Basic ResearchTechnology

Metallurgical Characterization of M-Wire Nickel-Titanium Shape Memory Alloy Used for Endodontic Rotary Instruments during Low-cycle Fatigue
Jia Ye, PhD,* and Yong Gao, PhD
Abstract
Introduction: Rotary instruments made of a new nickel-titanium (NiTi) alloy (M-Wire) have shown improved cyclic fatigue resistance and mechanical properties compared with those made of conventional superelastic NiTi wires. The objective of this study was to characterize microstructural changes of M-Wire throughout the cyclic fatigue process under controlled strain amplitude. Methods: The average fatigue life was calculated from 30 M-Wire samples that were subjected to a strain-controlled ($4%) rotating bend fatigue test at room temperature and rotational speed of 300 rpm. Microstructural evolution of M-Wire has been investigated by different metallurgical characterization techniques, including differential scanning calorimetry, Vickers microhardness, and transmission electron microscopy at 4 different stages (as-received state, 30%, 60%, and 90% of average fatigue life). Results: During rotating bend fatigue test, no statistically signicant difference (P > .05) was found on austenite nish temperatures between as-received M-Wire and fatigued samples. However, signicant differences (P < .05) were observed on Vickers microhardness for samples with 60% and 90% fatigue life compared with as-received and 30% fatigue life. Coincidentally, substantial growth of martensite grains and martensite twins was observed in microstructure under transmission electron microscopy after 60% fatigue life. Conclusions: The results of the present study suggested that endodontic instruments manufactured with M-Wire are expected to have higher strength and wear resistance than similar instruments made of conventional superelastic NiTi wires because of its unique nano-crystalline martensitic microstructure. (J Endod 2012;38:105107)

Key Words
Cyclic fatigue, differential scanning calorimetry (DSC), microstructure, M-Wire, nickel-titanium, rotary instrument, transmission electron microscopy (TEM), Vickers microhardness

ickel-titanium (NiTi) alloys have become the most popular shape memory alloys that have a wide range of biomedical applications owing to their unique ability to recover their original shape after undergoing large deformations (up to 8%) through heating, known as shape memory effect, or through removal of the load, known as superelastic effect. Endodontic instruments made of NiTi alloys have been widely selected by endodontists for removing dead or infected tissue and shaping canals to facilitate obturation because they have much greater exibility owing to their low elastic modulus and superelasticity compared with traditional les made of stainless steel (1). Even though there has been considerable improvement in le design, manufacturing methods, and preparation techniques on endodontic rotary instruments made of NiTi alloys, rotary instrument intracanal separation caused by cyclic fatigue has remained a primary concern in the practice of endodontics, especially for root canals with severe curvatures. The mechanical performance of NiTi alloys is extremely sensitive to their microstructures and associated thermomechanical treatment history. Therefore, one of many promising solutions to improve fatigue resistance of rotary instruments is to optimize the microstructure of NiTi alloys through novel thermomechanical processing or new manufacturing technologies. Recently, a new NiTi wire (termed M-Wire) has been developed through a proprietary thermomechanical processing procedure and showed signicantly improved cyclic fatigue resistance on endodontic rotary instrument products (GT series X and ProFile Vortex [Dentsply Tulsa Dental, Tulsa, OK]) in comparison with those made of conventional superelastic NiTi alloys (26). According to the latest study on the metallurgical characterization of M-Wire by Alapati et al (7), M-Wire contains all 3 crystalline phases, including deformed and microtwinned martensite, R-phase, and austenite. To better understand the mechanism of low-cycle fatigue failure of NiTi alloys used in endodontic instruments as well as explore a potential solution for prevention or early detection of fatigue failure of rotary instruments, microstructural evolutions during cyclic fatigue process under maximum strain level (4%) were examined on M-Wire at 4 different stages (as-received state, 30%, 60%, and 90% of average fatigue life) by different metallurgical characterization techniques, including differential scanning calorimetry (DSC), Vickers microhardness, and transmission electron microscope (TEM).

Materials and Methods

From the *Electron Microscopy Center, University of Kentucky, Lexington, Kentucky; and Dentsply Tulsa Dental Specialties, Tulsa, Oklahoma. This work was nancially supported by Dentsply Tulsa Dental Specialties. Address requests for reprints to Dr Yong Gao, Dentsply Tulsa Dental Specialties, 5100 East Skelly Drive, Tulsa, OK 74135. E-mail address: yong.gao@dentsply.com 0099-2399/$ - see front matter Copyright 2012 American Association of Endodontists. doi:10.1016/j.joen.2011.09.028

M-Wire instead of endodontic instruments made of M-Wire was selected in rotating bend fatigue test for the following 2 reasons: (1) for NiTi rotary instrument, the strain/stress level at the maximum exure is difcult to calculate because of complicated le design (size/taper, cross-section geometry, helical angle, etc); (2) ISO standardized test methods and devices for cyclic fatigue resistance of NiTi rotary instruments are not available. The average fatigue life was determined from 30 M-Wire samples (1.0 mm in diameter) that were subjected to a strain-controlled rotating bend fatigue test at room temperature and rotational speed of 300 rpm. The radius of curvature R (distance to the long or neutral axis of wire) at the maximum exure is controlled at 12 mm. The maximum strain level on the outer

