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`Docket No.: 115207.00005
`
`Dental and Medical Instruments Comprising Titanium
`
`CROSS-REFERENCES TO RELATED APPLICATIONS
`
`[0001]
`
`This application is a divisional application of U.S. Patent Application No.
`
`11/628,933 filed December 7, 2006 which is a 371 of PCT/USO5/19947 filed June 7,
`
`2005 which claims priority from United States Patent Application No. 60/578,091 filed
`
`June 8, 2004.
`
`STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH
`
`[0002]
`
`Not Applicable.
`
`1. Field of the Invention
`
`BACKGROUND 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 drills,
`
`burs and files, and to endodontic instruments such as drills, burs and files used by
`
`dentists.
`
`2. Description of the Related Art
`
`[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.
`
`[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
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`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
`
`Figure 2d with file 34, to result in a fully excavated cavity 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 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 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.
`
`[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 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
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`the instruments of larger diameter.
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`[0010]
`
`Various solutions have been proposed to limit the problems encountered
`
`when cleaning and enlarging a curved root canal with a file. For example, U.S.
`
`Patent No. 4,443,193 describes a shaped endodontic instrument that is said to solve
`
`this problem. U.S. Patent 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 U.S. 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.) U.S. 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. U.S. Patent
`
`No. 6,315,558 proposes 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 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
`
`[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 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.
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`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 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 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
`
`10
`
`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 detailed
`
`15
`
`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
`
`20
`
`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 - 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 “ISO Standard 3630-1 Dentistry -
`
`Root-canal instruments - Part 1: General requirements and ANSI/ADA Specification
`
`25
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`30
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`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-:::e:::-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” for untreated (Control)
`
`files, heat-treated files (TT), and titanium nitride coated files (Ti-N).
`
`[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 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 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
`
`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.
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`[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 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 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.
`
`[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-2.5Sn 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-22r—2Mo-0.25Si 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-0.35Bi-0.1Si near alpha alloy; Ti-2.25-Al-11Sn-
`
`5Zr-1Mo-0.28i near alpha alloy; Ti-3Al-2.5V alpha-beta alloy; Ti-10V-2Fe-3Al alpha-
`
`beta alloy; Ti-5Al-28n-22r—4Mo-4Cr alpha-beta alloy; Ti-6Al-28n-4Zr-6Mo alpha-beta
`
`alloy; Ti-4Al-4Mn alpha-beta alloy; Ti-6Al-28n-ZZr-2Mo-2Cr-0.25Si 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-0.75Cu alpha-beta alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-
`
`6Al-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-4.5Sn 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
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`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.
`
`[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 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 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-2.5Sn
`
`alpha alloy; Ti-5Al-2.5Sn-EL| (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;
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`Ti-6Al-2Sn-4Zr—2Mo near alpha alloy; Ti-6Al-2Sn-1.5Zr-1Mo-0.35Bi-0.1Si near alpha
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`alloy; Ti-2.25-Al-11Sn-5Zr-1Mo-0.2Si near alpha alloy; Ti-3Al-2.5V alpha-beta alloy;
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`Ti-10V-2Fe-3Al alpha-beta alloy; Ti-5Al-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6Al-
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`2Sn-4Zr-6Mo alpha-beta alloy; Ti-4Al - 4Mn alpha-beta alloy; Ti-6Al-2Sn-2Zr-2Mo-
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`2Cr-0.25Si alpha-beta alloy; Ti-4Al-3Mo-1V alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo
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`alpha-beta alloy; Ti-11Sn-5Zr—2Al-1Mo alpha-beta alloy; Ti-6Al-4V alpha-beta alloy;
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`Ti-6Al-4V-ELI (low 02) alpha-beta alloy; Ti-6Al-6V-2Sn-0.75Cu alpha-beta alloy; Ti-
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`7Al-4Mo alpha-beta alloy; Ti-6Al-2Sn-4Zr—2Mo alpha-beta alloy; Ti-5Al-1.5Fe-1.5Cr-
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`1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3Al beta alloy; Ti-
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`11.5Mo-6Zr—4.5Sn beta alloy; Ti-3Al-8V-6Cr—4Mo-4Zr beta alloy; and Ti-3Al-13V-
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`11Cr beta alloy (the numbers being percent by weight). These alloys of titanium
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`include phase stabilizing amounts of a metal selected from molybdenum, tin,
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`bismuth, tantalum, vanadium, zirconium, niobium, chromium, cobalt, nickel,
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`manganese, iron, aluminum and lanthanum. An endodontic instrument according to
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`this embodiment of the invention has improved sharpness, cutting ability, and
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`instrument longevity compared to instruments fabricated from untreated nickel-
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`titanium. Alpha-titanium, beta-titanium and alpha-beta-titanium are superior because
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`they are harder and hence will hold an edge better and still maintain near the
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`flexibility of nickel-titanium to negotiate curved canals. These alpha-titanium, beta-
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`titanium and alpha-beta-titanium instruments may include medical, dental and
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`endodontic instruments (both hand and engine driven), cutting burs (drills), and
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`enlarging instruments including hand, mechanical and rotary.
