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One of the most important challenges in endodontics is to have files that have excellent flexibility, toughness, and high fatigue life. Superelastic NiTi alloys have been a breakthrough and the new R-phase NiTi alloys promise to further optimize the good properties of NiTi alloys. In this work, two austenitic phase endodontic files with superelastic properties (Protaper and F6) and two austenitic phase files with the R-phase (M-wire and Reciproc) have been studied. The transformation temperatures were studied by calorimetry. Molds reproducing root canals at different angles (30, 45, and 70°) were obtained with cooling and loads simulating those used in the clinic. Mechanical cycles of different files were realized to fracture. Transformation temperatures were determined at different number of cycles. The different files were heat treated at 300 and 500 °C as the aging process, and the transformation temperatures were also determined. Scanning and transmission electron microscopy was used to observe the fractography and precipitates of the files. The results show that files with the R-phase have higher fracture cycles than files with only the austenitic phase. The fracture cycles depend on the angle of insertion in the root canal, with the angle of 70° being the one with the lowest fracture cycles in all cases. The R-Phase transformation increases the energy absorbed by the NiTi to produce the austenitic to R-phase and to produce the martensitic transformation causing the increase in the fracture cycles. Mechanical cycling leads to significant increases in the transformation temperatures Ms and Af as well as Rs and Rf. No changes in the transformation temperatures were observed for aging at 300 °C, but the appearance of Ni4Ti3 precipitates was observed in the aging treatments to the Nickel-rich files that correspond to those with the R transition. These results should be considered by endodontists to optimize the type of files for clinical therapy.

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The production and application of materials are evolving towards the low-dimensional micro-nano scale. Nevertheless, the fabrication of micron-scale alloy fibers remains a challenge. Herein, a novel Ni-Co-Cr-Fe-Mo high-entropy alloy (HEA) fiber with a cold-drawn reduction rate of 99.9995% and a strain (ɛ) of 12.19 is presented without requiring intermediate annealing. The exceptional deformation strain of 11.62 within the fiber leads to extraordinary tensile strengths of 2.8 GPa at room temperature and 3.6 GPa at 123 K. The in-depth investigation of the microstructure of fibers has revealed the cold drawing deformation mechanisms mediated by the synergistic effects of plane defects. Specifically, various geometrically necessary dislocation interfaces, such as dislocation walls and microbands, along with deformation twins and long-period 9R structures, form in response to external stress when ɛ≤2.7. As the strain increases, the saturated layered structure emerges and progressively evolves into a 3D equiaxed crystal. Moreover, the formation and evolution of the 9R structure (i.e., the migration of incoherent twin boundaries), coupled with the interaction of partial dislocations and the role of deformation twins, are crucial factors determining the fiber's plastic response. This work provides a novel approach to discovering new high-strength metallic fibers with excellent deformability through plane defects engineering.

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Inversion symmetry broken 3R phase transition metal dichalcogenides (TMDs) show fascinating prospects in spintronics, valleytronics, and nonlinear optics. However, the controlled synthesis of 3R phase TMDs is still a great challenge. In this work, two-dimensional 3R-NbSe2 single crystals up to 0.2 mm were synthesized for the first time through chemical vapor deposition method by designing a space-confined system. The crystal size and morphology can be controlled by the location of the stacked substrates and the amount of the Nb2O5 precursor. Scanning transmission electron microscopy and Raman measurements reveal the NbSe2 exhibits a pure 3R stacking mode with relatively weak interlayer van der Waals interactions. Importantly, 3R-NbSe2 shows obvious second harmonic generation signal which intensity intensified as thickness increases. Density functional theory calculations and optical absorption demonstrate the coexistence of metallic and semiconducting optical properties of 3R-NbSe2. We designed a NbSe2/WS2/NbSe2 photodetector utilizing the metallicity of 3R-NbSe2, which shows good performance especially an ultrafast response (6-7 µs, 0.5 ms - 7.9 s for Au electrodes in literature). The proposed strategy and findings are of great significance for the growth of many other 3R-TMDs and applications of nonlinear optical and ultrafast devices.

