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`115207.00009
`
`Attorney Docket No.
`
`"""'
`
`First Inventor
`
`Title
`
`Neill H. Luebke
`
`Dental and Medical Instruments Comprising Titanium
`
`UTILITY
`PATENT APPLICATION
`TRANSMITTAL
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`r
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`'
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`(Only for new nonprovisional applications under 37 CFR 1.53(b))
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`.I
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`of prior application No.: .1.~/~_3_E),_~!~ .............
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`/Richard T. Roche/
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`Richard T. Roche
`
`1 Date April 25, 2012
`Registration No. I
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`16630580
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`IPR2015-01476 - Ex. 1107
`US ENDODONTICS, LLC., Petitioner
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`

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`Dental and Medical Instruments Comprising Titanium
`
`Docket No.: 115207.00009
`
`CROSS-REFERENCES TO RELATED APPLICATIONS
`
`[0001]
`
`This application is a continuation of U.S. Patent Application No. 13/336,579
`
`filed December 23, 2011, which is a continuation of U.S. Patent Application No.
`
`12/977,625 filed December 23, 2010, now U.S. Patent No. 8,083,873, which is a
`
`5
`
`divisional application of U.S. Patent Application No. 11/628,933, now U.S. Patent No.
`
`8,062,033, filed December 7, 2006 which is a 371 of PCT/US05/19947 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
`
`10
`
`[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,
`
`15
`
`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
`
`20
`
`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
`
`25
`
`enamel 1 0 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
`
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`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
`
`5
`
`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
`
`10
`
`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
`
`15
`
`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
`
`20
`
`to fit the curved shape of the canal due to the flexibility of the small diameter file. In
`
`Figure 1 a, 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 1 b that extend along its
`
`25
`
`lower portion. The flutes 51 define a cutting edge. A helical land 53 is positioned
`
`between axially adjacent flutes as shown in Figure 1 b.
`
`[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
`
`30
`
`through the curved portion of the canal. In some cases, the relatively inflexible file
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`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 files, particularly with the respect to
`
`the instruments of larger diameter.
`[0010]
`
`Various solutions have been proposed to limit the problems encountered
`
`5
`
`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
`
`10
`
`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
`
`15
`
`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
`
`20
`
`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
`
`25
`
`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
`
`30
`
`endodontic instrument for use in performing root canal therapy on a tooth. The
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`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.
`
`5
`
`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
`
`10
`
`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(cid:173)
`
`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
`
`15
`
`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
`
`description, drawings, and appended claims.
`
`20
`
`25
`
`[0015]
`[0016]
`[0017]
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`
`Figure 1 is a cross-sectional view of a tooth.
`
`Figure 1 a is a side elevational view of an endodontic instrument.
`
`Figure 1 b is a partial detailed view of the shank of the endodontic
`
`instrument shown in Figure 1 a.
`[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,
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`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-
`
`5
`
`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
`
`10
`
`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
`
`15
`
`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
`
`20
`
`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
`
`25
`
`instrument for use in performing root canal therapy on a tooth. This embodiment of
`
`the invention is an endodontic instrument as shown in Figure 1 a 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
`
`30
`
`about 0.5 to about 1.6 millimeters. The shank 42 may include calibrated depth
`
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`markings 45 and further includes a distal end 48. The shank 42 includes two
`
`continuous helical flutes 51 as shown in Figure 1 b 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 1 b.
