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    • 专利摘要:
    abstract nanostructured titanium alloy article, and, method for making a nanostructured titanium alloy a nanostructured titanium alloy article is provided. the nanostructured alloy includes a developed titanium structure having at least 80% grains with a grain size = 1.0 microns. 1/1
    公开号:BR112015023754B1
    申请号:R112015023754-1
    申请日:2014-03-14
    公开日:2020-03-17
    发明作者:Gian Colombo；Venkata N. Anumalasetty；Graham McIntosh；Yuliya Mardakhayeva
    申请人:Manhattan Scientifics Inc.；
    IPC主号:
    专利说明:

    NANO-STRUCTURED TITANIUM ALLOY ARTICLE, AND METHOD FOR MANUFACTURING A NANO-STRUCTURED TITANIUM ALLOY
    FIELD OF THE INVENTION
    [001] The invention concerns a nanostructured material and, more particularly, a nanostructured titanium alloy having an α-titanium structure developed with improved material properties.
    BACKGROUND
    [002] It is known that the microstructure plays a key role in establishing the mechanical properties. Depending on the processing method, a material structure can be developed to improve the material's properties. For example, it is possible to modify the grain structure or crystalline structure of the material, using mechanical or thermomechanical processing techniques.
    [003] U.S. Patent Application 2011/0179848 discloses a commercially pure titanium product having improved properties for biomedical applications. The titanium product has a nanocrystalline structure, which provides improved properties over the original mechanical properties, including mechanical strength, resistance to fatigue breakdown, and biomedical properties. It is reported that the known titanium product is first subjected to severe plastic deformation (SPD) using an equal channel angular pressing technique (ECAP) at a temperature not exceeding 450 ° C with the total accumulated real deformation and> 4, and then subsequently developed using a thermomechanical treatment with a degree of deformation of 40 to 80%. In particular, the thermomechanical treatment includes plastic deformation carried out with a gradual decrease in temperature in the range T = 450 ... 350 ° C and the deformation rate of 102 ... 10 "4s_l.
    [004] Although this known technique achieves a higher level of mechanical properties of commercially pure titanium, there is a need to increase the level of tensile and / or shear strength, as well as fatigue properties in titanium alloys for various engineering applications , including, but not limited to, biomedical, energy, high performance sporting goods and aerospace applications.
    SUMMARY
    [005] Taking into account these shortcomings, an objective of the invention, among others, is to increase the level of strength and fatigue resistance of a titanium alloy.
    [006] As a result, a nanostructured titanium alloy article is provided. The nanostructured alloy includes a developed titanium structure having at least 80% grains of a size <1.0 microns.
    BRIEF DESCRIPTION OF THE FIGURES
    [007] Examples of embodiments of the invention will be described with reference to the accompanying figures, in which: [008] Figure 1 is a micrograph of a known commercially pure titanium alloy taken using backscattered electron diffraction;
    [009] Figure 2 is a micrograph of a nanostructured alloy of commercially pure titanium according to the invention taken using backscattered electron diffraction;
    [010] Figure 3 is a graphical representation, obtained using backscattered electron diffraction, showing the size distribution of the known commercially pure titanium alloy;
    [011] Figure 4 is a graphical representation, obtained using backscattered electron diffraction, showing the grain size distribution of the commercially pure titanium nanostructured alloy according to the invention;
    [012] Figure 5 is a graphical representation, obtained using backscattered electron diffraction, showing the angle distribution of different crystallographic orientation of the known commercially pure titanium alloy;
    [013] Figure 6 is a graphical representation, obtained using backscattered electron diffraction, showing the angle distribution of different crystallographic orientation of the commercially pure titanium nanostructured alloy according to the invention;
    [014] Figure 7 is a graphical representation obtained using backscattered electron diffraction, showing the distribution of aspect ratio of the grain shape in the longitudinal plane of the commercially pure titanium nanostructured alloy according to the invention;
    [015] Figure 8 is a graphical representation, obtained using backscattered electron diffraction, showing the distribution of aspect ratio of the grain shape in the transverse plane of the commercially pure titanium nanostructured alloy according to the invention;
    [016] Figure 9 is a micrograph of the commercially pure titanium nanostructured alloy according to the invention having a plurality of equiaxial grains, obtained by transmission electron microscopy;
    [017] Figure 10 is a micrograph of the commercially pure titanium nanostructured alloy according to the invention having a plurality of grains with high displacement density, obtained by transmission electron microscopy;