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`[0029]
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`Present medical and dental practice entails cutting of hard tissues such as
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`bone or teeth with instruments manufactured of carbide steel, stainless steel and
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`nickel-titanium. Present endodontic practice entails the preparation, cleaning, and
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`shaping of root canals in teeth utilizing carbide steel, stainless steel and nickel-
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`titanium instruments for hand, mechanical and rotary applications. This version of the
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`invention would use an alpha-titanium alloy, a beta-titanium alloy, or an alpha-beta-
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`titanium alloy to fabricate these instruments.
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`It may be coated (as described below)
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`or uncoated. Today a growing number of physicians and dentists (endodontists) are
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`utilizing engine driven drills and files with various names and applications. This
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`aspect of the present invention pertains to the fabrication of these cutting instruments
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`such as drills and files solely from an alpha-titanium alloy, a beta-titanium alloy, or an
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`alpha-beta-titanium alloy to produce a sharper cutting edge that should provide for
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`better cutting or a smooth finished surface. This includes instrumentation that will
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`facilitate the cleaning and sealing of the root canal system.
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`In addition, a coating or
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`heat-treatment may relieve stress in the instrument to allow it to withstand more
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`torque, rotate through a larger angle of deflection, change the handling properties, or
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`visually exhibit a near failure of the instrument. This aspect of the invention relates to
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`all drills, burs, files, and instruments used in medicine and dentistry.
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`[0030]
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`In another aspect, the present invention provides for coating and optionally
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`thereafter heat-treating dental and medical instruments including the coatings to
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`maintain and/or improve their sharpness, cutting ability, and/or instrument longevity.
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`Such an instrument may be manufactured from nickel-titanium, an alpha-titanium
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`alloy, a beta-titanium alloy, or an alpha-beta-titanium alloy, stainless steel, carbide
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`steel, as well as other materials. These instruments may be electropolished before
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`or after coating or heat-treating. These instruments will include medical, dental and
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`endodontic instruments (both hand and engine driven), cutting burs (drills), and
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`enlarging instruments including hand, mechanical and rotary.
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`[0031]
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`The coating processes may include but not limited to the following
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`processes: composite electroless plating (see, e.g., U.S. Patent Nos. 4,820,547;
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`4,997,686; 5,145,517; 5,300,330; 5,863,616; and 6,306,466); chemical vapor
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`deposition (see, e.g., US. Patent No. 4,814,294); microwave deposition (see, e.g.,
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`US. Patent No. 4,859,493); laser ablation process (see, e.g., US. Patent No.
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`5,299,937); ion beam assisted deposition (see, e.g., US. Patent No. 5,725,573);
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`physical vapor deposition (see, e.g., US. Patent Nos. 4,670,024, 4,776,863,
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`4,984,940, and 5,545,490); electropolishing; coatings including titanium nitride and
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`titanium aluminum nitride commercially available under the trademark FirexT'V';
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`coatings such as titanium nitride (TiN), titanium carbonitride (TiCN), titanium
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`aluminum nitride (TiAlN), aluminum titanium nitride (AlTiN); or multiple coatings or
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`combinations of coatings.
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`[0032]
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`As detailed above, present medical and dental practice entails cutting of
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`hard tissues such as bone or teeth with instruments manufactured of carbide steel,
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`stainless steel and nickel-titanium. Present endodontic practice entails the
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`preparation, cleaning, and shaping of root canals in teeth utilizing carbide steel,
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`stainless steel and nickel-titanium. These can be manufactured as hand, mechanical
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`and rotary instruments. Today a growing number of physicians and dentists
`
`(endodontists) are utilizing engine driven drills and files with various names and
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`applications. This aspect of the present invention pertains to the application of
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`coatings and optionally heat-treatment to cutting instruments such as drills and files
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`to produce a sharper cutting edge and a higher resistance to heat degradation that
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`should provide for better cutting, a smooth surface and/or different metallurgical
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`properties than the material from which it was manufactured. This includes
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`instrumentation that will facilitate the cleaning and sealing of the root canal system.
