Source: https://patents.google.com/patent/US8876991B2/en
Timestamp: 2019-05-27 01:24:26
Document Index: 84724339

Matched Legal Cases: ['Application No. 60', 'art 1', 'art 1', 'art 1', 'art 1', 'art 2', 'art 1', 'art 1', 'art 1', 'art 1', 'art 2', 'art 3', 'art 3']

US8876991B2 - Dental and medical instruments comprising titanium - Google Patents
Dental and medical instruments comprising titanium Download PDF
US8876991B2
US8876991B2 US14/167,311 US201414167311A US8876991B2 US 8876991 B2 US8876991 B2 US 8876991B2 US 201414167311 A US201414167311 A US 201414167311A US 8876991 B2 US8876991 B2 US 8876991B2
US14/167,311
US20140144022A1 (en
Neill Hamilton Luebke
Gold Standard Instruments LLC
2004-06-08 Priority to US57809104P priority Critical
2005-06-07 Priority to PCT/US2005/019947 priority patent/WO2005122942A1/en
2006-12-07 Priority to US62893306A priority
2010-12-23 Priority to US12/977,625 priority patent/US8083873B2/en
2011-12-23 Priority to US13/336,579 priority patent/US8562341B2/en
2012-04-25 Priority to US13/455,841 priority patent/US8727773B2/en
2014-01-29 Priority to US14/167,311 priority patent/US8876991B2/en
2014-01-29 Application filed by Gold Standard Instruments LLC filed Critical Gold Standard Instruments LLC
2014-01-30 Assigned to Gold Standard Instruments, LLC reassignment Gold Standard Instruments, LLC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LUEBKE, NEILL HAMILTON
2014-05-29 Publication of US20140144022A1 publication Critical patent/US20140144022A1/en
2014-06-24 First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=35509410&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=US8876991(B2) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
2014-11-04 Publication of US8876991B2 publication Critical patent/US8876991B2/en
2015-08-03 PTAB case PGR2015-00019 filed (Final Written Decision) litigation https://portal.unifiedpatents.com/ptab/case/PGR2015-00019 Petitioner: Institution date: 2016-01-29 Termination date: 2016-12-28 "Unified Patents PTAB Data" by Unified Patents is licensed under a Creative Commons Attribution 4.0 International License.
A61C5/023—
C22F1/004—Heat treatment in fluid bed
C23C8/30—Carbo-nitriding
Endodontic instruments 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.
This application is a continuation of U.S. patent application Ser. No. 13/455,841 filed Apr. 25, 2012, which is a continuation of U.S. patent application Ser. No. 13/336,579 filed Dec. 23, 2011, now U.S. Pat. No. 8,562,341, which is a continuation of U.S. patent application Ser. No. 12/977,625 filed Dec. 23, 2010, now U.S. Pat. No. 8,083,873, which is a divisional application of U.S. patent application Ser. No. 11/628,933, now U.S. Pat. No. 8,062,033, filed Dec. 7, 2006 which is a 371 of PCT/US05/19947 filed Jun. 7, 2005 which claims priority from U.S. Patent Application No. 60/578,091 filed Jun. 8, 2004.
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 FIG. 1 a, there is shown the file 34 of FIG. 2 d 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 FIG. 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 FIG. 1 b.
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 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.
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. 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.
FIG. 1 b is a partial detailed view of the shank of the endodontic instrument shown in FIG. 1 a.
FIGS. 2 a-2 e represent a prior art procedure for preparing a tooth for endodontic restoration.
FIG. 3 is a graph showing the results of a study of torsion (Mt) reported in g⊙cm performed in accordance with “ISO Standard 3630-1 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).
FIG. 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 No. 28, Endodontic files and reamers” for untreated (Control) files, heat-treated files (TT), and titanium nitride coated files (Ti—N).
FIG. 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 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).
FIG. 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).
FIG. 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”.
One embodiment of the invention provides an improved endodontic instrument for use in performing root canal therapy on a tooth. This embodiment of the invention is an endodontic instrument as shown in FIG. 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 markings 45 and further includes a distal end 48. The shank 42 includes two continuous helical flutes 51 as shown in FIG. 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 FIG. 1 b.
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.