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boundary at the maximum exure in the rotating bend fatigue test was estimated on the basis of the formula below: E d=2R d 1:0 mm=2 12:0 mm 1:0 mm 4% where 3 is strain level, R is radius of curvature in bending, and d is diameter of M-Wire. The average cyclic fatigue life of M-Wire was 1517 cycles (standard deviation, 134 cycles). Accordingly, M-Wire samples with 30%, 60%, and 90% of average fatigue life were prepared by manually interrupting the fatigue test at predetermined times. M-Wire samples with different percentages of fatigue life were cut at the maximum exure by using low-speed saw for further DSC, Vickers microhardness, and TEM characterization. DSC tests were performed (Jade DSC; Perkin Elmer, Shelton, CT) in general accordance with the American Society for Testing and Materials standard F 2004-05 on M-Wire segments with length between 3 and 4 mm. Five M-Wire samples from each of 4 different stages (as-received, 30%, 60%, and 90% fatigue life) were tested. Each sample was cooled from room temperature to 65 C, heated to 100 C, and cooled back to 65 C with a constant heating/cooling rate of 10 C/min and nitrogen purge gas. For better comparability the results in this article focused not on all phase transformation temperatures but only on the austenite nish temperature (Af). In Vickers microhardness test, 10 M-Wire samples were randomly selected at each of 4 different stages (as-received, 30%, 60%, and 90% fatigue life). All M-Wire segments were mounted and polished by using standard metallographic techniques. Vickers microhardness measurements were performed at half radius on the cross section with maximum exure (strain level $ 2%) by using Wilson Instruments 401 MVD Vickers Microindentation tester (Instron, Norwood, MA; 500-g load and 15-second dwell time). Microstructure evolutions of M-Wire at different fatigue life stages were characterized by using a JEOL (Tokyo, Japan) 2010F TEM. TEM observation was focused at half radius on the cross section with maximum exure. A section of the wire was mechanically polished to 20 mm thick and then ion-milled to electron transparency. The testing data for DSC and Vickers microhardness were analyzed statistically by using 1-way analysis of variance, and the comparison of means was conducted by using Tukey multiple comparison test. The statistical testing was performed at the 95% level of condence (P < .05). The detailed microstructural evolutions characterized by TEM at 4 different stages during low-cycle fatigue of M-Wire are shown in Figure 1. Figure 1A shows that the as-received sample has a mixture of austenite and martensite phases. The existence of martensite has been conrmed by selected area electron diffraction pattern shown in inset of Figure 1A. The austenite phase forms the matrix, whereas the 100-nm martensite grains are evenly distributed inside it. At 30% fatigue life the microstructure of the sample has not changed much, as shown in Figure 1B. At 60% fatigue life there is substantial growth of the martensite grains and martensite twins, shown in Figure 1C. However, the work hardening was not uniform. When at 90% fatigue life, severe deformation has caused high dislocation densities within the martensite phase (Fig. 1D).

Discussion
Fracture of rotary NiTi instruments because of cyclic fatigue usually occurs near the apical third of a root canal with the highest curvature without any warning. The microstructure of NiTi raw materials used in endodontic instruments plays a crucial role on their mechanical behavior and root canal outcome, especially regarding strength and fatigue resistance. The present study examined metallurgical microstructures, phase transition temperatures, and microhardness of M-Wire at 4 different stages (as-received state, 30%, 60%, and 90% of average fatigue life). On the basis of the study on high-amplitude cyclic straining by Bahia et al (8), only a moderate change in the physical and mechanical properties has been found on the initial deformation cycles of superelastic NiTi wires and endodontic instruments, indicating rapid nucleation and slow propagation of fatigue cracks in superelastic NiTi alloys. Brantley et al (9) found there was no evident effect of 3 periods of simulated clinical use on the transformation temperatures from martensite to austenite of the tip segments of the ProFile and Lightspeed instruments during the heating cycle of DSC tests. Similarly, no signicant difference of Af temperatures (all Af $50.8 C 0.5 C) was observed for M-Wire samples at 4 different stages from as-received to 90% fatigue life. However, the microhardness of M-Wire started to increase after 60% fatigue life. The average microhardness of M-Wire (385 VHN) tested in this study was generally higher than the Vickers hardness values of NiTi rotary instruments reported by Zinelis et al (10) (range, 312376 VHN). The mechanical strength of metals and alloys usually increases when the grain size of the material is reduced (11, 12). The same trend holds true with NiTi alloys (13). We believe the 100-nm martensite grains observed in the M-Wires contributed to their improved mechanical properties, especially on torque strength and wear resistance. A reliable and cost-effective nondestructive method to assess the structural status of used endodontic instruments is needed to prevent unexpected fracture during root canal procedures. Coercivity measurement was suggested as a useful quantitative and nondestructive method for characterizing work hardening of austenitic stainless steel in relation to the amount of its plastic deformation (dislocation density because of work hardening) (14). Repeated rotational loading

Results
The mean and standard deviation of Af temperature and Vickers microhardness number (VHN) on M-Wire at 4 different stages (asreceived, 30%, 60%, and 90% fatigue life) are shown in Table 1. There was no statistically signicant difference (P > .05) on Af temperatures between as-received M-Wire and samples cycled at 30%, 60%, and 90% fatigue life. For VHN, there was no signicant difference between as-received and 30% fatigue life. However, microhardness increased as the lowcycle fatigue test progressed after 60% fatigue life, and signicant differences (P < .05) were observed for samples with 60% and 90% fatigue life compared with as-received and 30% fatigue life.