    [018] Figure 11 is a micrograph of the commercially pure titanium nanostructured alloy according to the invention showing a plurality of sub-grains, obtained by transmission electron microscopy;
    [019] Figure 12 is a micrograph of a known Ti6Al4V titanium alloy taken using backscattered electron diffraction;
    [020] Figure 13 is a micrograph of a Ti6Al4V nanostructured titanium alloy according to the invention taken using backscattered electron diffraction;
    [021] Figure 14 is a graphical representation, obtained using backscattered electron diffraction, showing the grain size distribution of the Ti6Al4V nanostructured alloy according to the invention;
    [022] Figure 15 is a graphical representation, obtained using backscattered electron diffraction, showing the angle distribution of different crystallographic orientation of a known Ti6Al4V titanium alloy;
    [023] Figure 16 is a graphical representation, obtained using backscattered electron diffraction, showing the angle distribution of different crystallographic orientation of the Ti6Al4V nanostructured alloy according to the invention;
    [024] Figure 17 is a micrograph of a well-known Ti6Al4V ELI titanium alloy taken using backscattered electron diffraction;
    [025] Figure 18 is a micrograph of a Ti6Al4V ELI nanostructured alloy according to the invention taken using backscattered electron diffraction; and [026] Figure 19 is a graphical representation, obtained using backscattered electron diffraction, showing the grain size distribution of the Ti6Al4V ELI titanium alloy according to the invention;
    [027] Figure 20 is a graphical representation, obtained using backscattered electron diffraction, showing the angle distribution of different crystallographic orientation of a known Ti6Al4V ELI titanium alloy;
    [028] Figure 21 is a graphical representation, obtained using backscattered electron diffraction, showing the different crystallographic orientation of the Ti6Al4V ELI nanostructured alloy according to the invention. DETAILED DESCRIPTION OF THE MODE (S) [029] The invention is a nanostructured titanium alloy that can be used in different industries for the production of various useful articles, such as orthopedic implants, fasteners from the medical and aerospace sector , aerospace structural components, and high performance sporting goods. In an exemplary embodiment of the invention, a commercially pure titanium composition, having an α-titanium matrix that may contain retained β-titanium particles, is processed to develop the structure to achieve a nanostructure with at least 80% of the grains being < 1 micron. As a result, the nanostructured titanium alloy exhibits several changes in material properties such as an increase in tensile strength and / or shear strength and / or fatigue strength limit. In particular, the structure of the nanostructured titanium alloy is developed using a combination of thermomechanical processing steps according to the invention. This process provides a developed microstructure having a preponderance of ultrafine grain and / or nanocrystalline structures.
    [030] Figures 1, 12 and 17 show the initial commercially pure titanium alloy, Ti6Al4V, and the Ti6Al4V ELI microstructure, respectively. Figures 2, 13, and 18 show the resulting structure of the commercially pure titanium nanostructured alloy, Ti6Al4V, and Ti6Al4V ELI according to the invention, respectively. Examination of the figures clearly shows the difference between the initial titanium alloys and the nanostructured ones.
    [031] The workpiece may consist of several commercially available titanium alloys known in the art, such as commercially pure titanium alloys (Grades 1-4), Ti-6Al-4V, Ti-6Al-4V ELI, Ti-6 6Al-7Nb, Ti-ZR, or other known titanium alloys of alpha phase, almost alpha and alpha-beta.
    [032] Therefore, in other exemplary embodiments of the invention, an alpha-beta phase titanium alloy is processed from a combination of thermomechanical processing steps of the severe plastic deformation process type and the non-severe plastic deformation type to develop a nanostructure with at least 80% of the grains being <1 micron.
    [033] In an exemplary embodiment of the invention, a commercially pure coarse-grained titanium alloy is used for the workpiece which has the following composition, by weight percentage: nitrogen (N) 0.07% at most carbon (C) 0.1% maximum, hydrogen (H) 0.015% maximum, iron (Fe) 0.50% maximum, oxygen (0) 0.40% maximum, total other traces of impurities is 0 , 4% maximum, and titanium (Ti) as equilibrium.
    [034] Other titanium alloys may be used, including, but not limited to other commercially pure titanium alloys, Ti-6Al-4V, Ti-6Al-4V ELI, Ti-6Al-7Nb, and Ti-Zr. The standard chemical compositions of these titanium alloys can be found in Tables 1-3, which identify the standard chemical compositions by weight% max. (ASTM B348-11, Standard specification for Titanium and Titanium Alloy Bars and Billets; ASTM F1295 - 11 Standard Specification for Wrought Titanium-6Aluminum-7Niobium Alloy for Surgical Implant Applications; ASTM F136 - 12a Standard Specification for Wrought Titanium-6Aluminum-4Vanadium ELI (Extra Low Interstitial) Alloy for Surgical Implant Applications; and Titanium Alloy Ti-Zr, US Patent No. 8,168,012).