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Synthesizing a material with the desired polymorphic phase in a chemical vapor deposition (CVD) process requires a delicate balance among various thermodynamic variables. Here, we present a methodology to synthesize rhombohedral (3R)-phase MoS2 in a well-defined sword-like geometry having lengths up to 120 µm, uniform width of 2-3 µm and thickness of 3-7 nm by controlling the carrier gas flow dynamics from continuous mode to pulsed mode during the CVD growth process. Characteristic signatures such as high degree of circular dichroism (∼58% at 100 K), distinct evolution of low-frequency Raman peaks and increasing intensity of second harmonic signals with increasing number of layers conclusively establish the 3R-phase of the material. A high value (∼844 pm/V) of second-order susceptibility for few-layer-thick MoS2 swords signifies the potential of MoS2 to serve as an atomically thin nonlinear medium. A field effect mobility of 40 cm2/V-s and Ion/Ioff ratio of ∼106 further confirm the electronic-grade standard of this 3R-phase MoS2. These findings are significant for the development of emerging quantum electronic devices utilizing valley-based physics and nonlinear optical phenomena in layered materials.

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This study aimed to evaluate and compare the effects of ambient temperature and post-manufacture heat-treatment on the mechanical behavior of nickel-titanium (NiTi) wires. Four types of commercial NiTi variants (Stock NiTi, heat treated "Blue", "Gold", "Superflex", all Dentsply Maillefer, Ballaigues, Switzerland) were stressed in a tensile testing machine in a temperature-controlled water bath at three different temperatures. Stress and strain values were extrapolated from the raw data, and 2-way ANOVA and Tukey's test for multiple comparisons were performed to compare the differences of the mechanical constants. Differential scanning calorimetry (DSC) tests established the martensitic transformation starting (Ms), finishing (Mf) and austenitic (reverse-martensitic) starting (As) and finishing (Af) points. Austenitic modulus of elasticity and transformation stress values increased with temperature for all NiTi groups. The martensitic modulus of elasticity, maximum transformation strain and ultimate tensile stress were not significantly affected by temperature changes. Stock NiTi and Gold wire samples presented with clearly delineated austenitic and martensitic transformations in the DSC experiments. Differences in manufacturing/heat treatment conditions and ambient temperature affect the mechanical behavior of nickel-titanium and may have clinical implications. Further improvements to the experimental setup could be considered to provide more accurate measurements of strain.

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An inter-metallic phase in the Al-Mn-Ni system crystallizing in space group Cmcm (No. 63) and refined formula Al61.49Mn11.35Ni4 (called the R' phase) has been synthesized by high-temperature sinter-ing of a mixture with initial chemical composition Al60Mn7Ni3. In comparison with the structure model of the previously reported R phase with composition Al60Mn11Ni4 [Robinson (1954 ▸). Acta Cryst. 7, 494-497], there are two mutually exchanged Mn and Ni sites together with one positionally disordered Al site [occupancy ratio 0.811 (8):0.121 (7)] and one partially occupied Mn site [s.o.f. 0.677 (5)] in the current structure model of the R' phase.

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OBJECTIVES: This study aims to evaluate the effects of cyclic loading on the bending moments and the developed stress state of austenitic and R-phase endodontic files through finite element analysis. MATERIALS AND METHODS: The mechanical properties of two groups of NiTi wires, austenite and R-phase, were measured in samples at two different conditions: uncycled and cycled. The cycled condition was achieved by subjecting samples of the two groups to 80% of the corresponding fatigue life under rotating bending efforts. The measured mechanical properties were then used in the finite element analysis, where the boundary and loading conditions were set to replicate a standard bending test. RESULTS: The results showed that mechanical cycling leads to decreasing stress levels and bending moments in the simulated files, especially in the austenitic ones. In comparison with austenite, R-phase presented a more stable mechanical behavior during cycling. CONCLUSIONS: The results show that the moment and stress calculated for an instrument under bending can be considerably decreased after some cyclic work. CLINICAL RELEVANCE: The fatigue related to the clinical use of an endodontic file decreases the moment (as well as the forces) imposed by the instrument during the shaping of a curved root canal. This decrease is directly related to the type of atomic array present in the alloy.