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`In addition, a heat-treatment separately applied or as utilized in the coating process
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`may relieve stress in the instrument which should allow for more instrument longevity
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`by the ability to withstand more torque, rotate through a larger angle of deflection,
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`change the handling properties, remove shape memory or visually exhibit a near
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`failure of the instrument. This aspect of the invention relates to all drills, burs, files,
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`and instruments used in medicine and dentistry.
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`[0033]
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`One example process of this aspect of the present invention for such
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`instruments is a titanium nitride coating. This coating process is done with physical
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`vapor deposition with an inherent heat-treatment. Another process is a multilayer
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`process utilizing a titanium nitride coating and then a titanium aluminum nitride
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`coating. This last coating process is commercially available under the trademark
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`FIREXT'V'.
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`[0034]
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`Another example process of this aspect of the present invention for such
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`instruments is a metal or metal alloy coating incorporating particulate matter. One
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`process to produce such a coating to an instrument includes contacting the surface of
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`the instrument with a stable electroless metallizing bath comprising a metal salt, an
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`electroless reducing agent, a complexing agent, an electroless plating stabilizer, a
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`quantity of particulate matter which is essentially insoluble or sparingly soluble in the
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`metallizing bath, and a particulate matter stabilizer, and maintaining the particulate
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`matter in suspension in the metallizing bath during the metallizing of the instrument
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`for a time sufficient to produce a metallic coating with the particulate matter
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`dispersed.
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`Examples
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`[0035]
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`The following Examples have been presented in order to further illustrate
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`the invention and are not intended to limit the invention in any way.
`
`Example 1
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`[0036]
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`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size S2 files,
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`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were used
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`in a study of torsion (Mt) reported in g-:::s:::-cm performed in accordance with “ISO
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`Standard 3630-1 Dentistry - Root-canal instruments - Part 1: General requirements
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`and ANSI/ADA Specification No. 28, Endodontic files and reamers”. The results are
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`shown in Figure 3. The files were made from a titanium alloy comprising 54-57
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`weight percent nickel and 43-46 weight percent titanium, and included an elongate
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`shank having a cutting edge extending from a distal end of the shank along an axial
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`length of the shank. Ten of each ISO size were untreated (Control) files. Ten of
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`each ISO size were heat-treated in a furnace in an argon atmosphere at 500°C for 75
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`minutes and then slowly cooled. These are labeled “TT” in Figure 3. Ten of each
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`ISO size were coated with titanium nitride using physical vapor deposition with an
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`inherent heat-treatment. These are labeled “Ti-N” in Figure 3. M was determined for
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`each of the thirty files, and the mean and standard deviation for each group (Control,
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`TT, Ti-N) of ten files were calculated. The ten files that were heat-treated in a
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`furnace in an argon atmosphere at 500°C for 75 minutes showed the best result with
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`the highest Mt.
`
`Example 2
`
`[0037]
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`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 used
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`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 titanium alloy
`
`comprising 54-57 weight percent nickel and 43-46 weight percent titanium, and
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`included an elongate shank having a cutting edge extending from a distal end of the
`
`-11-
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`shank along an axial length of the shank. Ten of each ISO size were untreated
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`(Control) files. Ten of each ISO size were heat-treated in a furnace in an argon
`
`atmosphere at 500°C for 75 minutes and then slowly cooled. These are labeled “TT”
`
`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
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`4. A was determined for each of the thirty files, and the mean and standard
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`deviation for each group (Control, TT, Ti-N) of ten files were calculated. The ten files
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`that were heat-treated in a furnace in an argon atmosphere at 500°C for 75 minutes
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`showed the best results with the highest At.
`
`Example 3
`
`[0038]
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`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size SZ files,
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`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were used
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`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:
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`General requirements and ANSI/ADA Specification No. 28, Endodontic files and
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`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 and then slowly cooled. These are
`
`labeled “TT” in Figure 5 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 5. Mf was determined for each of the thirty files, and the mean and
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`standard deviation for each group (Control, TT, Ti-N) of ten files were calculated.
`
`It
`
`can be seen that the heat-treated files can withstand increased strain, and have
`
`higher high flexibility, have higher resistance to torsion breakage than untreated
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`(control) files.
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`Example 4
`
`[0039]
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`Thirty ISO size SX files, thirty ISO size S1 files, thirty ISO size SZ files,
`
`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were used
`
`in 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