Nanostructured titanium-nickel alloy with shape memory effect and method of making bar thereof

FIELD: metallurgy.

SUBSTANCE: proposed alloy features structure of nanocrystalline grains of B2-phase wherein volume fraction of 0.1 mcm-size grains and those of shape factor of 2 in mutually perpendicular planes makes at least 90%. Over 50% of grains have large angular boundaries misaligned relative to adjacent grains through 15 to 90 degrees. Method of making the bar from said alloy comprises thermomechanical processing including plastic straining and recovery annealing. Intensive plastic straining is made in two steps. At first step, equal-channel angular pressing is made to accumulated strain e≥4. At second step, forge ironing and/or drawing are made. Annealing is carried out either in process and/or after every straining step. Equal-channel angular pressing is performed at 400°C. Forge drawing and ironing are made to total reduction of over 60% at gradual decrease of temperature to t=450-200°C, while annealing is performed at t=400-200°C.

EFFECT: higher mechanical and functional properties.

2 cl, 2 dwg, 1 ex

 

The invention relates to deformation-thermal molding processing of alloys with shape memory effect (APF), in particular alloys based on the intermetallic compound TiNi, with the goal of significantly improving their mechanical and functional properties, and can be used in metallurgy, mechanical engineering and medicine. Especially attractive is its use in medical devices for traumatology, orthopedics, dentistry, minimally invasive surgery and other surgical devices such as implants and instruments.

A known method of manufacturing a hyperelastic alloy Nickel-titanium (JP 6065741, IPC C22F 1/10, publ. 24.08.94 year), according to which the alloy containing at 50-51.% Nickel, the rest is titanium, are annealed, cold-formed with the degree of deformation of 15-60%, and then fixed with some form of alloy and heat it up 175-600°C.

The disadvantage of this method is the use of only one mechanism for improving the properties of complex alloys - creating Polynesians dislocation substructure, which limits the possibility of simultaneous improvement of their mechanical (strength and plastic) characteristics and functional properties, such as maximum reversible strain and maximum reactive voltage.

A method of obtaining hyperelastic titanium-nick is left alloy (JP 58161753, IPC C22F 1/10, publ. 26.09.83 g), including pre-hardened coarse-grained alloy, subsequent cold deformation by rolling with a degree of deformation of ≥20% and annealing at a temperature of 250-550°C.

The disadvantages of the method are relatively low degree of deformation (e<1), and restrictions on the degree of crushing of the microstructure, which does not allow to achieve the highest mechanical and functional properties.

The closest to the invention is a method for ultrafine-grained splavov "titanium-Nickel shape memory effect, including thermomechanical processing, combining deformation and deregistrations annealing. Before thermomechanical processing carry out a preliminary hardening of the alloy, and the deformation is carried out in two stages, and the first step is conducted intensive plastic deformation accumulated true strain degree f>4 in the temperature range of 300-550°C., and the second stage are deformation by rolling or extrusion, or drawing with the degree of deformation of at least 20% at temperatures between 20 and 500°C, and annealing is carried out at temperatures of 350-550°C for 0.5 to 2.0 hours. (Patent RF №2266973 IPC C22F 1/18, publ. 27.12.2005,)

The disadvantage of this method is the high degree of anisotropy of the structure and properties of the material due to the heterogeneous morphology of the grains in the longitudinal and in erachem section of the workpiece, a large proportion of low-angle boundaries. This material has a high strength but limited plasticity that do not provide high resistance to fatigue failure.

The task of the invention is to improve the mechanical characteristics of the alloys, titanium-Nickel with shape memory effect with simultaneous improvement of functional properties by creating a nanocrystalline structure.

The problem is solved nanostructured alloy titanium Nickel with shape memory effect, characterized by the structure of nanokristallicheskikh austenitic grains B2 phase in which the volume fraction of grains with a size not more than 0.1 μm and aspect ratio of the grains is not more than 2 in mutually perpendicular planes is not less than 90%, and more than 50% of the grains have a large-angle boundaries misoriented relative to neighboring grains on the angles from 15° to 90°.