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Instrument failure during root canal preparation is still a concern among endodontists. However, it remains unclear whether the use of more martensitic alloys or the cross-sectional design parameters (i.e., core mass) significantly improve fracture resistance. The aim of the study was to evaluate the impact of core mass and alloy on dynamic cyclic fatigue resistance of nickel-titanium endodontic instruments in matching artificial canals at body temperature. Two groups were tested. (A) taper 0.04: F360 (Komet, Lemgo, Germany), Twisted file (Sybron Endo, Glendora, CA, USA) (=TF), JIZAI (Mani, Tochigi, Japan) (=J_04) (all size #25) and the variable tapered TruNatomy (Dentsply, Ballaigues, Switzerland) (size #26) (=TN). (B) size #25; taper 0.06: (Mtwo (VDW, Munich, Germany), JIZAI (Mani) (=J_06), and variable tapered Hyflex EDM OneFile (Coltene Whaledent, Altstätten, Switzerland) (=HF). Time, number of cycles to fracture (NCF), and number and length of fractured fragments were recorded and statistically analysed using ANOVA Student-Newman-Keuls, Kruskal-Wallis or Chi-square test (significance level = 0.05). (A) TN showed the significantly shortest time until fracture, followed by TF, F360 and J_04 which also differed significantly, while NCF showed the following order: F360 < TN < TF < J_04 (p < 0.05). Only one J_04 but all instruments of the other groups fractured within the test-limit of 10 min. (B) Mtwo was significantly inferior concerning time until fracture and NCF, compared to J_06 and HF (p < 0.05), which did not differ significantly (p > 0.05). While all Mtwo instruments fractured, only four instruments failed in the other groups (p < 0.05). Within the limitations of this study, alloy and cross-sectional design (i.e., core mass) were critical factors regarding instrument failure, but none of these factors could be determined as a main parameter for increased or decreased time, and cycles to fracture. Rather, it seemed to be the interaction of multiple factors (e.g., longitudinal and cross-sectional design, alloy, and rotational speed) that was responsible for differences in the time and cycles to fracture. Nonetheless, all instruments had lifetimes that allow safe clinical use. However, the superiority or inferiority of an instrument with regard to cyclic fatigue based on laboratory results-even when identical trajectories are guaranteed-may be considered questionable, as the characteristics and design parameters of the instruments vary considerably, and the experimental setups lack additional clinical parameters and thus clinical relevance.

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Thermoelastic deformation mechanisms in polycrystalline biomedical-grade superelastic NiTi are spatially mapped using in situ neutron diffraction during multiaxial loading and heating. The trigonal R-phase is formed from the cubic phase during cooling to room temperature and subsequently deforms in compression, tension, and torsion. The resulting R-phase variant microstructure from the variant reorientation and detwinning processes are equivalent for the corresponding strain in tension and compression, and the variant microstructure is reversible by isothermal loading. The R-phase variant microstructure is consistent between uniaxial and torsional loading when the principal stress directions of the stress state are considered (for the crystallographic directions observed here). The variant microstructure evolution is tracked and the similarity in general behavior between uniaxial and torsional loading, in spite of the implicit heterogeneous stress state associated with torsional loading, pointed to the ability of the reversible thermoelastic transformation in NiTi to accommodate stress and strain mismatch with deformation. This ability of the R-phase, despite its limited variants, to accommodate stress and strain and satisfy strain incompatibility in addition to the existing internal stresses has significance for reducing irrecoverable deformation mechanisms during loading and cycling through the phase transformation.

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Ever since their introduction, nickel-titanium (NiTi) alloys have continued to revolutionize the field of endodontics. They have considerable advantages over the conventional stainless steel file in terms of mechanical properties. However, despite of their superior mechanical properties, NiTi alloys still pose some risk of fracture. Consequently, there has been considerable research conducted to investigate the mechanisms behind the occurrence of these procedural errors. Since the last decade, different proprietary processing procedures have been introduced to further improve the mechanical properties of NiTi alloys. These treatments include thermal, mechanical, electropolishing, and recently introduced electric discharge machining. The main purpose of these treatments is to impart a more martensitic phase into the files at normal body temperature, so that the maximum advantage of flexibility can be obtained. These heat-treated instruments also possess improved cyclic fatigue resistance when compared to conventional NiTi alloys. NiTi alloys can be subclassified as the instruments mainly containing austenitic phase (conventional NiTi, M-wire, R-phase), and those containing martensitic phase (controlled memory wire, ProTaper Gold, and Vortex Blue). Instruments based on austenitic alloys possess superelastic properties due to the stress-induced martensitic transformation. Contrary to this, martensitic alloys can easily be deformed due to phase transformation, and they can demonstrate the shape memory effect when heated. This review discusses the different phase transformations and heat treatments that the NiTi instruments undergo.

