloy; Ti-5Al-2.5$n-ELI (low 02) alpha alloy; Ti-3Al-2.5V alpha alloy;
`
`Ti-5Al-52r—58n alpha alloy; Ti-6Al-2Cb-1Ta-O.8Mo alpha alloy; Ti-5Al-58n-22r-
`
`10
`
`2M0-0.25$i near alpha allOy; Ti-6Al-2Nb-1Ta-1Mo near alpha alloy; Ti-8Al-1Mo-
`
`15
`
`20
`
`1V near alpha alloy; Ti-6Al-28n-4Zr—2Mo near alpha alloy; Ti-6Al-28n-1.52r—1Mo-
`
`0.3SBi-O.1Si near alpha alloy; Ti-2.25-A|-11Sn-52r—1Mo-0.2$i near alpha alloy; Ti-
`
`3Al-2.5V alpha-beta alloy; Ti-1OV-2Fe-3Al alpha-beta alloy; Ti-5Al-28n-ZZr-4Mo-
`
`4Cr alpha-beta alloy; Ti-6Al-28n-4Zr-6Mo alpha—beta alloy; Ti-4Al - 4Mn alpha-
`
`beta alloy; Ti-6Al-28n-22r—2Mo-20r—0258i alpha-beta alloy; Ti-4Al-3Mo-1V alpha-
`
`beta alloy; Ti-6Al-28n-4Zr-6Mo alpha-beta alloy; Ti-11Sn-52r—2Al-1Mo alpha-beta
`
`alloy; Ti-6Al-4V alpha-beta alloy; Ti-6Al-4V—ELI (low 02) alpha-beta alloy; Ti-6Al-
`
`6V-28n-0.75Cu alpha-beta alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-6Al-ZSn-4Zr-
`
`2M0 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—4.58n beta alloy; Ti-3Al-
`
`8V-6Cr—4Mo-4Zr beta alloy; and Ti-3Al-13V-1 1 Cr beta alloy (the numbers being
`
`percent by weight). These alloys of titanium include phase stabilizing amounts of
`
`a metal selected from molybdenum, tin, bismuth, tantalum, vanadium, zirconium,
`
`niobium, chromium, cobalt, nickel, manganese, iron, aluminum and lanthanum.
`
`25
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`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-
`
`titanium and alpha-beta-titanium are superior because they are harder and hence
`
`will hold an edge better and still maintain near the flexibility of nickel-titanium to
`
`30
`
`negotiate curved canals. These alpha-titanium, beta-titanium and alpha-beta-
`
`titanium instruments may include medical, dental and endodontic instruments
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`(both hand and engine driven), cutting burs (drills), and enlarging instruments
`
`including hand, mechanical and rotary.
`
`[0029]
`
`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
`
`1O
`
`described below) or uncoated. Today a growing number of physicians and
`
`dentists (endodontists) are utilizing engine driven drills and files with various
`
`names and applications. This aspect of the present invention pertains to the»
`
`fabricatidn of these cutting instruments such as drills and files solely from an
`
`alpha-titanium alloy, a beta-titanium alloy, or an alpha-beta-titanium alloy to
`
`15
`
`produce a sharper cutting edge that should provide for better cutting or a smooth
`
`finished 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 deflection, change the handling properties, or visually exhibit a
`
`20
`
`near failure of the instrument. This aspect of the invention relates to all drills,
`
`burs, files, and instruments used in medicine and dentistry.
`
`[0030]
`
`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
`
`25
`
`instrument longevity. Such an instrument may be manufactured from nickel-
`
`titanium, an alpha-titanium alloy, a beta-titanium 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
`
`30
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`and engine driven), cutting burs (drills), and enlarging instruments including hand,
`
`mechanical and rotary.
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`‘ PCT/US2005/019947
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`[0031]
`
`The coating processes may include but not limited to the following
`
`processes: composite electroless plating (see, e.g., US. Patent Nos. 4,820,547;
`
`4,997,686; 5,145,517; 5,300,330; 5,863,616; and 6,306,466); chemical vapor
`
`deposition (see, e.g., US. Patent No. 4,814,294); microwave deposition (see,
`
`e.g., U.S. Patent No. 4,859,493); laser ablation process (see, e.g., US. Patent
`
`No. 5,299,937); ion beam assisted deposition (see, e.g., US. Patent No.
`
`5,725,573); physical vapor deposition (see, e.g., US. Patent Nos. 4,670,024,
`
`4,776,863, 4,984,940, and 5,545,490); Molybdenum Disulfide Coating (M082)
`
`(see, e.g., US. Patent No. 5,037,516 or SAE Standard AM82526);
`
`1O
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`electropolishing; coatings including titanium nitride and titanium aluminum nitride
`
`commercially available under the trademark FirexTM; coatings such as titanium
`
`nitride (TiN), titanium carbonitride (TiCN), titanium aluminum nitride (TiAlN),
`
`aluminum titanium nitride (AlTiN); or multiple coatings or combinations of coatings.