The problem is solved by a method of producing rod of an alloy of titanium-Nickel nanocrystalline structure, including thermomechanical processing, combining the intense plastic deformation and deregistrations annealing, and the intensive plastic deformation is carried out in two stages, the first stage Ravnica national angular pressing with the achievement of the accumulated strain is e≥4, and at the second stage of implementation is Aut deformation forging hood and/or drawing, as the annealing carried out during and/or after each stage of deformation, which unlike the prototype of equal channel angular pressing is carried out at a temperature not exceeding 400°C, forging the hood and drawing is carried out with the total accumulated strain E. more than 60% with a gradual decrease in the temperature interval t=450-200°C, and annealing is performed at a temperature equal to t=400-200°C.

The proposed invention allows to obtain a higher level of mechanical and fatigue properties in combination with good functional properties such as shape memory effect.

Increasing the strength of the material due to the very small grain size (not more than 0.1 μm) in the structure that provides increased voltage currents during plastic deformation according to a known ratio Hollo-Petch (Large plastic deformation and fracture of metals. Rybin V.V. M.: metallurgy, 1986, 224). A significant increase in strength is achieved also by a large number of grains with belleplaine boundaries (not less than 50%), which in comparison with low-angle and special borders make the greatest contribution to hardening (R.Z. Valiev, I.V. Alexandrov. Bulk nanostructured metallic materials. - M.: ICC called "Akademkniga", 2007. - 398 C.). In this case the formation of grains with an aspect ratio of not more than 2 (the ratio of the width and length of the grain in 1:2) reduces the ambiguity of godnosti plastic flow of the metal, the level of microstresses, thus preventing early localization of deformation, leading to fracture of the material.

The method is as follows.

Preparation of splavov titanium-Nickel in the form of a cylindrical rod is subjected to severe plastic deformation equal channel angular pressing (pressing) at a temperature not higher than 400°C in multiple passes number of passes is determined based on the achievement of the true accumulated strain is e≥4. While the workpiece after each passage rotate around its longitudinal axis in a clockwise direction at a 90° angle to the uniformity of structure processing. To improve the technological plasticity and the formation of a microstructure predominantly grain type carry out intermediate annealing between aisles or final annealing after the final passage at a temperature of 400-200°C.

The higher the accumulated degree of deformation of the pressing, the lower temperature annealing. Annealing at temperatures above 400°C reduces the effect of hardening from pressing.

At this stage, the main crushing of the microstructure in the volume of the workpiece without changing its size. In the initial stages of plastic deformation (e=1 after the first iteration pressing) original grains are fragmented due to the formation of low-angle dislocation boundaries. With increasing true the second accumulated strain to e=4 (after 4 passages pressing) in the structure is fragmented grains and the formation of cellular structure. At the same time dislocation walls of the cells become more narrow and streamlined, increasing the angle of misorientation, which contributes to the transformation of the cellular structure in the grain structure. In the evolution of structure in the process of pressing the material is formed Sereno/subgrain structure, characterized by strongly non-equilibrium boundaries and high density of grain boundary and lattice dislocations with grain size in the range of 0.1-0.5 micron.

At the next stage, the plastic deformation of the workpiece forging hood and/or drawing. The treatment is carried out with the total accumulated strain over 60% with a gradual decrease in the temperature interval t=450-200°C. the Degree of deformation less than 60% does not lead to a significant change in the structure. Intermediate anneals at various stages of deformation in the temperature range 400-200°C serve to increase the deformability of solid billet, and the choice of annealing temperature depends on the prior accumulated deformation. In the final stages of deformation to form a homogeneous nanocrystalline structure throughout the cross section of the rod with a grain size of 0.09-0.1 ám use intermediate low-temperature annealing at a temperature not higher than 200°C. Intermediate anneals at temperatures over 200°C lead to the intensification of the processes of return and not p is help form a nanocrystalline structure.