    [035] The workpiece, for example a rod or bar, is subjected to severe plastic deformation ("SPD") and thermomechanical process. The combined processing steps induce a large amount of shear deformation that significantly refines the initial structure by creating a large number of high angle grain boundaries (angle of different crystallographic orientation> 15 °) and high displacement density.
    [036] In particular, in the exemplary modality, the workpiece is processed using an equal channel angular pressing machine (ECAP-C), which consists of a rotating wheel having a circumferential groove and two stationary dies that form a channel that intersects at a defined angle. However, it is also possible, in other modalities, to subject the workpiece to severe plastic deformation using other types of known processes, including angular pressing of equal channel, angular extrusion of equal channel, angular pressing of equal channel with increment, angular pressing of equal channel with parallel channels, equal channel angular pressing with multiple channels, hydrostatic equal channel angular pressing, cyclic extrusion and compression, double roller equal channel angular extrusion, hydrostatic extrusion plus equal channel angular pressing, equal channel angular pressing plus hydrostatic extrusion, high-pressure continuous twisting, equal channel angular pressing, equal channel angular rolling or equal channel angular stretching.
    [037] First, using the ECAP-C machine, the workpiece is pressed into the groove of the wheel and is driven through the channel by frictional forces generated between the workpiece and the wheel. A commercially pure titanium alloy workpiece is processed using the ECAP-C machine at temperatures below 500 ° C, preferably 100-300 ° C. Other titanium alloys: Ti6Al4V, Ti6Al4V ELI, and Ti6Al7Nb are processed using the ECAP-C machine at a temperature below 650 ° C, preferably 400-600 ° C. The workpiece passes through the ECAP-C machine between 1 and 12 times, preferably 4 to 8 times. The die is defined by a channel intersection angle between Ψ = 75 ° and Ψ = 135 °, 90 ° to 120 °, and 100 ° to 110 °. To allow comparable structural evolution, a lower channel intersection angle will require fewer passages and / or a higher temperature, and an upper channel intersection angle will require more passages and / or a lower temperature. The workpiece is rotated around its longitudinal axis at an angle of 900 between each pass through the ECAP-C machine, which provides homogeneity in the developed structure. This method of rotation is known as the ECAP Bc route. However, in other modalities, the ECAP route can be changed, including, but not limited to, known routes A, C, BA, E, or some combination of these.
    [038] After the workpiece has been processed using severe plastic deformation from the ECAP-C processing steps, the workpiece is then subjected to an additional thermomechanical process using non-SPD metal forming techniques. In particular, thermomechanical processing further evolves the workpiece structure, more than the ECAP-C alone. In the exemplary mode, one or more thermomechanical processing steps can be performed, including, but not limited to, drawing, lamination, extrusion, forging, stamping, or some combination of these. In the exemplary embodiment, thermomechanical processing for commercially pure titanium alloy is carried out at temperatures T <500 ° C, preferably at room temperature up to 250 ° C. Thermomechanical processing of titanium alloys: Ti6Al4V, Ti6Al4V ELI, and Ti6A17Nb is carried out at temperatures not exceeding 550 ° C, preferably 400-500 ° C. Thermomechanical processing provides a reduction of> 35%, preferably> 65% of the cross-sectional area.
    [039] The combination of severe plastic deformation and thermomechanical processing substantially refines the initial structure, which consists of an α-titanium matrix that can contain retained β-titanium particles, to a predominantly submicron grain size. In the exemplary embodiment of the invention, the ECAP-C process fragments the initial grain structure by introducing a large number of flaps and displacements that are organized to form displacement cells with walls having a low angle of different crystallographic orientation <15 °.
    [040] During thermomechanical processing, the displacement density increases, and some of the low-angle cell walls evolve to high-angle sub-grain boundaries, improving strength by retaining ductility levels usable in industrial applications.
    [041] In the exemplary modality, the resulting nanostructured titanium alloy includes an α-titanium matrix that may contain retained β-titanium particles.