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 O2) alpha alloy; Ti-3Al-2.5V alpha alloy; Ti-5Al-5Zr-5Sn alpha alloy; Ti-6Al-2Cb-1Ta-0.8Mo alpha alloy; Ti-5Al-5 Sn-2Zr-2Mo-0.25Si near alpha alloy; Ti-6Al-2Nb-1Ta-1Mo near alpha alloy; Ti-8Al-1Mo-1V near alpha alloy; Ti-6Al-2Sn-4Zr-2Mo near alpha alloy; Ti-6Al-2Sn-1.5Zr-1Mo-0.35Bi-0.1Si near alpha alloy; Ti-2.25-AI-11Sn-5Zr-1Mo-0.25i near alpha alloy; Ti-3Al-2.5V alpha-beta alloy; Ti-10V-2Fe-3Al alpha-beta alloy; Ti-5Al-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta alloy; Ti-4Al-4Mn alpha-beta alloy; Ti-6Al-2Sn-2Zr-2Mo-2Cr-0.25Si alpha-beta alloy; Ti-4Al-3Mo-1V alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta alloy; Ti-11Sn-5Zr-2Al-1Mo alpha-beta alloy; Ti-6Al-4V alpha-beta alloy; Ti-6Al-4V-ELI (low O2) alpha-beta alloy; Ti-6Al-6V-2Sn-0.75Cu alpha-beta alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-6Al-2Sn-4Zr-2Mo alpha-beta alloy; Ti-5Al-1.5Fe-1.5Cr-1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3Al beta alloy; Ti-11.5Mo-6Zr-4.5Sn beta alloy; Ti-3Al-8V-6Cr-4Mo-4Zr beta alloy; and Ti-3Al-13V-11Cr beta alloy (the numbers being percent by weight). An example, nickel-titanium alloy includes 54-57 weight percent nickel and 43-46 weight percent titanium. Preferably, the titanium alloy used for the shank includes 54-57 weight percent nickel and 43-46 weight percent titanium and is commercially available as Nitinol 55. Thus, most preferably, the shank consists essentially of 54-57 weight percent nickel and 43-46 weight percent titanium thereby avoiding the inclusion of elements that affect the superelastic properties of the alloy.
Another embodiment of the invention provides an improved endodontic instrument for use in performing root canal therapy on a tooth. This embodiment of the invention is an endodontic instrument as shown in FIG. 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 markings 45 and further includes a distal end 48. The shank 42 includes two continuous helical flutes 51 as shown in FIG. 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 FIG. 1 b. 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.
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 O2) alpha alloy; Ti-3Al-2.5V alpha alloy; Ti-5Al-5Zr-5Sn alloy; Ti-6Al-2Cb-1Ta-0.8Mo alpha alloy; Ti-5Al-5Sn-2Zr-2Mo-0.25Si near alpha alloy; Ti-6Al-2Nb-1Ta-1Mo near alpha alloy; Ti-8Al-1Mo-1V near alpha alloy; Ti-6Al-2Sn-4Zr-2Mo near alpha alloy; Ti-6Al-2Sn-1.5Zr-1Mo-0.35Bi-0.1Si near alpha alloy; Ti-2.25-Al-11Sn-5Zr-Mo-0.2Si near alpha alloy; Ti-3Al-2.5V alpha-beta alloy; Ti-10V-2Fe-3Al alpha-beta alloy; Ti-5Al-2Sn-2Zr-4Mo-4Cr alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta alloy; Ti-4Al-4Mn alpha-beta alloy; Ti-6Al-2Sn-2Zr-2Mo-2Cr-0.25Si alpha-beta alloy; Ti-4Al-3Mo-1V alpha-beta alloy; Ti-6Al-2Sn-4Zr-6Mo alpha-beta alloy; Ti-11Sn-5Zr-2Al-1Mo alpha-beta alloy; Ti-6Al-4V alpha-beta alloy; Ti-6Al-4V-ELI (low O2) alpha-beta alloy; Ti-6Al-6V-2Sn-0.75Cu alpha-beta alloy; Ti-7Al-4Mo alpha-beta alloy; Ti-6Al-2Sn-4Zr-2Mo alpha-beta alloy; Ti-5Al-1.5Fe-1.5Cr-1.5Mo alpha-beta alloy; Ti-8Mn alpha-beta alloy; Ti-8Mo-8V-2Fe-3Al beta alloy; Ti-11.5Mo-6Zr-4.5Sn beta alloy; Ti-3Al-8V-6Cr-4Mo-4Zr beta alloy; and Ti-3Al-13V-11Cr beta alloy (the numbers being percent by weight). These alloys of titanium include phase stabilizing amounts of a metal selected from molybdenum, tin, bismuth, tantalum, vanadium, zirconium, niobium, chromium, cobalt, nickel, manganese, iron, aluminum and lanthanum. An endodontic instrument according to this embodiment of the invention has improved sharpness, cutting ability, and instrument longevity compared to instruments fabricated from untreated nickel-titanium. Alpha-titanium, beta-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-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.
