![]() METHOD FOR REFINING ALPHA-BETA GRAIN SIZE IN AN ALPHA-BETA TITANIUM ALLOY WORK PIECE
专利摘要:
abstract “thermomechanical processing of alpha-beta titanium alloys” an embodiment of a method of refining alpha phase grain size in an alpha-beta titanium alloy comprises working an alpha-beta titanium alloy at a first working temperature within of a first temperature range in the alpha-beta phase field of the alpha-beta titanium alloy. the alloy is slowly cooled from the first working temperature. Upon completion of work at and slow cooling from the first working temperature, the alloy comprises a primary globularized alpha phase particle microstructure. the alloy is worked at a second working temperature within a second temperature range in the alpha-beta phase field. the second working temperature is lower than the first working temperature. a is worked at a third working temperature in a third temperature range in the alpha-beta phase field. the third working temperature is lower than the second working temperature. After working at the third working temperature, the titanium alloy comprises a desired refined alpha phase grain size. 公开号:BR112015015681B1 申请号:R112015015681-9 申请日:2014-02-28 公开日:2020-02-11 发明作者:Jean-Philippe A. Thomas;Ramesh S. Minisandram;Robin M. Forbes Jones;John V. Mantione;David J. Bryan 申请人:Ati Properties Llc; IPC主号:
专利说明:
1/35 “METHOD FOR REFINING SIZE OF ALPHA-STAIN GRAIN IN A TITANIUM ALLOY WORK PIECE ALPHA-BETA” DECLARATION ON RESEARCH OR DEVELOPMENT SPONSORED BY THE FEDERAL GOVERNMENT [001] This invention was made with the support of the United States government under NIST Contract Number 70NANB7H7038, granted by the National Institute of Standards and Technology (NIST), United States Department of Commerce. The United States government may have certain rights in the invention. TECHNOLOGY FUNDAMENTALS TECHNOLOGY FIELD [002] The present invention relates to methods for processing alpha-beta titanium alloys. More specifically, the disclosure is directed to methods for processing alpha-beta titanium alloys to promote a fine grain, superfine grain or ultrafine grain microstructure. DESCRIPTION OF THE FUNDAMENTALS OF THE TECHNOLOGY [003] Alpha-beta titanium alloys having fine-grain (FG), superfine-grain (SFG) or ultra-fine-grain (UFG) microstructures have been shown to exhibit a number of beneficial properties such as, for example, improved formability, lower formation flow stress (which is beneficial for deformation formation) and higher flow stress at ambient to moderate service temperatures. [004] As used here, when referring to the microstructure of titanium alloys: the term fine grain refers to alpha grain sizes in the range from 15 pm to greater than 5 pm; the term superfine grain refers to alpha grain sizes from 5 pm to greater than 10 pm; and the term ultrafine grain refers to alpha grain sizes of 1.0 pm or less. [005] Known commercial methods for forging titanium and titanium alloys to produce coarse-grained or fine-grained microstructures employ Petition 870190084256, of 08/28/2019, p. 5/77 2/35 formation from 0.03 s-1 to 0.10 s-1 using multiple reheating and forging steps. [006] The known methods for the manufacture of fine-grained, very fine-grained or ultra-fine grained microstructures apply a multi-axis forging process (MAF) at an ultralent deformation rate of 0.001 s-1 or slower (see, for example, example, G. Salishchev, et. al., Materials Science Forum, Vol. 584586, pp. 783-788 (2008)). The generic MAF process is described in, for example, C. Desrayaud, et. al, Journal of Materials Processing Technology, 172, pp. 152-156 (2006). In addition to the MAF process, it is known that an equal channel angular extrusion (ECAE) process, otherwise called equal channel angular pressing (ECAP), can be used to achieve fine grain, very fine grain or ultra fine grain microstructures. titanium and titanium alloys. A description of an ECAP process is found, for example, in V.M. Segal, USSR Patent 575892 (1977), and for Titanium and Ti-6-4, in S.L. Semiatin and D.P. Delo, Materials and Design, Vol. 21, pp 311322 (2000). However, the ECAP process also requires very low strain rates and very low temperatures in isothermal or quasi-isothermal conditions. When using such high-strength processes, such as MAF and ECAP, any starting microstructure can eventually be transformed into an ultrathin grain microstructure. However, for economic reasons that are still described in this document, only laboratory-scale MAF and ECAP processing is currently conducted. [007] The key to grain refinement in the ultra-slow strain rate MAF and ECAP processes is the ability to operate continuously in a dynamic recrystallization regime which is a result of the ultra slow strain rates used, ie 0.001 s-1 or more slow. During dynamic recrystallization, the grains simultaneously nucleus, grow and accumulate displacements. The generation of displacements within the newly nucleated grains continuously reduces the force Petition 870190084256, of 08/28/2019, p. 6/77 3/35 motive for grain growth, and grain nucleation is energetically favorable. The ultra-slow strain rate MAF and ECAP processes use dynamic recrystallization to continuously recrystallize grains during the forging process. [008] A method for processing titanium alloys for grain refinement is disclosed in International Patent Publication WO 98/17386 (Publication WO'386) which is incorporated by reference in its entirety into this document. The method in Publication WO'386 discloses heating and deforming an alloy to form fine-grained microstructure as a result of dynamic recrystallization. [009] The relatively uniform billets of ultra-fine grain Ti-6-4 alloy (UNS R56400) can be produced using the ultra slow creep rate MAF or ECAP processes, but the cumulative time taken to perform the MAF or ECAP steps can be excessive in a commercial environment. In addition, conventional large-scale commercially available open die forging equipment may not be able to achieve the ultralent strain rates required in these modalities, and therefore customized forging equipment may be required to perform rate MAF or ECAP. of ultralent deformation on a production scale. [010] It is common knowledge that thinner lamellar starting microstructures require less deformation to produce thin to globularized ultrathin microstructures. However, while it was possible to make laboratory scale quantities of titanium and ultra-fine alpha grain size titanium alloys using isothermal or quasi-isothermal conditions, scaling the process on a laboratory scale can be problematic due to yield losses. In addition, isothermal processing on an industrial scale proves to be cost prohibitive due to the expense of operating the equipment. High-throughput techniques involving non-isothermal open matrix processes have proved difficult because of the speed Petition 870190084256, of 08/28/2019, p. 7/77 4/35 very slow forging times required, which requires long periods of use of the equipment, and because of cracks related to cooling, which reduces throughput. In addition, alpha lamellar structures such as tempered exhibit low ductility, especially at low processing temperatures. [011] It is generally known that alpha-beta titanium alloys in which the microstructure is formed of globularized alpha phase particles exhibit better ductility than alpha-beta titanium alloys having lamellar alpha microstructures. However, the forging of alpha-beta titanium alloys with globularized alpha phase particles does not produce significant particle refinement. For example, since alpha phase particles have thickened to a certain size, for example, 10 pm or greater, it is almost impossible, using conventional techniques, to reduce the size of such particles during subsequent thermomechanical processing, as observed by optical metallography. [012] A process for refining the microstructure of titanium alloys is disclosed in European Patent No. 1 546 429 B1 (the EP'429 Patent) which is hereby incorporated by reference in its entirety. In the EP'429 process, since the alpha phase was globularized at high temperature, the alloy is quenched to create secondary alpha phase in the form of a thin lamellar alpha phase between relatively thick globular alpha phase particles. Subsequent forging at a lower temperature than the first alpha processing leads to globularization of the thin alpha lamellae into fine alpha phase particles. The resulting microstructure is a mixture of coarse and fine alpha phase particles. Due to the coarse alpha phase particles, the microstructure resulting from methods disclosed in the EP'429 patent is not suitable for further grain refinement in a fully formed microstructure of ultrafine to fine alpha phase grains. [013] US Patent Publication 2012-0060981 A1 (US'981 publication), which is incorporated herein by reference in its entirety, discloses a sc Petition 870190084256, of 08/28/2019, p. 8/77 5/35 industrial length to provide redundant work through multiple turning and stretching forging steps (the MUD Process). US Publication '981 discloses starting structures comprising alpha lamellar structures generated by quenching from the beta phase field of titanium or a titanium alloy. The MUD Process is performed at low temperatures to inhibit excessive particle growth during the deformation sequence and alternating reheating steps. The lamellar starting stock exhibits low ductility at the low temperatures used and scaling for open die forgings can be problematic in terms of yield. [014] It would be advantageous to provide a process to produce titanium alloys having fine, very fine or ultrafine grain microstructure that accommodates higher strain