    [042] In the exemplary embodiment, the resulting titanium nanostructured alloy includes an α-titanium matrix that may contain retained β-titanium particles. Figures 4, 14, and 19 are histograms showing the grain size distribution in the commercially pure titanium nanostructured alloy Ti6Al4V, and Ti6Al4V ELI according to the invention, respectively. The average grain size of nanostructured titanium alloys is reduced from the initial titanium alloys. Figure 5 shows that the initial commercially pure titanium alloy has 90% -95% of the grain boundaries with an angle of different crystallographic orientation> 15 °, while Figure 6 shows that the commercially pure titanium nanostructured alloy retains 20% - 40% of the grain limits with an angle of different crystallographic orientation> 15 °, Figures 15 and 20 show that the initial titanium alloys: Ti6Al4V and Ti6Al4V ELI have 40-55% of the grain limits with an angle of different crystallographic orientation> 15 °, and Figures 16 and 21 show that the nanostructured Ti6Al4V and Ti6Al4V ELI retain 20-40% of the grain limits with an angle of different crystallographic orientation> 15 °. These distributions contribute to the retention of useful ductility levels.
    [043] Figures 7 and 8 show the distribution of grain aspect ratio in the longitudinal and transverse planes of the commercially pure titanium nanostructured alloy, which demonstrates an increased proportion of lower grain aspect ratio quotient in the plane longitudinal compared to the transverse plane. The similar aspect ratio is observed in nanostructured alloys of Ti6AI4V and Ti6Al4V ELI.
    [044] The size of these displacement cells and sub-grains can be measured by a variety of techniques, including, but not limited to, transmission electron microscopy (TEM) and X-ray diffraction (XRD), in particular, the adjustment of the total multi-convolutional profile extended as applicable to XRD. For example, Figures 9-11 are TEM micrographs showing equiaxial grains, high displacement density, and a high number of sub-grains in the nanostructured alloy of commercially pure titanium, according to the invention. In Figure 9, the equiaxial grains are highlighted by continuous lines, while in Figure 10 the regions of high displacement density are highlighted with continuous lines. In Figure 11, the grains are highlighted with continuous lines and the sub grains are highlighted with dotted lines.
    [045] Table 4 shows the levels of room temperature mechanical properties typical of the initial titanium alloys and the nanostructured titanium alloys according to the invention that can be achieved due to the development of structure. | TÍ6A14V ELI | | IIIII Ί * Fatigue strength limit measured at 107 cycles [046] Table 4 clearly shows that the resulting titanium nanostructured alloy exhibits several changes in material properties, such as an increase in tensile strength and / or shear strength and / or fatigue strength limit. In particular, nanostructured titanium alloys according to the exemplary embodiment of the invention have a total tensile elongation greater than 10%, and an area reduction greater than 25%. In addition, nanostructured titanium alloys have at least 80% of grains with a size <1.0 microns, with about 2040% of all grains with high angle grain limits, and> 80% of all grains have a grain shape aspect ratio in the range of 0.3 to 0.7. In addition, nanostructured titanium alloy articles have grains with an average crystallite size of less than 100 nanometers and a displacement density> 1015m-2.
    [047] Thus, the invention provides a nanocrystalline structure having improved properties over the initial workpiece, as a result of severe plastic deformation and thermomechanical processing.
    [048] Titanium alloys that can be used in accordance with the present invention include commercially pure titanium alloys (grades 1-4), Ti-6Al-4V, Ti-6Al-4V ELI, Ti-Zr or Ti-6Al -7Nb. The nanostructured titanium alloy according to the present invention can be used to produce useful articles with improved material properties, including aerospace fasteners, aerospace structural components, high performance sporting goods, as well as articles for medical applications, such as column rods spine, screws, intramedullary nails, bone plates and other orthopedic implants. For example, the invention can provide aerospace fasteners composed of nanostructured Ti alloy having an increased tensile strength limit, such as greater than 1200 MPa, and greater shear strength, such as greater than 650 MPa.
    [049] The previous one illustrates some possibilities for the practice of the invention. Many other modalities are possible within the scope and spirit of the invention. It is therefore intended that the foregoing description is considered to be illustrative rather than limiting, and that the scope of the invention is determined by the appended claims in conjunction with its full range of equivalents.
    权利要求:
    Claims (22)
    [1]
    1. NANO-STRUCTURED TITANIUM ALLOY ARTICLE, comprising one of the commercially pure titanium alloys (Grades 1-4), Ti6Al4V, Ti6Al4V-ELI, Ti6Al7Nb or Ti-Zr, characterized by a developed titanium structure comprising:> 80% section grain area being a size <1.0 micron, an average crystallite size of <100 nanometers, fraction of number 20-40% of grains including high grain angle limits with an angle of different crystallographic orientation> 15 ° , and fraction of number> 80% of grains having a grain shape aspect ratio in the range of 0.3 to 0.7.
    [2]
    2. ARTICLE, according to claim 1, characterized by the developed titanium structure being a developed α-titanium structure.