`
`[0032]
`
`As detailed above, present medical and dental practice entails cutting of
`
`15
`
`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. These can be manufactured as hand,
`
`mechanical and rotary instruments. Today a growing number of physicians and
`
`20
`
`dentists (endodontists) are utilizing engine driven drills and files 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 files to produce a sharper cutting edge and a higher resistance to
`
`heat degradation that should provide for better cutting, a smooth surface and/or
`
`25
`
`different metallurgical properties than the material from which it was
`
`manufactured. 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 withstand more torque,
`
`,30
`
`rotate through a larger angle of deflection, change the handling properties,
`
`remove shape memory or visually exhibit a near failure of the instrument. This
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`aspect of the invention relates to all drills, burs, files, and instruments used in
`
`medicine and dentistry.
`
`[0033]
`
`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
`multilayer process utilizing a titanium nitride coating and then a titanium aluminum
`
`nitride coating. This last coating process is commercially available under the
`
`trademark FIREXTM.
`
`[0034]
`
`Another example process of this aspect of the present invention for
`
`1O
`
`such instruments is a metal or metal alloy coating incorporating particulate matter.
`
`One process to produce such a coating to an instrument includes contacting 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 essentially insoluble or
`
`15
`
`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 sufficient to produce a metallic coating with
`
`the particulate matter dispersed.
`
`Examples
`
`20
`
`[0035]
`
`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
`
`[0036]
`
`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size 82 files,
`
`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were
`
`25
`
`used in a study of torsion (Mt) reported in g-cm performed in accordance with “ISO
`
`Standard 3630-1 Dentistry - Root-canal instruments - Part 1: General
`
`requirements" and “ANSI/ADA Specification No. 28, Endodontic files and
`
`reamers". The results are shown in Figure 3. The files were made from a titanium
`
`alloy comprising 54-57 weight percent nickel and 43-46 weight percent titanium,
`
`30
`
`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) files. Ten of each ISO size were heat-treated in a furnace in
`
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`an argon atmosphere at 500°C for 75 minutes. These are labeled “"TI' in Figure
`
`3. Ten of each ISO size were coated with titanium nitride using physical vapor
`
`deposition with an inherent heat-treatment. These are labeled “Ti-N" in Figure 3.
`
`MI was determined for each of the thirty files in each size, and the mean and
`
`standard deviation for each group (Control, Tl', Ti-N) of ten files were calculated.
`
`The ten files in all but one size that were heat-treated in a furnace in an argon
`
`atmosphere at 500°C for 75 minutes showed the best result with the highest Mt.
`
`Example 2
`
`[0037]
`
`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size 82 files,
`
`10
`
`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were
`
`used in a study of torsion (At) reported in degrees of deflection performed in
`
`accordance with “ISO Standard 3630-1 Dentistry - Root-canal instruments - Part
`
`1: General requirements" and “ANSI/ADA Specification No. 28, Endodontic files
`
`and reamers”. The results are shown in Figure 4. The files were made from a
`
`15
`
`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) files. Ten of each ISO size were heat-treated in a
`
`furnace in an argon atmosphere at 500°C for 75 minutes. These are labeled ""TT
`
`20
`
`in Figure 4. Ten of each ISO size were coated with titanium nitride using physical
`
`vapor deposition with an inherent heat-treatment. These are labeled “Ti-N” in
`
`Figure 4. A: was determined for each of the thirty files in each size, and the mean
`
`and standard deviation for each group (Control, TT, Ti-N) of ten files were
`
`Calculated. The ten files in each size that were heat-treated in a furnace in an
`
`25
`
`argon atmosphere at 500°C for 75 minutes showed the best results with the
`
`highest At.
`
`Example 3
`
`[0038]
`
`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size S2 files,
`
`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were
`
`30
`
`used in a study of maximUm torque at 45° of flexion (Mf) reported in g-cm
`
`performed in accordance with “ISO Standard 3630-1 Dentistry - Root-canal
`
`instruments - Part 1: General requirements” and “ANSI/ADA Specification No. 28,
`
`-11-
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`Endodontic files and reamers". The shank is held in a torque meter, flexed at an
`
`angle of 45°, and then torque is measured. The results are shown in Figure 5.
`
`The files 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) files. Ten of each ISO size
`
`were heat-treated in a furnace in an argon atmosphere at 500°C for 75 minutes.
`
`These are labeled “”‘IT in Figure 5. Ten of each ISO size were coated with
`
`titanium nitride using physical vapor deposition with an inherent heat-treatment.
`
`10
`
`These are labeled “Ti-