rates, reduces the required processing time and / or eliminates the need for custom forging equipment. SUMMARY [015] In accordance with a non-limiting aspect of the present disclosure, a method for refining alpha phase grain size in an alpha-beta titanium alloy comprises working an alpha-beta titanium alloy at a first working temperature within a first temperature range. The first temperature range is an alpha-beta phase field of the alpha-beta titanium alloy. The alpha-beta titanium alloy is cooled slowly from the first working temperature. Upon completion of work on and slow cooling from the first working temperature, the alpha-beta titanium alloy comprises a primary globularized alpha phase particle microstructure. The alpha-beta titanium alloy is subsequently worked at a second working temperature within a second temperature range. The second working temperature is lower than the first working temperature and is also in the alpha-beta phase field of the alpha-beta titanium alloy. [016] In a non-limiting modality, subsequent to work on the second Petition 870190084256, of 08/28/2019, p. 9/77 6/35 working temperature, the alpha-beta titanium alloy is worked at a third working temperature in a final temperature range. The third working temperature is lower than the second working temperature and the third temperature range is in the alpha-beta phase field of the alpha-beta titanium alloy. After working the alpha-beta titanium alloy at the third working temperature, a desired refined alpha phase grain size is achieved. [017] In another non-limiting modality, after working the alpha-beta titanium alloy at the second working temperature, and before working the alpha-beta titanium alloy at the third working temperature, the alpha-beta titanium alloy is worked at one or more progressively lower working temperatures. Each of the one or more progressively lower working temperatures is lower than the second working temperature. Each of the one or more progressively lower fourth working temperatures is within one of a fourth temperature range and the third temperature range. Each of the fourth working temperatures is lower than the fourth immediately preceding working temperature. In a non-limiting mode, at least one of working the alpha-beta titanium alloy at the first temperature, working the alpha-beta titanium alloy at the second temperature, working the alpha-beta titanium alloy at the third temperature and working the titanium alloy alpha-beta at one or more progressively lower working temperatures comprises at least one step of forging in an open die press. In another non-limiting modality, at least one of working the alpha-beta titanium alloy at the first temperature, working the alpha-beta titanium alloy at the second temperature, working the alpha-beta titanium alloy at the third temperature and working the alpha-beta titanium at one or more fourth progressively lower working temperatures comprises a plurality of forging steps in an open die press, the method further comprising reheating the alpha-beta titanium alloy in an intermediate way during Petition 870190084256, of 08/28/2019, p. 10/77 7/35 the successive press forging steps. [018] According to another aspect of the present disclosure, a non-limiting embodiment of a method for refining alpha phase grain size in an alpha-beta titanium alloy comprises forging an alpha-beta titanium alloy at a first forging temperature within of a first forging temperature range. The forging of the alpha-beta titanium alloy at the first forging temperature comprises at least one pass of both turning forging and stretching forging. The first forging temperature range comprises a temperature range spanning 300 ° F below the beta transus temperature of the alpha-beta titanium alloy to a temperature of 30 ° F lower than the beta transus temperature of the alpha-beta titanium alloy. After forging the alpha-beta titanium alloy at the first forging temperature, the alpha-beta titanium alloy is cooled slowly from the first forging temperature. [019] The alpha-beta titanium alloy is forged at a second forging temperature within a second forging temperature range. The forging of the alpha-beta titanium alloy at the second forging temperature comprises at least one pass from both turning forging and stretching forging. The second forging temperature range is 600 ° F below the beta transus temperature of the alpha-beta titanium alloy to 350 ° F below the beta transus temperature of the alpha-beta titanium alloy and the second forging temperature is lower than the first forging temperature. [020] The alpha-beta titanium alloy is forged at a third forging temperature within a third forging temperature range. The forging of the alpha-beta titanium alloy at the third forging temperature comprises radial forging. The third forging temperature range is 1000 ° F and 1400 ° F, and the final forging temperature is lower than the second forging temperature. Petition 870190084256, of 08/28/2019, p. 11/77 8/35 [021] In a non-limiting mode, after forging the alpha-beta titanium alloy at the second forging temperature, and before forging the alpha-beta titanium alloy at the third forging temperature, the alpha-beta titanium alloy can be annealed. [022] In a non-limiting mode, after forging the alphabetical titanium alloy at the second working temperature, and before forging the alpha-beta titanium alloy at the third forging temperature, the alpha-beta titanium alloy is forged in a or more progressively lower fourth forging temperatures. The progressively lower one or more fourth forging temperatures are lower than the second forging temperature. Each of the one or more progressively lower forging temperatures is within one of the second temperature range and the third temperature range. Each of the progressively lower fourth working temperatures is lower than the immediately preceding fourth working temperature. [023] In accordance with another aspect of the present disclosure, a non-limiting embodiment of a method for refining alpha phase grain size in an alpha-beta titanium alloy comprises forging an alpha-beta titanium alloy comprising a phase particle microstructure. globularized alpha at an initial forging temperature within an initial forging temperature range. The forging of the alpha-beta titanium alloy at the initial forging temperature comprises at least one pass of both turning forging and stretching forging. The initial forging temperature range is 500 ° F below the beta transus temperature of the alpha-beta titanium alloy to 350 ° F below the beta transus temperature of the alpha-beta titanium alloy. [024] The workpiece is forged at a final forging temperature within a final forging temperature range. Forging the workpiece at the final forging temperature comprises radial forging. The final forging temperature range is 1000 ° F to 1400 ° F. The forging temperature Petition 870190084256, of 08/28/2019, p. 12/77 Final 9/35 is lower than the initial forging temperature. BRIEF DESCRIPTION OF THE DRAWINGS [025] The characteristics and advantages of articles and methods described here can be better understood by reference to the accompanying drawings, in which: [026] FIG. 1 is a flow diagram of a non-limiting embodiment of a method of refining alpha phase grain size in an alpha-beta titanium alloy according to the present disclosure; [027] FIG. 2 is a schematic illustration of the microstructure of alpha-beta titanium alloys after processing steps according to a non-limiting embodiment of the method of the present disclosure; [028] FIG. 3 is a backscattered electron micrograph (BSE) of the microstructure of an alpha-beta phase titanium alloy workpiece forged and slowly cooled according to a non-limiting modality of the method of the present disclosure; [029] FIG. 4 is a BSE micrograph of the microstructure of a titanium alloy of alpha-beta phase forged and cooled slowly according to a non-limiting modality of the method of the present disclosure; [030] FIG. 5 an electrospray scattered micrograph (EBSD) of a titanium alloy of alpha-beta phase forged and cooled slowly according to a non-limiting modality of the method of the present disclosure; [031] FIG. 6A is a BSE micrograph of the microstructure of an alpha-beta phase titanium alloy forged and slowly cooled according to a non-limiting embodiment of the present disclosure and FIG. 6B is a BSE micrograph of the microstructure of a titanium alloy of alpha-beta phase forged and cooled slowly according to the non-limiting modality of Fig. 6A which has been additionally forged and annealed according to a non-limiting modality of the method of the present disclosure ; Petition 870190084256, of 08/28/2019, p. 13/77 10/35 [032] FIG. 7 is an EBSD micrograph of a slowly forged and slowly cooled alphabetical titanium alloy which was further forged and annealed according to a non-limiting embodiment of the method of the present disclosure; [033] FIG. 8 is an EBSD micrograph of a slowly forged and slowly cooled alphabetical titanium alloy which was further forged and annealed according to a non-limiting embodiment of the method of the present disclosure; [034] FIG. 9A is an EBSD micrograph of the sample of Example 2 which is a slowly forged and slowly cooled alpha-beta titanium alloy which has been further forged and annealed according to a non-limiting embodiment of the method of the present disclosure; [035] FIG. 9B is a graph showing the concentration of grains having a particular grain size in the sample of Example 2 shown in FIG 9A; [036] FIG. 9C is a graph of the disorientation distribution of the alpha phase grain boundaries of the sample of Example 2 shown in FIG. 