The coating processes may include but not limited to the following processes: composite electroless plating (see, e.g., U.S. Pat. Nos. 4,820,547; 4,997,686; 5,145,517; 5,300,330; 5,863,616; and 6,306,466); chemical vapor deposition (see, e.g., U.S. Pat. No. 4,814,294); microwave deposition (see, e.g., U.S. Pat. No. 4,859,493); laser ablation process (see, e.g., U.S. Pat. No. 5,299,937); ion beam assisted deposition (see, e.g., U.S. Pat. No. 5,725,573); physical vapor deposition (see, e.g., U.S. Pat. Nos. 4,670,024, 4,776,863, 4,984,940, and 5,545,490); 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 aluminum nitride (TiAlN), aluminum titanium nitride (AITiN); or multiple coatings or combinations of coatings.
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 (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 FIG. 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 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 FIG. 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 FIG. 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 500° C. for 75 minutes showed the best result with the highest Mt.
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 requirements and ANSI/ADA Specification No. 28, Endodontic files and reamers”. The results are shown in FIG. 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 (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 FIG. 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 FIG. 4. At 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 500° C. for 75 minutes showed the best results with the highest At.
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 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, 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 FIG. 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 FIG. 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 FIG. 5. Mf 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. 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 (control) files.
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 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”. The results are shown in FIG. 6. 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 FIG. 6. 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 FIG. 6. ADP 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 500° C. for 75 minutes showed the highest ADP. Thus, the heat-treated files maintain the acquired (test deformed) shape rather than the shape memory exhibited in the untreated control (nickel-titanium instruments).
Six groups of thirty ISO size SX, S1, S2, F1, F2 and F3 files were used in a study of the fatigue reported in cycles (revolutions) to failure 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”. The results are shown in FIG. 7. 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 files of each ISO size were untreated (Control) files. Ten files 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 FIG. 7. Ten files of each ISO size were coated with titanium nitride using physical vapor deposition with an inherent heat-treatment. These are labeled “Ti—N” in FIG. 7. Fatigue cycles were determined for each of the files, and the mean and standard deviation for each group (Control, TT, Ti—N) of the six file sizes were calculated. In five of the six file sizes, the files that were heat-treated in a furnace in an argon atmosphere at 500° C. for 75 minutes showed the highest fatigue cycles (revolutions) to failure.
1. A method for manufacturing or modifying a dental instrument or device, the method comprising:
(a) providing a dental instrument or device including an elongated shank comprising a superelastic nickel titanium alloy, and
(b) after step (a), heat-treating the entire instrument or device at a temperature above 25° C. up to but not equal to the melting point of the superelastic nickel titanium alloy, wherein the heat-treated instrument or device has an angle greater than 10 degrees of permanent deformation after torque at 45° of flexion when tested in accordance with ISO Standard 3630-1.
step (b) further comprises heat-treating the entire instrument or device in an atmosphere consisting essentially of a gas unreactive with the instrument or device.
the instrument or device consists essentially of a titanium alloy comprising 54-57 weight percent nickel.
the instrument or device is heat-treated for 1 to 2 hours.
the instrument or device is an endodontic instrument or device.
6. A method for manufacturing or modifying a dental instrument or device, the method comprising:
(b) after step (a), heat-treating the entire instrument or device at a temperature of 300° C. up to but not equal to the melting point of the superelastic nickel titanium alloy, wherein the heat-treated instrument or device has an angle greater than 10 degrees of permanent deformation after torque at 45° of flexion when tested in accordance with ISO Standard 3630-1.
the instrument shank is heat-treated for 1 to 2 hours.