The combination of plastic deformation and intermediate anneals further evolution obtained after pressing structure: the formation of new subgrain boundaries, their transformation in the grain structure, thereby increasing the share of large angle boundaries, the formation of new nanocrystalline grains, the decrease in the density of lattice dislocations due to the simultaneously occurring processes of return and dynamic recrystallization.

An example of a specific implementation of the invention.

As the blanks used a cylindrical rod (100×20 mm) alloy Ti49.4Ni50.6. At the first stage of processing conducted pressing the workpiece at a temperature of 400°C, the number of passes n=8. While the workpiece after each pass, turned around its longitudinal axis in a clockwise direction at a 90° angle to ensure uniform development patterns. Between passes was carried out by annealing at 400°C. In total, the cumulative degree of deformation was e=6,4. The result was the resulting solid billet length 80 mm, diameter 18 mm

After pressing the workpiece was subjected to TMO, which was carried out by plastic deformation in several stages forge hood and drawing with a gradual decrease in the temperature interval t=450-200°C. the Total accumulated strain ε after forging and drawing and drawing with the put 90%

In the processing result received a rod with a diameter of 5.9 mm length 800 mm

From the obtained rod samples were made to study the microstructure of the method of transmission electron microscopy (TEM), which was carried out on microscope JEM-2100 b. Samples for testing were cut electroerosion method in the form of plates in transverse and longitudinal cross sections of the rod. For the preparation of thin foils wafers were subjected to mechanical thinning to a thickness of 150 μm and the subsequent electrolytic polishing on the installation Tenupol-5 (Struers) at room temperature in an electrolyte consisting of perchloric acid (HClO4) and butanol (C4H9OH).

Studies of microstructure method TEM show that the result of the processing of the proposed method in the alloy, titanium-Nickel is a significant refinement of the structure and is formed of nanocrystalline structure in which up to 90% grain B2 phase with an average size of 0.09-0.1 ám in bright and dark field and aspect ratio of the grains is not more than 2 in mutually perpendicular planes. Measurement error was not more than 5%.

The microstructure of the alloy after pressing, forging and drawing and drawing illustrated with photographs: figure 1 - microstructure in the longitudinal (a) and transverse (b) sections with magnification of 20,000 times, figure 2 - poper is cnom section with increasing 75,000 times. According to structural studies share blueeagle borders amounted to not less than 50%, allowing you to greatly improve the mechanical properties. Studies have shown that the proposed method thermomechanical processing of titanium alloy, Nickel, a combination of pressing and subsequent forging the hood and drawing (ε=90%) with annealing processing at specified temperature and time parameters allowed us to obtain the following characteristics: tensile strength up to 1460 MPa with ductility 35%, the maximum reactive voltage - 1000 MPa, the maximum reversible strain - 9%. The achieved results on the mechanical and functional properties are higher than those provided by the prototype.

Thus, the proposed invention allows to form in the alloy, titanium-Nickel with shape memory effect of nanocrystalline structure of the B2 phase, providing material increased strength, flexibility and improved performance.

1. Nanostructured alloy titanium Nickel with shape memory effect, characterized by the structure of nanokristallicheskikh austenitic grains B2 phase in which the volume fraction of grains with size less than 0.1 μm and aspect ratio of the grains is not more than 2 in mutually perpendicular planes is not less than 90%, and more than 50% C is Ren have large-angle boundaries, misoriented relative to neighboring grains on the angles from 15° to 90°.

2. A method of producing rod of nanostructured alloy titanium Nickel with shape memory effect according to claim 1, including thermomechanical processing workpieces of alloy titanium Nickel, combining the intense plastic deformation and deregistrations annealing, and the intensive plastic deformation is carried out in two stages, the first stage is realized by equal channel angular pressing with the achievement of the accumulated strain is e≥4, and in the second stage, the deformation of the forging hood and/or drawing, and annealing is carried out in the process and/or after each stage of deformation, with equal-channel angular pressing is carried out at a temperature not exceeding 400°C, blacksmith the hood and the drawing is carried out with the total accumulated strain ε of more than 60% with a gradual decrease in the temperature interval t=450-200°C, and annealing is performed at a temperature equal to t=400-200°C.



 

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