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AIMS: The aim of this in vitro study was to compare the static cyclic fatigue resistance of thermal treated rotary files with a conventional nickel-titanium (NiTi) rotary file. SUBJECTS AND METHODS: Four groups of 60 rotary files with similar file dimensions, geometries, and motion were selected. Groups were set as HyFlex Group [controlled memory wire (CM-Wire)], ProfileVortex Group (M-Wire), Twisted File Group (R-Phase Wire), and OneShape Group (conventional NiTi wire)] and tested using a custom-made static cyclic fatigue testing apparatus. The fracture time and fragment length of the each file was also recorded. Statistical analysis was performed using one-way analysis of variance and Tukey's test at the 95% confidence level (P = 0.05). RESULTS: The HyFlex group had a significantly higher mean cyclic fatigue resistance than the other three groups (P < 0.001). The OneShape groups had the least fatigue resistance. CONCLUSIONS: CM-Wire alloy represented the best performance in cyclic fatigue resistance, and NiTi alloy in R-Phase had the second highest fatigue resistance. CM and R-Phase manufacturing technology processed to the conventional NiTi alloy enhance the cyclic fatigue resistance of files that have similar design and size. M-wire alloy did not show any superiority in cyclic fatigue resistance when compared with conventional NiTi wire.

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INTRODUCTION: The purpose of this study was to assess the effects of sodium hypochlorite (NaOCl) immersion and sterilization on the cyclic fatigue resistance of heat-treated nickel-titanium (NiTi) rotary instruments. METHODS: Two hundred ten new 25/.06 Twisted Files (TFs; SybronEndo, Orange, CA) and Hyflex CM (Coltene Whaledent, Cuyahoga Falls, OH) files were divided into 7 groups (n = 15) for each brand. Group 1 (control group) included new instruments that were not immersed in NaOCl or subjected to autoclave sterilization. Groups 2 and 3 were composed of instruments dynamically immersed for 3 minutes in 5% NaOCl solution 1 and 3 times, respectively. Groups 4 and 5 consisted of instruments only autoclaved 1 and 3 times, respectively. Groups 6 and 7 recruited instruments that received a cycle of both immersion in NaOCl and sterilization 1 and 3 times, respectively. Instruments were subsequently subjected to a fatigue test. The surface morphology of fractured instruments was studied by field-emission scanning electron microscopy and x-ray energy-dispersive spectrometric (EDS) analyses. The means and standard deviations of the number of cycles to failure (NCF) were calculated and statistically analyzed using 2-way analysis of variance (P < .05). RESULTS: Comparison among groups indicated no significant difference of NCF (P > .05) except for the groups of TFs sterilized 3 times without and with immersion in NaOCl (P < .05). HyFlex CM files exhibited higher cyclic fatigue resistance than TFs when files were sterilized 3 times, independently from immersion in NaOCl (P < .05). EDS analysis showed the presence of an oxide-rich layer on the Hyflex CM files' external surface. No morphologic or chemical differences were found between files of the same brand subjected to different treatments. CONCLUSIONS: Repeated cycles of sterilization did not influence the cyclic fatigue of NiTi files except for TFs, which showed a significant decrease of flexural resistance after 3 cycles of sterilization. Immersion in NaOCl did not reduce significantly the cyclic fatigue resistance of all heat-treated NiTi files tested.