TABLE 1. Statistical Analysis (mean standard deviation, n = 5 for DSC and n = 10 for Vickers microhardness) of Af and VHN on M-Wire at 4 Different Stages (as-received, 30%, 60%, and 90% fatigue life) Fatigue life % As-received
Af ( C) VHN


30%
51.16 1.23 382.4 5.7b
a

60%
50.59 0.53 390.6 5.5c
a

90%
50.66 0.83a 392.4 7.7c

50.38 0.82 384.6 6.5b

Values with different superscript letters were signicantly different (P < .05).

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Figure 1. TEM microstructure characterization on M-Wire at 4 different stages (as-received, 30%, 60%, and 90% fatigue life). (A) Microstructure of as-received M-Wire sample, showing 100-nm martensite grains are embedded in austenite matrix. The existence of martensite has been conrmed by selected area electron diffraction pattern shown on the upper right corner. (B) Microstructure of M-Wire sample with 30% fatigue life showing nano-crystalline martensite grains are evenly distributed inside austenite matrix. (C) Microstructure of M-Wire sample with 60% fatigue life, showing substantial growth of martensite grains and martensite twins. (D) Microstructure of M-Wire sample with 90% fatigue life showing high dislocation densities within the martensite phase.

resulted in a signicant decrease in natural frequency when the tested ProFile instruments reached 77%85% of their total life limit (15). As a new NiTi wire used for rotary les, M-Wire showed substantial growth of the martensite grains and martensite twins in the microstructure after 60% fatigue life. The effect of work hardening became pronounced afterward, as shown by the increasing dislocation densities, which is consistent with the increase in Vickers microhardness after 60% fatigue life during rotating bend fatigue test. Understanding the microstructural evolution under cyclic loading will enable us to acquire and use nondestructive techniques to improve the safety and reliability of M-Wire NiTi instruments.

Conclusion
The results of the present study suggested that endodontic instruments manufactured with M-Wire are expected to have higher strength and wear resistance than similar instruments made of conventional superelastic NiTi wires because of its unique nano-crystalline martensitic microstructure.

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3. Larsen CM, Watanabe I, Glickman G, et al. Cyclic fatigue analysis of a new generation of nickel titanium rotary instruments. J Endod 2009;35:4013. 4. Al-Hadlaq SMS, AlJarbou FA, AlThumairy RI. Evaluation of cyclic exural fatigue of M-Wire nickel-titanium rotary instruments. J Endod 2010;36:3057. 5. da Cunha Peixoto IF, Pereira  ESJ, da Silva JG, et al. Flexural fatigue and torsional resistance of ProFile GT and ProFile GT series X instruments. J Endod 2010;36: 7414. 6. Gao Y, Shotton V, Wilkinson K, et al. Effects of raw material and rotational speed on the cyclic fatigue of ProFile Vortex rotary instruments. J Endod 2010;36:12059. 7. Alapati SB, Brantley WA, Iijima M, et al. Metallurgical characterization of a new nickel-titanium wire for rotary endodontic instruments. J Endod 2009;35:158993. 8. Bahia MG, Dias RF, Buono VTL. The inuence of high amplitude cyclic straining on the behaviour of superelastic NiTi. Inter J Fat 2006;28:108791. 9. Brantley WA, Svec TA, Iijima M, et al. Differential scanning calorimetric studies of nickel-titanium rotary endodontic instruments after simulated clinical use. J Endod 2002;28:7748. 10. Zinelis S, Eliades T, Eliades G. A metallurgical characterization of ten endodontic NiTi instruments: assessing the clinical relevance of shape memory and superelastic properties of Ni-Ti endodontic instruments. Int Endod J 2010;43:12534. 11. Hall EO. The deformation and ageing of mild steel: IIIdiscussion of results. Proc Phys Soc 1951;64:74751. 12. Petch NJ. The cleavage strength of polystrals. J Iron Steel Inst 1953;174:258. 13. Ye J, Mishra RK, Pelton AR, et al. Direct observation of the NiTi martensitic phase transformation in nanoscale volumes. Acta Mater 2010;58:4908. 14. Sullivan DO, Cotterell M, Meszaros I. The characterisation of work-hardened austenitic stainless steel by NDT micro-magnetic techniques. NDT & E International 2004; 37:2659. 15. Hsieh SC, Lee SY, Ciou CY, et al. Non-destructive natural frequency tests of cyclic fatigue-loaded nickel-titanium rotary instruments. Med Biol Eng Comput 2010; 48:55560.

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