9A; [037] FIGS. 10A and 10B are BSE micrographs, respectively, of the first and second forged and annealed samples; [038] FIG. 11 is an EBSD micrograph of the first sample in Example 3; [039] FIG. 12 is an EBSD micrograph of the second sample from Example 3; [040] FIG. 13A is an EBSD micrograph of the second sample from Example 3; [041] FIG. 13B is a graph of the relative amount of alpha grains in the sample of Example 3 having particular grain sizes; [042] FIG. 13C is a graph of the disorientation distribution of the alpha phase grain limits in the sample of Example 3; [043] FIG. 14A is an EBSD micrograph of the second sample from Example 3; [044] FIG. 14B is a graph of the relative amount of alpha grains in the sample Petition 870190084256, of 08/28/2019, p. 14/77 11/35 of Example 3 having particular grain sizes; [045] FIG. 14C is a graph of the disorientation distribution of the alpha phase grain limits in the sample of Example 3; [046] FIG. 15 is a BSE micrograph of the microstructure of a slowly forged and slowly cooled alpha-beta titanium alloy which was further forged according to a non-limiting modality of the method of the present disclosure; [047] FIG. 16 is an EBSD micrograph of a slowly forged and slowly cooled alphabetical titanium alloy which was further forged according to a non-limiting embodiment of the method of the present disclosure; [048] FIG. 17A is an EBSD micrograph of the sample from Example 4 which is a slowly forged and slowly cooled alpha-beta titanium alloy which has been further forged according to a non-limiting embodiment of the method of the present disclosure; [049] FIG. 17B is a graph showing the concentration of grains having a particular grain size in the sample of Example 4 shown in FIG 17A; [050] FIG. 17C is a graph of the disorientation distribution of the alpha phase grain limits of the sample of Example 4 shown in FIG. 17A; [051] FIG. 18 is an EBSD micrograph of a slowly forged and slowly cooled alphabetical titanium alloy which was further forged according to a non-limiting modality of the method of the present disclosure; [052] FIG. 19A is an EBSD micrograph of the sample from Example 4 which is a slowly forged and slowly cooled alpha-beta titanium alloy which was further forged according to a non-limiting embodiment of the method of the present disclosure; [053] FIG. 19B is a graph showing the concentration of grains having a particular grain size in the sample of Example 4 shown in FIG 19A; and [054] FIG. 19C is a graph of the distribution of boundary disorientation Petition 870190084256, of 08/28/2019, p. 15/77 12/35 of alpha phase grain from the sample of Example 4 shown in FIG. 19A; [055] The reader will appreciate the previous details, as well as others, when considering the following detailed description of certain non-limiting modalities in accordance with the present disclosure. DETAILED DESCRIPTION OF CERTAIN NON-LIMITING MODALITIES [056] It is to be understood that certain descriptions of the modalities described here have been simplified to illustrate only those elements, characteristics and aspects that are relevant to a clear understanding of the disclosed modalities, while eliminating, for the purposes of clarity , other elements, characteristics and aspects. Persons skilled in the art, upon consideration of the present description of the disclosed modalities, will recognize that other elements and / or characteristics may be desirable in a particular implementation or application of the disclosed modalities. However, as these other elements and / or characteristics can be readily confirmed and implemented by persons skilled in the art upon consideration of the present description of the disclosed modalities and, therefore, are not necessary for a complete understanding of the revealed modalities, a description of such elements and / or features is not provided here. As such, it is to be understood that the description set out here is merely exemplary and illustrative of the disclosed modalities and is not intended to limit the scope of the invention as defined solely by the claims. [057] In addition, any numerical range recited here is intended to include all the sub-ranges included therein. For example, a range from 1 to 10 is intended to include all sub-ranges between (and including) the minimum recited value of 1 and the maximum recited value of 10, that is, having a minimum value equal to or greater than 1 and a value maximum equal to or less than 10. Any maximum numerical limitation mentioned here is intended to include all lower numerical limits included here and which Petition 870190084256, of 08/28/2019, p. 16/77 13/35 any minimum numerical limitation mentioned here is intended to include all the higher numerical limits included here. Accordingly, claimants reserve the right to change the present disclosure, including the claims, to expressly mention any sub-range subsumed within the ranges expressly cited herein. All of these bands are intended to be inherently disclosed herein so that the amendment to expressly recite any such sub-bands would meet the requirements of 35 U.S.C. § 112, first paragraph and 35 U.S.C. § 132 (a). [058] The grammatical articles "one", "one", "a" and "o", as used herein, are intended to include "at least one" or "one or more", unless otherwise specified. Thus, articles are used here to refer to one or more of one (that is, at least one) of the grammatical objects of the article. As an example, “a component” means one or more components and, therefore, possibly more than one component is contemplated and can be used or used in an implementation of the described modalities. [059] All percentages and ratios are calculated based on the total weight of the alloy composition, unless otherwise stated. [060] Any patent, publication or other disclosure material that is said to be incorporated, in whole or in part, by reference in this document is incorporated here only insofar as the incorporated material does not conflict with the definitions, statements, or other existing disclosure material set out in this disclosure. As such, and to the extent necessary, the disclosure as set forth herein cancels any conflicting material incorporated herein by reference. Any material, or portion thereof, that is said to be incorporated by reference in this document, but which conflicts with definitions, statements, or other disclosure material contained herein is incorporated only to the extent that there is no conflict between that material and the existing disclosure material. Petition 870190084256, of 08/28/2019, p. 17/77 14/35 [061] This disclosure includes descriptions of several modalities. It is to be understood that all the modalities described here are exemplary, illustrative and not limiting. Thus, the invention is not limited by the description of the various exemplary, illustrative and non-limiting modalities. Instead, the invention is defined solely by the claims which can be amended to recite any features expressly or inherently described or otherwise expressly or inherently supported by the present disclosure. [062] According to one aspect of the disclosure, FIG. 1 is a flow diagram illustrating various non-limiting modalities of a method 100 for refining alpha phase grain size in an alpha-beta titanium alloy according to the present disclosure. Figure 2 is a schematic illustration of a microstructure 200 that results from processing steps in accordance with the present disclosure. In a non-limiting embodiment according to the present disclosure, a method 100 for refining alpha phase grain size in an alpha-beta titanium alloy comprises providing 102 an alpha-beta titanium alloy comprising a lamellar alpha phase microstructure 202. A person knowledgeable in the art knows that a lamellar alpha phase microstructure 202 is obtained by beta heat treatment of an alpha-beta titanium alloy followed by quenching. In a non-limiting modality, an alpha-beta titanium alloy is heat treated in beta and tempered 104 in order to provide an alpha-lamellar phase microstructure 202. In a non-limiting modality, the beta heat treatment of the alloy still comprises working at binds to the beta heat treatment temperature. In yet another non-limiting modality, working the alloy at the beta heat treatment temperature comprises one or more of rolled forging, stamping, rough rolling, open die forging, printing die forging, press forging, automatic hot forging, forging radial, turned forging, stretch forging and multiaxial forging. [063] Still with reference to FIGS. 1 and 2, a non-limiting modality of Petition 870190084256, of 08/28/2019, p. 18/77 A method 100 for refining alpha phase grain size in an alphabetical titanium alloy comprises working the alloy at a first working temperature within a first temperature range. It will be recognized that the alloy can be forged one or more times in the first temperature range and can be forged at one or more temperatures in the first temperature range. In a non-limiting mode, when the alloy is worked more than once in the first temperature range, the alloy is first worked at a lower temperature in the first temperature range and then subsequently worked at a higher temperature in the first temperature range temperature. In a non-limiting mode, when the alloy is worked more than once in the first temperature range, the alloy is first worked at a higher temperature in the first temperature range and then subsequently worked at a lower temperature in the first temperature range temperature. The first temperature range is in the alpha-beta phase field of the alpha-beta titanium alloy. In a non-limiting embodiment, the first temperature range