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OBJECTIVE: The aim of this study was to compare the incidence of root cracks after root canal instrumentation with thermomechanically processed nickel-titanium (Ni-Ti) files with different instrumentation kinematics. MATERIALS AND METHODS: A total of 150 extracted mandibular premolars with mature apices and straight root canals were divided into five groups and used in this study. In Group 1, 30 teeth were prepared using hand K-files and assigned to control group, Group 2 was instrumented using K3XF Rotary files (SybronEndo, Glendora, CA, USA) with continuous rotary motion. The teeth in Group 3 were instrumented by ProTaper Next (Dentsply Maillefer, Ballaigues, Switzerland) rotary files which make asymmetric rotary motion, In Group 4, teeth were instrumented by RECIPROC (VDW, Munich, Germany) with reciprocation motion and in Group 5, teeth were instrumented by Twisted File (TF) Adaptive (SybronEndo, Orange, CA, USA) files that use combination of continuous rotation and reciprocation motion (n = 30/per group). All the roots were horizontally sectioned 3, 6, and 9 mm from the apex with a low speed saw under water cooling. Then, the slices were examined through a stereomicroscope to determine the presence of dentinal microcracks. RESULTS: For the apical (3-mm) and coronal (9-mm) sections, the ProTaper Next and TF Adaptive produced significantly more cracks than the hand files, RECIPROC, and K3XF (P < 0.05). There was no significant difference between the experimental groups and control group at the 6-mm level (P > 0.05). CONCLUSIONS: Within the limitations of this in vitro study, all thermal-treated Ni-Ti instruments and hand files caused microcracks in root canal dentin.

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BACKGROUND/PURPOSE: Heat treatment of nickel-titanium (NiTi) alloy produces a better arrangement of the crystal structure, thereby leading to increased flexibility and improved fatigue resistance or plastic behavior. This study aimed to assess the performance of various heat-treated NiTi rotary instruments in S-shaped resin canals. MATERIALS AND METHODS: Forty S-shaped resin canals were instrumented (10/group) with either Twisted Files (R-phase), WaveOne (M-wire), Hyflex CM, or V Taper 2H (CM-wire) with the same apical size and taper (25/0.08). Each S-shaped resin canal was scanned both before and after instrumentation with microcomputed tomography. Changes in canal volume and transportation were evaluated at regular intervals (0.5 mm). Differences between instruments at the apical curve, coronal curve, and straight portion of the canals were analyzed statistically. RESULTS: All tested instruments caused more transportation at the coronal rather than apical curvatures, with the exception of Twisted Files for which apical transportation was the highest for any instrument or location (P < 0.05). The transportation was mostly influenced by the alloy type rather than their cross-sectional characteristics (P < 0.05). The volumetric increase after instrumentation was similar for all tested instruments at the apical curve (P > 0.05), whereas Hyflex CM created the most conservative preparations at the coronal curve (P < 0.05). At the straight portion, volumetric changes were largest for Twisted Files and smallest for V Taper 2H (P < 0.05). CONCLUSION: Amongst heat-treated NiTi instruments, the CM-wire based instruments created the most favorable preparations in S-shaped resin canals.

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CONTEXT: Recent introduction of shape memory (SM) nickel-titanium (NiTi) alloy into endodontics is a major breakthrough. Although the flexibility of these instruments was enhanced, fracture of rotary endodontic instruments during instrumentation is an important challenge for the operator. Implementation of supplementary manufacturing methods that would improve the fatigue life of the instrument is desirable. AIM: The purpose of this study was to investigate the role of dry cryogenic treatment (CT) conditions on the microstructure of martensitic SM NiTi alloy. MATERIALS AND METHODS: Experiments were conducted on Ni-51 wt% Ti-49 wt% SM alloy. Five cylindrical specimens and five sheet specimens were subjected to different CT conditions: Deep CT (DCT) 24 group: -185°C; 24 h, DCT 6 group: -185°C; 6 h, shallow CT (SCT) 24 group: -80°C, 24 h, SCT 6 group: -80°C, 6 h and control group. Microstructure of surface was observed on cylindrical specimens with an optical microscope and scanning electron microscope at different magnifications. Subsurface structure was analyzed on sheet specimens using X-ray diffraction (XRD). RESULTS: Microstructures of all SM NiTi specimens had equiaxed grains (approximately 25 µm) with well-defined boundaries and precipitates. XRD patterns of cryogenically treated specimens revealed accentuation of austenite and martensite peaks. The volume of martensite and its crystallite size was relatively more in DCT 24 specimen. CONCLUSIONS: DCT with 24 h soaking period increases the martensite content of the SM NiTi alloy without altering the grain size.