`[0025]
`
`The shank 42 comprises a titanium alloy, and is prepared by heat-treating
`
`5
`
`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 400oc 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
`
`1 0
`
`consisting of he I ium, 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(cid:173)
`
`treated at 500oc 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(cid:173)
`
`15
`
`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-5AI-2.5Sn alpha alloy; Ti-5AI-2.5Sn(cid:173)
`
`ELI (low 02) alpha alloy; Ti-3AI-2.5V alpha alloy; Ti-5AI-5Zr-5Sn alpha alloy; Ti-6AI-
`
`20
`
`2Cb-1Ta-0.8Mo alpha alloy; Ti-5AI-5Sn-2Zr-2Mo-0.25Si near alpha alloy; Ti-6AI-2Nb-
`
`1Ta-1Mo near alpha alloy; Ti-8AI-1Mo-1V near alpha alloy; Ti-6AI-2Sn-4Zr-2Mo near
`
`alpha alloy; Ti-6AI-2Sn-1.5Zr-1 Mo-0.35Bi-0.1 Si near alpha alloy; Ti-2.25-AI-11 Sn-
`
`5Zr-1 Mo-0.2Si near alpha alloy; Ti-3AI-2.5V alpha-beta alloy; Ti-1 OV-2Fe-3AI alpha(cid:173)
`
`beta alloy; Ti-5AI-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6AI-2Sn-4Zr-6Mo alpha-beta
`
`25
`
`alloy; Ti-4AI-4Mn alpha-beta alloy; Ti-6AI-2Sn-2Zr-2Mo-2Cr-0.25Si alpha-beta alloy;
`
`Ti-4AI-3Mo-1V alpha-beta alloy; Ti-6AI-2Sn-4Zr-6Mo alpha-beta alloy; Ti-11 Sn-5Zr-
`
`2AI-1 Mo alpha-beta alloy; Ti-6AI-4V alpha-beta alloy; Ti-6AI-4V-ELI (low 02) alpha(cid:173)
`
`beta alloy; Ti-6AI-6V-2Sn-0.75Cu alpha-beta alloy; Ti-7AI-4Mo alpha-beta alloy; Ti-
`
`6AI-2Sn-4Zr-2Mo alpha-beta alloy; Ti-5AI-1.5Fe-1.5Cr-1.5Mo alpha-beta alloy; Ti-
`
`30
`
`8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3AI beta alloy; Ti-11.5Mo-6Zr-4.5Sn beta alloy;
`
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`Ti-3AI-8V-6Cr-4Mo-4Zr beta alloy; and Ti-3AI-13V-11 Cr 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
`
`5
`
`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
`
`10
`
`instrument for use in performing root canal therapy on a tooth. This embodiment of
`
`the invention is an endodontic instrument as shown in Figure 1 a 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
`
`15
`
`markings 45 and further includes a distal end 48. The shank 42 includes two
`
`continuous helical flutes 51 as shown in Figure 1 b, 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 1 b. The endodontic instrument is
`
`fabricated solely from an alpha-titanium alloy, a beta-titanium alloy, or an alpha-beta-
`
`20
`
`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-5AI-2.5Sn
`
`alpha alloy; Ti-5AI-2.5Sn-ELI (low 02) alpha alloy; Ti-3AI-2.5V alpha alloy; Ti-5AI-5Zr-
`
`5Sn alpha alloy; Ti-6AI-2Cb-1Ta-0.8Mo alpha alloy; Ti-5AI-5Sn-2Zr-2Mo-0.25Si near
`
`25
`
`alpha alloy; Ti-6AI-2Nb-1 Ta-1 Mo near alpha alloy; Ti-8AI-1 Mo-1V near alpha alloy;
`
`Ti-6AI-2Sn-4Zr-2Mo near alpha alloy; Ti-6AI-2Sn-1.5Zr-1 Mo-0.35Bi-0.1 Si near alpha
`
`alloy; Ti-2.25-AI-11 Sn-5Zr-1 Mo-0.2Si near alpha alloy; Ti-3AI-2.5V alpha-beta alloy;
`
`Ti-1 OV-2Fe-3AI alpha-beta alloy; Ti-5AI-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6AI-
`
`2Sn-4Zr-6Mo alpha-beta alloy; Ti-4AI - 4Mn alpha-beta alloy; Ti-6AI-2Sn-2Zr-2Mo-
`
`30
`
`2Cr-0.25Si alpha-beta alloy; Ti-4AI-3Mo-1V alpha-beta alloy; Ti-6AI-2Sn-4Zr-6Mo
`
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`alpha-beta alloy; Ti-11 Sn-5Zr-2AI-1 Mo alpha-beta alloy; Ti-6AI-4V alpha-beta alloy;
`
`Ti-6AI-4V-ELI (low 02) alpha-beta alloy; Ti-6AI-6V-2Sn-0.75Cu alpha-beta alloy; Ti-
`
`7 AI-4Mo alpha-beta alloy; Ti-6AI-2Sn-4Zr-2Mo alpha-beta alloy; Ti-5AI-1.5Fe-1.5Cr-
`
`1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3AI beta alloy; Ti-
`
`5
`
`11.5Mo-6Zr-4.5Sn beta alloy; Ti-3AI-8V-6Cr-4Mo-4Zr beta alloy; and Ti-3AI-13V-
`
`11 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. An endodontic instrument according to
`
`10
`
`this embodiment of the invention has improved sharpness, cutting ability, and
`
`instrument longevity compared to instruments fabricated from untreated nickel(cid:173)
`
`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 negotiate curved canals. These alpha-titanium, beta-
`
`15
`
`titanium and alpha-beta-titanium instruments may include medical, dental and
`
`endodontic instruments (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
`
`20
`
`nickel-titanium. Present endodontic practice entails the preparation, cleaning, and
`
`shaping of root canals in teeth utilizing carbide steel, stainless steel and nickel(cid:173)
`
`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(cid:173)
`
`titanium alloy to fabricate these instruments. It may be coated (as described below)
`
`25
`
`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 fabrication 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 produce a sharper cutting edge that should provide for
`
`30
`
`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. 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 near failure of the instrument. This aspect of the invention relates to
`
`5
`
`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 instrument longevity.