is a temperature range that results in a microstructure that comprises primary globular alpha phase particles. The phrase primary globular alpha phase particles, as used herein, refers to generally equiaxial particles comprising the hexagonal alpha phase allotrope intimately packaged in titanium metal that forms after working at the first working temperature in accordance with the present disclosure, or that forms from any other thermomechanical process known now or in the future of a person skilled in the art. In a non-limiting mode, the first temperature range is in the highest domain of the alpha-beta phase field. In a specific non-limiting mode, the first temperature range is 300 ° F below the beta transus to a temperature 30 ° F below a beta transus temperature of the alloy. It will be recognized that the alloy work 104 at temperatures within the first temperature range, which can be relatively high in the alpha-beta phase domain, produces a microstructure 204 comprising Petition 870190084256, of 08/28/2019, p. 19/77 16/35 primary globular alpha phase particles. [064] The term work, as used here, refers to thermomechanical work or thermomechanical processing (“TMP”). Thermomechanical work is defined here as generally covering a variety of metal forming processes combining controlled heat and deformation treatments to obtain synergistic effects such as, for example, and without limitation, improved strength without loss of stiffness. This definition of thermomechanical work is consistent with the meaning attributed, for example, in ASM Materials Engineering Dictionary, J.R. Davis, ed., ASM International (1992), p. 480. In addition, as used herein, the terms forging, forging in an open die press, turning forging, stretching forging and radial forging refer to forms of thermomechanical work. The term die press forging, as used herein, refers to the forging of metal or metal alloy between dies, in which the material flow is not completely restricted, by mechanical or hydraulic pressure, accompanied by a single working stroke from press for each matrix session. This definition of open press die forging is consistent with the meaning given, for example, in ASM Materials Engineering Dictionary, J.R. Davis, ed., ASM International (1992), pp. 298 and 343. The term radial forging, as used herein, refers to a process that uses two or more anvils or mobile dies to produce forgings with constant or variable diameters along their length. This definition of radial forging is consistent with the meaning given, for example, in ASM Materials Engineering Dictionary, J.R. Davis, ed., ASM International (1992), p. 354. The term turning forging, as used herein, refers to forging a workpiece in an open die such that a length of the workpiece generally decreases and the cross section of the workpiece generally increases. The term turning forging, as used herein, refers to forging a workpiece in an open die such that a Petition 870190084256, of 08/28/2019, p. 20/77 17/35 length of the workpiece generally increases and the cross section of the workpiece generally decreases. Those having common knowledge of the technique in the metallurgical arts will readily understand the meanings of these various terms. [065] In a non-limiting method according to the present disclosure, the alpha-beta titanium alloy is selected from a Ti-6Al-4V alloy (UNS R56400), a Ti-6Al-4V ELI alloy (UNS R56401) , a Ti-6Al-2Sn-4Zr-2Mo alloy (UNS R54620), a Ti-6Al-2Sn-4Zr-6Mo alloy (UNS R56260) and a Ti-4Al-2.5V-1.5Fe alloy (UNS 54250; ATI 425® alloy). In another non-limiting modality of the methods according to the present disclosure, the titanium alpha-beta alloy is selected from Ti6Al-4V alloy (UNS R56400) and Ti-6Al-4V ELI alloy (UNS R56401). In a non-limiting modality specific to the methods according to the present disclosure, the titanium alpha-beta alloy is a Ti-4Al-2.5V-1.5Fe alloy (UNS 54250). [066] After working 106 the alloy at the first working temperature in the first temperature range, the alloy is cooled slowly 108 from the first working temperature. By slow cooling of the alloy from the first working temperature, the microstructure comprising the primary globular alpha phase is maintained and is not transformed into the secondary alpha lamellar phases, as occurs after rapid cooling, or quenching, as disclosed in EP'429, discussed above. A microstructure formed of globularized alpha phase particles is believed to exhibit better ductility at low forging temperatures than a microstructure comprising lamellar alpha phase. [067] The terms slow cooling and slow cooling, as used herein, refer to the cooling of the workpiece at a cooling rate of no more than 5 ° F per minute. In a non-limiting mode, slow cooling 108 comprises oven cooling at a preprogrammed deceleration rate of no more than 5 ° F per minute. It will be recognized that cooling Petition 870190084256, of 08/28/2019, p. 21/77 18/35 slow according to the present disclosure may comprise slow cooling to room temperature or slow cooling to a lower working temperature at which the alloy will still be worked. In a non-limiting mode, slow cooling comprises transferring the alpha-beta titanium alloy from an oven chamber at the first working temperature to an oven chamber at a second working temperature. In a specific non-limiting modality, when the diameter of the workpiece is greater than or equal to 12 inches, and it is ensured that the workpiece has sufficient thermal inertia, the slow cooling comprises transferring the alpha-beta titanium alloy from a chamber of the oven at the first working temperature to an oven chamber at a second working temperature. The second working temperature is described below. [068] Before slow cooling 108, in a non-limiting mode, the alloy can be heat treated 110 at a heat treatment temperature in the first temperature range. In a specific non-limiting heat treatment modality 110, the heat treatment temperature range covers a temperature range of 1600 ° F to a temperature that is 30 ° F less than a beta transus temperature of the alloy. In a non-limiting embodiment, heat treatment 110 comprises heating to the heat treatment temperature and maintaining the workpiece at the heat treatment temperature. In a non-limiting heat treatment mode 110, the workpiece is maintained at the heat treatment temperature for a heat treatment time of 1 hour to 48 hours. Heat treatment is believed to help complete the globularization of primary alpha phase particles. In a non-limiting embodiment, after slow cooling 108 or heat treatment 110 the microstructure of an alpha-beta titanium alloy comprises at least 60 percent by volume of the alpha phase fraction, where the alpha phase comprises or consists of phase particles alpha globular primaries. [069] It is recognized that a microstructure of an alpha-beta titanium alloy Petition 870190084256, of 08/28/2019, p. 22/77 19/35 including a microstructure comprising globular primary alpha phase particles may be formed by a process other than that described above. In such a case, a non-limiting embodiment of the present disclosure comprises providing an alpha-beta titanium alloy comprising a microstructure which comprises or consists of globular primary alpha phase particles. [070] In non-limiting modes, after working 106 the alloy at the first working temperature and slowly cooling 108 the alloy, or after heat treatment 110 and slow cooling 108 of the alloy, the alloy is worked 114 one or more times at a time. second working temperature within a second temperature range and can be forged at one or more temperatures in the second temperature range. In a non-limiting mode, when the alloy is worked more than once in the second temperature range, the alloy is first worked at a lower temperature in the second temperature range and then subsequently worked at a higher temperature in the second temperature range temperature. It is believed that when the workpiece is first worked at a lower temperature in the second temperature range and then subsequently worked at a higher temperature in the second temperature range, the recrystallization is intensified. In a non-limiting mode, when the alloy is worked more than once in the first temperature range, the alloy is first worked at a higher temperature in the first temperature range and then subsequently worked at a lower temperature in the first temperature range temperature. The second working temperature is lower than the first working temperature and the second temperature range is in the alpha-beta phase field of the alphabetical titanium alloy. In a specific non-limiting mode, the second temperature range is 600 ° F to 350 ° F below the beta transus and can be forged at one or more temperatures in the first temperature range. [071] In a non-limiting mode, after working 114 the connection to Petition 870190084256, of 08/28/2019, p. 23/77 20/35 second working temperature, the alloy is cooled from the second working temperature. After work 114 at the second working temperature, the alloy can be cooled at any cooling rate including, but not limited to, cooling rates that are provided by either oven cooling, air cooling, and liquid quenching, such as known to a person skilled in the art. It will be recognized that the cooling may comprise cooling to room temperature or to the next working temperature at which the workpiece will still be worked, such as one of the third working temperature or a progressively lower fourth working temperature, as described below . It will also be recognized that, in a non-limiting mode, if a desired degree of grain refinement is reached after the alloy is worked at the second working