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INTRODUCTION: The aim of this study was to evaluate the ability of the Twisted File Adaptive (TF Adaptive; SybronEndo, Orange, CA) system in maintaining the original profile of root canal anatomy. The ProTaper Universal (Dentsply Maillefer, Ballaigues, Switzerland) and Twisted File (TF) (SybronEndo) systems were used as reference techniques for comparison. METHODS: Thirty simulated curved root canals manufactured in clear resin blocks were randomly assigned to 3 groups (n = 10) according to the instrumentation system: TF in rotary motion, TF in TF Adaptive motion, and ProTaper Universal. Color stereomicroscopic images from each block were taken exactly at the same position before and after instrumentation. All image processing and data analysis were performed with an open-source program (Fiji). Evaluation of canal transportation was obtained for 2 independent canal regions: straight and curved levels. Univariate analysis of variance and Tukey Honestly Significant Difference were used, and a cutoff for significance was set at alpha = 5%. RESULTS: Instrumentation systems significantly influenced canal transportation (P = .000). A significant interaction between instrumentation system and root canal level (P = .000) was also found as follows: at the straight part, TF and TF Adaptive systems produced similar canal transportation, which was significantly lower than for the ProTaper Universal system; at the curved part, TF resulted in the lowest canal transportation followed by TF Adaptive and ProTaper Universal systems. Canal transportation was higher at the curved canal parts (P = .00). CONCLUSIONS: The TF in rotary motion produced overall less canal transportation in the curved portion when compared with the others tested systems. The ProTaper Universal system showed the highest canal transportation.

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INTRODUCTION: The aim of the study was to compare the K3 and K3XF systems (SybronEndo, Glendora, CA) after 1 and 2 uses by evaluating apical transportation, working length loss, and working time in a manikin model. METHODS: Mesial canals of 40 extracted first mandibular molars were instrumented. Radiographs taken after instrumentation with #25, #30, #35, and #40 files were superimposed on the preoperative image in both mesiodistal and buccolingual angulations. AutoCAD (Autodesk Inc, San Rafael, CA) was used to measure working length loss and apical transportation at 0, 0.5, and 1 mm from the working length (WL). The working time was measured. Group comparison was analyzed using post hoc Tukey honestly significant difference tests (P < .05). RESULTS: No significant differences were found in apical transportation, working length loss between K3 and K3XF systems, or between the number of uses. Significant differences were found when canal enlargement was performed to a #35-40 (P < .05). K3 instrumentation performed significantly faster (29.6 ± 15.4) than with the K3XF system (40.2 ± 17.7) (P < .05). No differences were observed in working time when comparing the number of uses. CONCLUSIONS: K3 and R-phase K3XF rotary systems shaped curved root canals safely with minimal apical transportation, even up to a 40/04 file.

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INTRODUCTION: New designs and alloys and different motions have been introduced to increase the cyclic fatigue (CF) resistance of nickel-titanium (NiTi) files. The aim of this study was to compare the CF resistance of K3 (SybronEndo, Orange, CA), K3XF (SybronEndo), and TF (SybronEndo) files under continuous rotation and reciprocating motion. METHODS: A total of 210 files (30-tip diameter, 0.06 fixed taper), 60 K3, 60 K3XF, and 90 TF files, were divided into 7 groups (30 files each): K3-C, K3XF-C, and TF1-C were rotated at 300 rpm; TF2-C was rotated at 500 rpm; and K3-R, K3XF-R, and TF1-R were used in a reciprocating motion. CF resistance was tested in stainless steel, curved canals (60°, r = 3 mm) until fracture, and the time to fracture was recorded. The mean half-life, beta, and eta were calculated for each group and were compared with Weibull analysis. RESULTS: The probability of a longer mean life was greater under reciprocating motion for all of the files (100% for K3, 87% for K3XF, and 99% for TF). Under continuous rotation, K3XF was more resistant than K3 and TF. TF lasted significantly longer than K3. TF was more resistant to CF when rotated at 300 rpm instead of 500 rpm. Under reciprocating motion, there were no significant differences between K3XF and TF mean lives, but both were significantly longer than the K3 mean life (78% for TF and 86% for K3XF). CONCLUSIONS: Reciprocating motion and R-phase increase CF resistance.

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