12. A method for manufacturing or modifying an endodontic instrument for use in performing root canal therapy on a tooth, the method comprising:
(a) providing an elongate shank having a cutting edge extending from a distal end of the shank along an axial length of the shank, the shank comprising a superelastic nickel titanium alloy, and
(b) after step (a), heat-treating the entire shank at a temperature above 25° C. up to but not equal to the melting point of the superelastic nickel titanium alloy,
wherein the heat treated shank has an angle greater than 10 degrees of permanent deformation after torque at 45 degrees of flexion when tested in accordance with ISO Standard 3630-1.
step (b) is performed in an atmosphere that is unreactive, ambient or any other acceptable heat treatment process.
the temperature is from 300° C. up to but not equal to the melting point of the superelastic nickel titanium alloy.
the instrument shank has a diameter of 0.5 to 1.6 millimeters.
the instrument shank consists essentially of a titanium alloy comprising 54-57 weight percent nickel.
US14/167,311 2004-06-08 2014-01-29 Dental and medical instruments comprising titanium Active US8876991B2 (en)
US57809104P true 2004-06-08 2004-06-08
PCT/US2005/019947 WO2005122942A1 (en) 2004-06-08 2005-06-07 Dental and medical instruments comprising titanium
US62893306A true 2006-12-07 2006-12-07
US12/977,625 US8083873B2 (en) 2004-06-08 2010-12-23 Dental and medical instruments comprising titanium
US13/336,579 US8562341B2 (en) 2004-06-08 2011-12-23 Dental and medical instruments comprising titanium
US13/455,841 US8727773B2 (en) 2004-06-08 2012-04-25 Dental and medical instruments comprising titanium
US14/167,311 US8876991B2 (en) 2004-06-08 2014-01-29 Dental and medical instruments comprising titanium
US14/522,013 US9314316B2 (en) 2004-06-08 2014-10-23 Dental and medical instruments comprising titanium
US14/722,840 US9732410B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US14/722,390 US10023949B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US14/722,309 US10023948B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US15/671,349 US10047428B2 (en) 2004-06-08 2017-08-08 Dental and medical instruments comprising titanium
US16/021,917 US20180305803A1 (en) 2004-06-08 2018-06-28 Dental and Medical Instruments Comprising Titanium
US13/455,841 Continuation US8727773B2 (en) 2004-06-08 2012-04-25 Dental and medical instruments comprising titanium
US14/522,013 Continuation US9314316B2 (en) 2004-06-08 2014-10-23 Dental and medical instruments comprising titanium
US20140144022A1 US20140144022A1 (en) 2014-05-29
US8876991B2 true US8876991B2 (en) 2014-11-04
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US11/628,933 Active US8062033B2 (en) 2004-06-08 2005-06-07 Dental and medical instruments comprising titanium
US12/977,625 Active US8083873B2 (en) 2004-06-08 2010-12-23 Dental and medical instruments comprising titanium
US13/336,579 Active US8562341B2 (en) 2004-06-08 2011-12-23 Dental and medical instruments comprising titanium
US13/455,841 Active US8727773B2 (en) 2004-06-08 2012-04-25 Dental and medical instruments comprising titanium
US14/167,311 Active US8876991B2 (en) 2004-06-08 2014-01-29 Dental and medical instruments comprising titanium
US14/522,013 Active US9314316B2 (en) 2004-06-08 2014-10-23 Dental and medical instruments comprising titanium
US14/722,840 Active US9732410B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US14/722,309 Active US10023948B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US14/722,390 Active US10023949B2 (en) 2004-06-08 2015-05-27 Dental and medical instruments comprising titanium
US15/671,349 Active US10047428B2 (en) 2004-06-08 2017-08-08 Dental and medical instruments comprising titanium
US16/021,917 Pending US20180305803A1 (en) 2004-06-08 2018-06-28 Dental and Medical Instruments Comprising Titanium
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2015-09-15 PGR Aia trial proceeding filed before the patent and appeal board: post-grant review
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Free format text: POST-GRANT REVIEW CERTIFICATE; TRIAL NO. PGR2015-00019, AUG. 3, 2015POST-GRANT REVIEW CERTIFICATE FOR PATENT 8,876,991, ISSUED NOV. 4, 2014, APPL. NO. 14/167,311, JAN. 29, 2014POST-GRANT REVIEW CERTIFICATE ISSUED FEB. 22, 2018