temperature, additional work by the alloy is not necessary. [072] In non-limiting modalities, after working 114 the alloy at the second working temperature, the alloy is worked 116 at a third working temperature, or worked one or more times at one or more third working temperatures. In a non-limiting embodiment, a third working temperature can be a final working temperature within a third working temperature range. The third working temperature is lower than the second working temperature and the third temperature range is in the alpha-beta phase field of the alpha-beta titanium alloy. In a specific non-limiting mode, the third temperature range is 1000 ° F to 1400 ° F. In a non-limiting embodiment, after working the alloy at the third working temperature, a desired refined alpha phase grain size is achieved. After working at the third working temperature, the alloy can be cooled at any cooling rate including, but not limited to, cooling rates that are provided by either oven cooling, air cooling and liquid quenching, as known per person skilled in the art. Petition 870190084256, of 08/28/2019, p. 24/77 21/35 [073] Still with reference to FIGS. 1 and 2, while not being bound by any particular theory, it is believed that when working 106 an alpha-beta titanium alloy at a relatively high temperature in the alpha-beta field, and possibly heat treatment 110 followed by slow cooling 108 , the microstructure is transformed from one comprising mainly an alpha phase lamellar microstructure 202 into a globularized alpha phase particle microstructure 204. It will be recognized that certain amounts of beta phase titanium, that is, the cubic phase allotrope of centered body of titanium, may be present between the alpha phase coverslip or between the primary alpha phase particles. The amount of beta-phase titanium present in the alpha-beta titanium alloy after any working and cooling steps is essentially dependent on the concentration of beta-phase stabilizing elements present in a specific alpha-beta titanium alloy, which is well understood by a person skilled in the art. It is noted that the lamellar alpha phase microstructure 202, which is subsequently transformed into the primary globularized alpha particles 204, can be produced by beta heat treatment and tempering 104 of the alloy before working the alloy at the first working and tempering temperature, as described above. [074] The globularized alpha phase microstructure 204 serves as a starting stock to work at the subsequent lowest temperature. The globularized alpha phase microstructure 204 generally has better ductility than a lamellar alpha phase microstructure 202. Although the deformation required to recrystallize and refine globular alpha phase particles may be greater than the deformation necessary to globularize lamellar alpha phase microstructures, the microstructure globular particle alpha phase 204 also exhibits much better ductility, especially when working at low temperatures. In a non-limiting mode in which the work comprises forging, the best ductility is observed even at moderate forging die speeds. In other words, Petition 870190084256, of 08/28/2019, p. 25/77 22/35 gains in forging deformation allowed for better ductility at moderate matrix velocities of the globularized alpha phase microstructure 204 exceed the deformation requirements to refine the alpha phase grain size, for example, low matrix velocities, and may result in better yields and lower press times. [075] Although not yet bound by any particular theory, it is still believed that since the globularized alpha phase particle microstructure 204 has a higher ductility than a lamellar alpha phase microstructure 202, it is possible to refine the alpha phase grain size using lower temperature sequences working in accordance with the present disclosure (steps 114 and 116, for example) to trigger waves of recrystallization and controlled grain growth within the globular alpha phase particles 204,206. In the end, in alpha-beta titanium alloys processed according to non-limiting modalities in this document, the primary alpha phase particles produced in the globularization obtained by the first work 106 and by the cooling stages 108 are not themselves thin or ultrafine, but in instead they comprise or consist of a large number of fine alpha to ultrafine recrystallized grains 208. [076] Still with reference to FIG. 1, a non-limiting mode of refining alpha phase grains according to the present disclosure comprises an optional annealing or reheating 118 after working 114 the alloy at the second working temperature, and before working 116 the alloy at the third working temperature . The optional annealing 118 comprises heating the alloy to an annealing temperature in an annealing temperature range spanning 500 ° F below the beta transus temperature of the alpha-beta titanium alloy to 250 ° F below the beta transus temperature of the alpha- beta for an annealing time of 30 minutes to 12 hours. It will be recognized that shorter times can be applied when choosing higher temperatures and longer annealing times Petition 870190084256, of 08/28/2019, p. 26/77 23/35 longs can be applied when choosing lower temperatures. Annealing is believed to increase recrystallization, albeit at the cost of some grain thickening and that ultimately helps in the refinement of alpha phase grain. [077] In non-limiting modalities, the alloy can be reheated to a working temperature before any alloy working stage. In one embodiment, any of the work steps can comprise multiple work steps such as, for example, multiple stretch forging steps, multiple turning forging steps, any combination of multiple turning forging and multiple stretching and forging forging. radial. In any method for refining alpha phase grain size according to the present disclosure, the alloy can be reheated to an intermediate working temperature of any of the working or forging steps at that working temperature. In a non-limiting mode, reheating to a working temperature comprises heating the alloy to the desired working temperature and keeping the alloy at temperature for 30 minutes to 6 hours. It will be recognized that when the workpiece is taken out of the oven for an extended time, such as 30 minutes or more, for intermediate conditioning, such as cutting, for example, the reheating can be extended for more than 6 hours, such like 12 hours, or, in any case, long for a skilled practitioner to know that the entire workpiece is reheated to the desired working temperature. In a non-limiting mode, reheating to a working temperature comprises heating the alloy to the desired working temperature and keeping the alloy at temperature for 30 minutes to 12 hours. [078] After working 114 at the second working temperature, the alloy is worked 116 at the third working temperature, which can be a final working step, as described above. In a non-limiting embodiment, work 116 at the third temperature comprises radial forging. When the work steps Petition 870190084256, of 08/28/2019, p. 27/77 Previous 24/35 comprise forging in an open-end press, forging in an open-end press gives more deformation to a central region of the workpiece, as disclosed in copending US Order 13 / 792.285, which is incorporated by reference here in its wholeness. Note that radial forging provides better control of final size and gives more deformation to the surface region of an alloy workpiece, so that deformation in the surface region of the forged workpiece can be comparable to deformation in the region center of the forged workpiece. [079] According to another aspect of the present disclosure, a non-limiting embodiment of a method for refining alpha phase grain size in an alpha-beta titanium alloy comprises forging an alpha-beta titanium alloy at a first forging temperature, or forging more than once at one or more forging temperatures within a first forging temperature range. The forging of the alloy at the first forging temperature, or at one or more first forging temperatures, comprises at least one pass from both turning forging and stretching forging. The first forging temperature range comprises a temperature range covering 300 ° F below the beta transus to a temperature 30 ° F below a beta transus temperature of the alloy. After forging the alloy at the first forging temperature and possibly annealing it, the alloy is cooled slowly from the first forging temperature. [080] The alloy is forged once or more than once at a second forging temperature, or at one or more second forging temperatures, within a second forging temperature range. The forging of the alloy at the second forging temperature comprises at least one pass of both turning forging and stretching forging. The second forging temperature range is 600 ° F to 350 ° F below the beta transus. [081] The alloy is forged once or more than once to a third temperatu Petition 870190084256, of 08/28/2019, p. 28/77 25/35 forging range, or at one or more third forging temperatures within a third forging temperature range. In a non-limiting mode, the third forging operation is a final forging operation within a third forging temperature range. In a non-limiting embodiment, the forging of the alloy at the third forging temperature comprises radial forging. The third forging temperature range comprises a temperature range spanning 1000 ° F and 1400 ° F and the third forging temperature is lower than the second forging temperature. [082] In a non-limiting mode, after forging the alloy at the second forging temperature, and before forging the alloy at the third forging temperature, the alloy is forged at one or more progressively lower fourth forging temperatures. The progressively