    [3]
    3. ARTICLE, according to claim 1, characterized by the grains being α phase grains.
    [4]
    4. ARTICLE, according to claim 1, characterized by the developed titanium structure having a displacement density> 1015m-2.
    [5]
    5. ARTICLE, according to claim 1, characterized by the developed titanium structure being processed from a combination of thermomechanical processing steps of a type of severe and non-severe plastic deformation process.
    [6]
    6. ARTICLE, according to claim 1, characterized by the developed titanium structure having a tensile strength limit> 1200 MPa.
    [7]
    7. ARTICLE, according to claim 6, characterized by the limit of tensile strength being> 1400 MPa.
    [8]
    8. ARTICLE, according to claim 7, characterized by the developed titanium structure having a total tensile elongation> 10%.
    [9]
    9. ARTICLE, according to claim 8, characterized by the developed titanium structure having an area reduction> 25%.
    [10]
    10. ARTICLE, according to claim 9, characterized by the developed titanium structure having a shear strength limit> 650 MPa.
    [11]
    11. ARTICLE according to claim 10, characterized in that a shear strength limit is> 740 MPa.
    [12]
    12. ARTICLE, according to claim 10, characterized by the developed titanium structure having an axial fatigue strength limit> 700 MPa measured at 107 cycles.
    [13]
    13. ARTICLE according to claim 12, characterized by a limit of resistance to axial fatigue being> 950 MPa measured at 107 cycles.
    [14]
    14. ARTICLE, according to claim 12, characterized by the developed titanium structure having a limit of resistance to axial fatigue of cantilever rotation beam> 650 MPa measured at 107 cycles.
    [15]
    15. ARTICLE according to claim 14, characterized by the limit of resistance to axial fatigue of cantilever rotation beam> 700 MPa measured at 107 cycles.
    [16]
    16. ARTICLE, according to claim 1, characterized by the developed titanium structure including α-titanium matrix with retained β-titanium particles.
    [17]
    17. ARTICLE, according to claim 1, characterized by the developed titanium structure having a composition in weight percentage: nitrogen (N) 0.07%, at most; carbon (C) 0.1% maximum; hydrogen (H) 0.015% maximum; iron (Fe) 0.50% maximum; oxygen (0) 0.40% at most; impurity traces 0.40% maximum; and a titanium (Ti) balance.
    [18]
    18. ARTICLE, according to claim 17, characterized by the developed titanium structure having a composition in weight percentage: Aluminum (Al) 6.75% at most; and Vanadium (V) 4.5% maximum.
    [19]
    19. ARTICLE, according to claim 17, characterized by the developed titanium structure having a composition in weight percentage: Aluminum (Al) 6.5% at most; Niobium (Nb) maximum 7.5%; and Tantalum (Ta) 0.5%, at most.
    [20]
    20. ARTICLE, according to claim 17, characterized by the developed titanium structure having a composition in weight percentage: Zirconium (Zr) maximum 25%; and other elements maximum 1%.
    [21]
    21. METHOD FOR MANUFACTURING A NANO-STRUCTURED TITANIUM ALLOY, as defined in claims 1 to 20, characterized by comprising the steps of: providing a piece of a commercially pure titanium alloy (Grades 1-4); induce severe plastic deformation to the workpiece using an angular channel pressing machine equal to temperatures between 100 ° C and 300 ° C and having a die set at an intersection channel angle between Ψ = 75 ° and Ψ = 135 ° ; and subject the part to thermomechanical processing at temperatures between room temperature and 250 ° C to prepare an article having a reduction in cross-sectional area> 35%.
    [22]
    22. METHOD FOR MANUFACTURING A NANO-STRUCTURED TITANIUM ALLOY, characterized by comprising the steps of: providing a part made of titanium alloys Ti6Al4V, Ti6Al4V-ELI, Ti6Al7Nb or Ti-Z; induce severe plastic deformation to the workpiece using an angular channel pressing machine equal to temperatures below 500 ° C and having a die defined by a channel intersection angle between Ψ = 75 ° and Ψ = 135 °; and subjecting the part to thermomechanical processing at temperatures below 500 ° C to prepare an article having a reduction in cross-sectional area> 35%.
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    法律状态:
    2019-07-09| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|
    2020-02-11| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-03-17| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 14/03/2014, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    US13/833,148|US20140271336A1|2013-03-15|2013-03-15|Nanostructured Titanium Alloy And Method For Thermomechanically Processing The Same|
    US13/833,148|2013-03-15|
    PCT/US2014/028197|WO2014143983A1|2013-03-15|2014-03-14|Nanostructured titanium alloy and method for thermomechanically processing the same|
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