`
`Such an instrument may be manufactured from nickel-titanium, an alpha-titanium
`
`10
`
`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 and engine driven), cutting burs (drills), and
`
`enlarging instruments including hand, mechanical and rotary.
`[0031]
`
`The coating processes may include but not limited to the following
`
`15
`
`processes: composite electroless plating (see, e.g., U.S. 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., U.S. Patent No. 4,814,294); microwave deposition (see, e.g.,
`
`U.S. Patent No. 4,859,493); laser ablation process (see, e.g., U.S. Patent No.
`
`20
`
`5,299,937); ion beam assisted deposition (see, e.g., U.S. Patent No. 5,725,573);
`
`physical vapor deposition (see, e.g., U.S. Patent Nos. 4,670,024, 4,776,863,
`
`4,984,940, and 5,545,490); electropolishing; coatings including titanium nitride and
`
`titanium aluminum nitride commercially available under the trademark Firex™;
`
`coatings such as titanium nitride (TiN), titanium carbonitride (TiCN), titanium
`
`25
`
`aluminum nitride (TiAIN), aluminum titanium nitride (AITiN); or multiple coatings or
`
`combinations of coatings.
`
`[0032]
`
`As detailed above, 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
`
`30
`
`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
`
`and rotary instruments. 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 application of
`
`5
`
`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 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.
`
`10
`
`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, rotate through a larger angle of deflection,
`
`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, files,
`
`15
`
`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
`
`20
`
`coating. This last coating process is commercially available under the trademark
`
`FIREX™.
`
`[0034]
`
`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 contacting the surface of
`
`25
`
`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 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
`
`30
`
`for a time sufficient to produce a metallic coating with the particulate matter
`
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`dispersed.
`
`5
`
`[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.
`
`Examples
`
`Example 1
`
`[0036]
`
`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
`
`10
`
`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, and included an elongate
`
`15
`
`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 500oc for 75
`
`minutes and then slowly cooled. These are labeled "TT" in Figure 3. Ten of each
`
`ISO size were coated with titanium nitride using physical vapor deposition with an
`
`20
`
`inherent heat-treatment. These are labeled "Ti-N" in Figure 3. Mt was determined for
`
`each of the thirty files, and the mean and standard deviation for each group (Control,
`
`TT, Ti-N) of ten files were calculated. The ten files that were heat-treated in a
`
`furnace in an argon atmosphere at 500oc for 75 minutes showed the best result with
`
`the highest Mt.
`
`25
`
`Example 2
`
`[0037]
`
`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
`
`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
`
`30
`
`requirements and ANSI/ADA Specification No. 28, Endodontic files and reamers".
`
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`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
`
`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
`
`5
`
`(Control) files. Ten of each ISO size were heat-treated in a furnace in an argon
`
`atmosphere at 500oc 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
`
`4. At was determined for each of the thirty files, and the mean and standard
`
`10
`
`deviation for each group (Control, TT, Ti-N) of ten files were calculated. The ten files
`
`that were heat-treated in a furnace in an argon atmosphere at 500oc 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,
`
`15
`
`thirty ISO size F1 files, thirty ISO size F2 files and thirty ISO size F3 files were used
`
`in a study of maximum torque at 45° of flexion (Mf) reported in g ·em 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 shank is held in a torque meter, flexed at an angle of 45°, and then
`
`20
`
`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 inc