lower one or more fourth forging temperatures are lower than the second forging temperature. Each of the fourth working temperatures is lower than, if any, the immediately previous fourth working temperature. [083] In a non-limiting mode, high alpha-beta high field forging operations, that is, forging at the first forging temperature, result in a range of primary globularized alpha phase particle sizes from 15 pm to 40 pm. The second forging process begins with multiple forging, reheating and annealing operations, such as one to three turns and stretches, between 500 ° F to 350 ° F below the beta transus, followed by multiple forging, reheating and annealing operations, such as as one to three turns and stretches, between 550 ° F to 400 ° F below the beta transus. In a non-limiting mode, the workpiece can be reheated in an intermediate way at any forging stage. In a non-limiting mode, in any reheating step in the second forging process, the alloy can be annealed between 500 ° F and 250 ° F below the beta transus for an annealing time of 30 minutes Petition 870190084256, of 08/28/2019, p. 29/77 26/35 to 12 hours, shorter times being applied when choosing higher temperatures and longer times being applied when choosing lower temperatures, as would be recognized by a skilled practitioner. In a non-limiting embodiment, the alloy can be forged down in size at temperatures between 600 ° F to 450 ° F below the beta transus temperature of the alpha-beta titanium alloy. Forging dies can be used at this point, together with lubricating compounds such as, for example, boron nitride or graphite sheets. In a non-limiting mode, the alloy is forged radially or in a series of 2 to 6 reductions made at 1100 ° F to 1400 ° F, or in multiple series of 2 to 6 reductions and reheats with temperatures starting at no more than 1400 ° F and decreasing for each new reheat to not less than 1000 ° F. [084] In accordance with another aspect of the present disclosure, a non-limiting embodiment of a method for refining alpha phase grain size in an alpha-beta titanium alloy comprises forging an alpha-beta titanium alloy comprising a phase particle microstructure. globularized alpha at an initial forging temperature within an initial forging temperature range. The forging of the alloy at the initial forging temperature comprises at least one pass from both the forging and drawing forging. The initial forging temperature range is 500 ° F to 350 ° F below the beta transus temperature of the alpha-beta titanium alloy. [085] The alloy is forged at a final forging temperature within a final forging temperature range. Forging the workpiece at the final forging temperature comprises radial forging. The final forging temperature range is 600 ° F to 450 ° F below the beta transus. The final forging temperature is lower than each of the one or more progressively lower forging temperatures. [086] The following examples are intended to further describe Petition 870190084256, of 08/28/2019, p. 30/77 27/35 certain non-limiting modalities, without restricting the scope of the present invention. Persons skilled in the art will appreciate that variations on the following examples are possible within the scope of the invention which is defined solely by the claims. EXAMPLE 1 [087] A workpiece comprising Ti-6Al-4V alloy and was heated and forged in the first working temperature range according to methods usual to those familiar with the art of forming a substantially globularized primary alpha microstructure. The workpiece was then heated to a temperature of 1800 ° F which is in the first forging temperature range for 18 hours (as per box 110 in Fig. 1). It was then cooled slowly in the oven at -100 ° F per hour or between 1.5 and 2 ° F per minute up to 1200 ° F and then cooled in air to room temperature. Backscattered electron micrographs (BSE) of the microstructure of the forged and slowly cooled alloy are shown in FIGS. 3 and 4. [088] In the BSE micrographs of FIGS. 3 and 4, it is observed that after forging at a relatively high temperature in the alpha-beta phase domain followed by slow cooling, the microstructure comprises primary globularized alpha phase particles interspersed with beta phase. In micrographs, gray shading levels are related to the average atomic number, thereby indicating variables of chemical composition, and also vary locally based on crystal orientation. The light colored areas in the micrographs are beta phase which is rich in vanadium. Due to the relatively higher atomic number of vanadium, the beta phase appears as a lighter shade of gray. The darkest colored areas are globularized alpha phase. FIG. 5 is an electron backscattered diffraction micrograph (EBSD) from the same alloy sample showing the quality of the diffraction pattern. Again, the light-colored areas are beta phase, as they exhibited patterns of Petition 870190084256, of 08/28/2019, p. 31/77 28/35 sharper diffraction in these experiments and the dark colored areas are alpha phase, as they exhibited less clear diffraction patterns. It has been observed that the forging of an alpha-beta titanium alloy at a relatively high temperature in the alpha-beta phase field, followed by slow cooling, results in a microstructure comprising primary globularized alpha phase particles interspersed with beta phase. EXAMPLE 2 [089] Two workpieces in the form of 4 cubes of Ti-6-4 material produced using a method similar to Example 1 were heated to 1300 ° F and forged through two cycles (6 strokes to 3.5 mm) height) of multi-axis forging in a very fast open matrix operated at deformation rates of about 0.1 to 1 / s to achieve a central deformation of at least 3. Fifteen second retentions were made between strokes to allow for some dissipation of adiabatic heating. The workpieces were subsequently annealed at 1450 ° F for almost 1 hour and then moved to a 1300 ° F oven to be soaked for about 20 minutes. The first piece of work was finally cooled in the air. The second workpiece was forged again through two cycles (6 taps up to 3.5 in height) of multi-axis forging in an open die quite fast operated at strain rates of about 0.1 to 1 / s to give a central deformation of at least 3, namely a total deformation of 6. Retentions of fifteen seconds were also made between strokes to allow for some adiabatic heating dissipation. FIGs. 6A and 6B are BSE micrographs of the first and second samples, respectively, after they have been processed. Again, gray shading levels are related to the average atomic number, thereby indicating variations in chemical composition and also variations locally with respect to crystal orientation. In this sample shown in FIGS. 6A and 6B, light-colored regions are beta phase, while the regions Petition 870190084256, of 08/28/2019, p. 32/77 29/35 darker colored particles are globular alpha phase particles. Variation of gray levels within the globularized alpha phase particle reveals changes in crystal orientation, such as the presence of sub-grains and recrystallized grains. [090] FIGS. 7 and 8 are EBSD micrographs, respectively, of the first and second samples of Example 2. The gray levels in this micrograph represent the quality of the EBSD diffraction patterns. In these EBSD micrographs, the light areas are beta phase and the dark areas are alpha phase. Some of these areas appear darker and shaded with substructures: these are the non-crystallized areas, deformed areas within the original or primary alpha particles. They are surrounded by small, deformation-free, recrystallized alpha grains that nuclear and grew on the periphery of these alpha particles. The lighter small grains are recrystallized beta grains interspersed between alpha particles. It is seen in the micrographs of FIGs. 7 and 8 that by forging the globularized material like that of the sample in Example 1, the primary globularized alpha phase particles are beginning to recrystallize into finer alpha phase grains within the original or primary globularized particles. [091] FIG. 9A is an EBSD micrograph of the second sample from Example 2. The gray shading levels in the micrograph represent alpha grain sizes and the gray shading levels of the grain boundaries are indicative of their disorientation. FIG. 9B is a graph of the relative amount of alpha grains in the sample having particular grain sizes and FIG. 9C is a graph of the disorientation distribution of the alpha phase grain limits in the sample. As can be determined from FIG. 9B, a larger number of alpha grains obtained by forging the globularized sample of Example 1 and then annealing at 1450 ° F, then again forging are superfine, that is, 1 to 5 pm in diameter and they are altogether finer than the first sample in example 2, right after annealing at 1450 ° F which allowed some grain growth and intermediate progression, es Petition 870190084256, of 08/28/2019, p. 33/77 30/35 recrystallization tactic. EXAMPLE 3 [092] Two workpieces such as a 4 cube of ATI 425® alloy material produced using a method similar to Example 1 were heated to 1300 ° F and forged through a cycle (3 strokes up to 3.5 in height) ) forging multiple axes in a very fast open matrix operated at strain rates of about 0.1 to 1 / s to achieve a central strain of at least 1.5. Fifteen-second holds were made between strokes to allow for some adiabatic heating dissipation. The workpieces were subsequently annealed at 1400 ° F for 1 hour and then moved to a 1300 ° F oven to be soaked for 30 minutes. The first piece of work was finally cooled in the air. The second workpiece was forged again through a cycle (3 taps up to 3.5 in height) of forging multiple axes in an open matrix quite fast operated at deformation rates of about 0.1 to 1 / s to give a central deformation of at least 1.5, namely, a total deformation of 3. Retentions of fifteen seconds were also made between strokes to allow some dissipation of adiabatic heating. [093] FIGS. 10A and 10B are BSE micrographs, respectively, of the first and second forged and annealed samples. Again, gray shading levels are related to the average atomic number, thereby indicating variations in chemical composition and also variations locally with respect to crystal orientation. In this sample shown in FIGS. 10A and FIG. 10B, light colored regions are beta phase, while the darkest colored regions are globular alpha phase particles. Variation of gray levels within the globularized alpha phase particle reveals changes in crystal orientation, such as the presence of recrystallized grains and grains. [094] FIGS. 11 and 12 are EBSD micrographs, respectively, of the first Petition 870190084256, of 08/28/2019, p. 34/77 31/35 and the second sample of Example 3. The gray levels in this micrograph represent the quality of the EBSD diffraction patterns. In these EBSD micrographs, the light areas are beta phase and the dark areas are alpha phase. Some of these areas appear darker and shaded with substructures: these are the non-crystallized areas, deformed areas within the original or primary alpha particles. They are surrounded by small, deformation-free, recrystallized alpha grains that nuclear and grew on the periphery of these alpha particles. The lighter small grains are recrystallized beta grains interspersed between alpha particles. It is seen in the micrographs of FIGs. 11 and 12 that when forging the globularized material like that of the sample of Example 1, the primary globularized alpha phase particles are beginning to recrystallize into finer alpha phase grains within the original or primary globularized particles. [095] FIG. 13A is an EBSD micrograph of the first sample in Example 3. The gray shading levels in the micrograph represent alpha grain sizes and the gray shading levels of the grain boundaries are indicative of their disorientation. FIG. 13B is a graph of the relative amount of alpha grains in the sample having particular grain sizes and FIG. 13C is a graph of the disorientation distribution of the alpha phase grain limits in the sample. As can be determined from FIG. 13B, the alpha grains obtained by forging the globularized sample of Example 1 and then annealing at 1400 ° F recrystallized and grown again during annealing, resulting in a wide alpha grain size distribution in which most grains are fine, that is, 5 to 15 pm in diameter. [096] Fig. 14A is an EBSD micrograph of the second sample from Example 3. The gray shading levels in the micrograph represent alpha grain sizes and the gray shading levels of the grain boundaries are indicative of their disorientation. FIG. 14B is a graph of the relative amount of alpha grains in the sample having particular grain sizes and FIG. 14C is a graph of the distribution Petition 870190084256, of 08/28/2019, p. 35/77 32/35 disorientation of alpha phase grain limits in the sample. As can be determined from FIG. 14B, a number of the alpha grains obtained by forging the globularized sample of Example 1 and then annealing at 1400 ° F, then again forging is superfine, ie, that is, 1 to 5 pm in diameter. The thickest unrecrystallized grains are remnants of the grains that grew the most during annealing. This shows that the annealing time and temperature must be chosen carefully to be totally beneficial, that is, to allow an increase in the recrystallized fraction without excessive grain growth. EXAMPLE 4 [097] A 10-diameter workpiece of Ti-6-4 material produced using a method similar to that of Example 1 was additionally forged through four turns and stretches performed at temperatures between 1450 ° F and 1300 ° F decomposed as a first in a series of stretches and reheats at 1450 ° F to 7.5 in diameter, then second, two sequences of turns and similar stretches made from a turn of about 20% at 1450 ° F and stretches back to 7 , 5 in diameter at 1300 ° F, then third, stretches up to 5.5 in diameter at 1300 ° F, then fourth, two sequences of turns and similar stretches made of a turn of about 20% at 1400 ° F and stretches back to 5.0 in diameter at 1300 ° F and finally stretches up to 4 to 1300 ° F. [098] FIG. 15 is a BSE micrograph of the resulting alloy. Again, gray shading levels are related to the average atomic number, thereby indicating variations in chemical composition and also variations locally with respect to crystal orientation. In the sample, light colored regions are beta phase and darker colored regions are globular alpha phase particles. Variation of gray shading levels within the globularized alpha phase particles reveals changes in crystal orientation, such as the presence of sub-grains and recrystallized grains. Petition 870190084256, of 08/28/2019, p. 36/77 33/35 [099] FIG. 16 is an EBSD micrograph of the sample from Example 4. The gray levels in this micrograph represent the quality of the EBSD diffraction patterns. It is seen in the micrograph of FIG. 16 that when forging the globularized sample of Example 1, the primary globularized alpha phase particles recrystallize into finer alpha phase grains within the original or primary globularized particles. The recrystallization transformation is almost complete, as only a few non-recrystallized areas can be seen. [0100] FIG. 17A is an EBSD micrograph of the sample from Example 4. The gray shading levels in this micrograph represent grain sizes and the gray shading levels of the grain boundaries are indicative of their disorientation. FIG. 17B is a graph showing the relative concentration of grains with particular grain sizes and FIG. 17C is a graph of the disorientation distribution of the alpha phase grain limits. It can be determined from FIG. 17B that after forging the globularized sample of Example 1 and performing additional forging through 4 turns and stretches at a temperature between 1450 ° F and 1300 ° F, the alpha phase grains are superfine (1 pm to 5 pm in diameter). EXAMPLE 5 [0101] A full-scale Ti-6-4 billet was hardened after some forging operations carried out in the beta field. This workpiece was also forged through a total of 5 turns and stretches in the following approach: The first two turns and stretches were carried out in the first temperature range to start the lamella breaking and globularization process, maintaining its size in the about 22 to about 32 and a length or height range of about 40 to 75. It was then annealed at 1750 ° F for 6 hours and cooled in the oven to 1400 ° F at -100 ° F per hour, in order to obtain a microstructure similar to that of the sample in Example 1. It was then forged through 2 turns and stretches with reheating between 1400 ° F and 1350 ° F, maintaining its Petition 870190084256, of 08/28/2019, p. 37/77 34/35 size in the range of about 22 to about 32 with a length or height of about 40 to 75. Then, other turns and stretches were performed with reheating between 1300 ° F and 1400 ° F, in a size range of about 20 to about 30 and a length or height range of about 40 to 70. Subsequent stretches to about 14 in diameter were performed with reheats between 1300 ° F and 1400 ° F. This included some V-die forging steps. Finally, the part was forged radially over a temperature range of 1300 ° F to 1400 ° F to about 10 in diameter. Throughout this process, intermediate conditioning and end cutting steps were introduced to prevent crack propagation. [0102] FIG. 18 is an EBSD micrograph of the resulting sample. The levels of gray shading in this micrograph represent the quality of EBSD diffraction patterns. It is seen in the micrograph of FIG. 18 that when forging first in the high alpha-beta field, cool slowly and then in the low alpha-beta field, the primary globularized alpha phase particles begin to recrystallize into finer alpha phase grains within the original or primary globularized particles. It is noted that only three turns and stretches were performed in the low alpha-beta field as opposed to Example 3, where four of such turns and stretches had been performed in this temperature range. In the present case, this resulted in a lower recrystallization fraction. An additional sequence of turning and stretching would have caused the microstructure to be very similar to that of Example 3. In addition, an intermediate annealing during the low alpha-beta series of turns and stretches (box 118 of Fig. 1) would have improved the recrystallized fraction . [0103] FIG. 19A is an EBSD micrograph of the sample from Example 5. The gray shading levels in this micrograph represent grain sizes and the gray shading levels of the grain boundaries are indicative of their disorientation. FIG. 19B is a graph of the relative grain concentration with ta Petition 870190084256, of 08/28/2019, p. 38/77 35/35 particular grain growers and FIG. 19C is a graph of the alpha phase grain orientation. It can be determined from FIG. 19B that after forging the globularized sample of Example 1, with additional forging through 5 turns and stretches and an annealing carried out at 1750 ° F to 1300 ° F, the alpha phase grains are considered to be fine (5 pm to 15 pm) at superfines (from 1 pm to 5 pm in diameter). [0104] It will be understood that the present description illustrates those aspects of the invention relevant to a clear understanding of the invention. Certain aspects that would be evident to those skilled in the art and, therefore, would not facilitate a better understanding of the invention have not been presented in order to simplify the present description. Although only a limited number of embodiments of the present invention are necessarily described herein, one skilled in the art, in considering the foregoing description, recognizes that many modifications and variations of the invention can be employed. All such variations and modifications of the present invention are intended to be covered by the foregoing description and the following claims.
权利要求:
Claims (8) [1] 1. Method for refining alpha phase grain size in an alpha-beta titanium alloy workpiece, the method FEATURED by the fact that it comprises: working an alpha-beta titanium alloy workpiece at a first working temperature within a first temperature range, where the first temperature range is in the alpha-beta field of the alpha titanium alloy alphabet, and where the first temperature range is 300 ° F below the beta transus temperature of the alpha-beta titanium alloy to a temperature 30 ° F below the beta transus temperature of the alpha-beta titanium alloy; slowly cooling the alpha-beta titanium alloy from the first working temperature, where upon completion of work at the first working temperature and slow cooling from the first working temperature, the alphabetical titanium alloy comprises an alpha phase particle microstructure primary globularized and, in which the slow cooling comprises cooling the workpiece at a cooling rate of no more than 5 ° F per minute; working the alpha-beta titanium alloy at a second working temperature within a second temperature range, where the second working temperature is lower than the first working temperature and, where the second temperature range is in the field of alpha-beta phase of the alpha-beta titanium alloy, where the second temperature range is 600 ° F below the beta transus temperature of the alpha-beta titanium alloy to a temperature 350 ° F below the beta transus temperature of the alloy alpha-beta titanium; and working the alpha-beta titanium alloy at a third working temperature in a third temperature range, where the third working temperature is lower than the second working temperature, where the third temperature range is in the field of alpha-beta phase of the alpha-beta titanium alloy, Petition 870190084256, of 08/28/2019, p. 40/77 [2] 2. Method, according to claim 1, CHARACTERIZED by the fact that it also comprises, before slowly cooling the titanium alloy alpha-beta from the first working temperature: heat treating the alpha-beta titanium alloy at a heat treatment temperature, in a heat treatment temperature range that is 300 ° F below a beta transus temperature of the alpha-beta titanium alloy to a temperature 30 ° F below beta transus temperature of the alpha-beta titanium alloy; and maintaining the alpha-beta titanium alloy at the heat treatment temperature. 2/8 third temperature range is 1000 ° F to 1400 ° F and where, after working at the third working temperature, the alpha-beta titanium alloy comprises a desired refined alpha phase grain size selected from among a grain fine, superfine grain and an ultrafine grain; where the alpha-beta titanium alloy is selected from Ti-6Al-4V alloy (UNS R56400), Ti-6Al-4V ELI alloy (UNS R56401), a Ti-6Al-2Sn-4Zr-2Mo alloy (UNS R54620) , a Ti-6Al-2Sn-4Zr-6Mo alloy (UNS R56260) and a Ti-4Al-2.5V-1.5Fe alloy (UNS 54250). [3] 3/8 3. Method, according to claim 2, CHARACTERIZED by the fact that maintaining the alpha-beta titanium alloy at the heat treatment temperature comprises maintaining the alpha-beta titanium alloy at the heat treatment temperature for 1 hour to 48 hours . [4] 4/8 working temperature; wherein the beta heat treatment temperature is within a temperature range of a beta transus temperature of the alpha-beta titanium alloy at a temperature 300 ° F higher than the beta transus temperature of the alpha-beta titanium alloy; and tempering the alpha-beta titanium alloy. 11. Method according to claim 10, CHARACTERIZED by the fact that the beta heat treatment of the alpha-beta titanium alloy comprises working the alpha-beta titanium alloy at the beta heat treatment temperature. 12. Method according to claim 11, CHARACTERIZED by the fact that working the alpha-beta titanium alloy at the beta heat treatment temperature comprises one or more laminated forging, stamping, rough lamination, open die forging, forging in printing die, press forging, automatic hot forging, radial forging, turning forging, stretch forging and multiaxial forging. 13. Method for refining alpha phase grain size in an alpha-beta titanium alloy workpiece, the method FEATURED by the fact that it comprises: forging an alpha-beta titanium alloy at a first forging temperature within a first forging temperature range, where forging the alpha-beta titanium alloy at the first forging temperature comprises at least one pass from both turning forging and stretch forging, and wherein the first forging temperature range spans 300 ° F below the beta transus to a temperature 30 ° F below a beta transus temperature of the alpha-beta titanium alloy; slowly cool the alpha-beta titanium alloy from the first temperature Petition 870190084256, of 08/28/2019, p. 43/77 4. Method according to claim 1, CHARACTERIZED by the fact that it further comprises, after working the alpha-beta titanium alloy at a second working temperature, the annealing of the alpha-beta titanium alloy comprising heating the titanium alloy alpha-beta at a temperature in an annealing temperature range of 500 ° F below a beta transus temperature of the alpha-beta titanium alloy at 250 ° F below the beta transus temperature of the alpha-beta titanium alloy for 30 minutes at 12 hours. Petition 870190084256, of 08/28/2019, p. 41/77 [5] 5/8 forging, where slow cooling comprises cooling the workpiece at a cooling rate of no more than 5 ° F per minute; forging the alpha-beta titanium alloy at a second forging temperature within a second forging temperature range, where forging the alpha-beta titanium alloy at the second forging temperature comprises at least one pass from both turning forging and drawing forging, wherein the second forging temperature range comprises a temperature range ranging from 600 ° F to 350 ° F below the beta transus, and where the second forging temperature is lower than the first forging temperature; and forging the alpha-beta titanium alloy at a third forging temperature within a third forging temperature range, wherein forging the alpha-beta titanium alloy at the third forging temperature comprises radial forging, where the third band forging temperature is 1000 ° F to 1400 ° F, and the third forging temperature is lower than the second forging temperature. 14. Method according to claim 13, CHARACTERIZED by the fact that the alpha-beta titanium alloy is one of Ti-6Al-4V alloy (UNS R56400), a Ti6Al-4V ELI alloy (UNS R56401), an alloy Ti-6Al-2Sn-4Zr-2Mo (UNS R54620), a Ti6Al-2Sn-4Zr-6Mo alloy (UNS R56260) and a Ti-4Al-2.5V-1.5Fe alloy (UNS 54250). 15. Method according to claim 13, CHARACTERIZED by the fact that the slow cooling comprises cooling the alpha-beta titanium alloy at a cooling rate of no more than 5 ° F per minute. 16. Method, according to claim 13, CHARACTERIZED by the fact Petition 870190084256, of 08/28/2019, p. 44/77 5. Method, according to claim 1, CHARACTERIZED by the fact that at least one of working the alpha-beta titanium alloy at the first temperature, working the alpha-beta titanium alloy at the second temperature and working the alpha titanium alloy -beta at the third temperature comprises at least one step of forging in an open die press. [6] 6/8 which further comprises, after the step of slowly cooling the alphabetical titanium alloy from the first forging temperature, heat treatment of the alpha-beta titanium alloy to a heat treatment temperature in the first forging temperature range and keep the alpha-beta titanium alloy at the heat treatment temperature. 17. Method according to claim 16, CHARACTERIZED by the fact that maintaining the alpha-beta titanium alloy at the heat treatment temperature comprises maintaining the alpha-beta titanium alloy at the heat treatment temperature for a period of heat treatment in a time range 1 hour to 48 hours. 18. Method, according to claim 13, CHARACTERIZED by the fact that it further comprises annealing the alpha-beta titanium alloy after forging at the second forging temperature. 19. Method according to claim 18, CHARACTERIZED by the fact that the annealing comprises heating the alpha-beta titanium alloy to an annealing temperature in an annealing temperature range ranging from 500 ° F to 250 ° F below the beta transus and for 30 minutes to 12 hours. 20. Method according to claim 13, CHARACTERIZED by the fact that it further comprises reheating the alpha-beta titanium alloy in an intermediate way to any one of at least one or more press forging steps. 21. Method according to claim 20, CHARACTERIZED by the fact that reheating comprises heating the alpha-beta titanium alloy back to a previous working temperature and maintaining the alpha-beta titanium alloy at the previous working temperature for a reheat time in a range ranging from 30 minutes to 6 hours. 22. Method according to claim 13, CHARACTERIZED by the fact that the radial forging comprises a series of at least two and no more Petition 870190084256, of 08/28/2019, p. 45/77 6. Method, according to claim 1, CHARACTERIZED by the fact that at least one of working the alpha-beta titanium alloy at the first temperature, working the alpha-beta titanium alloy at the second temperature and working the alpha titanium alloy -beta at the third temperature comprises a plurality of forging steps in an open die press, the method further comprising reheating the alpha-beta titanium alloy in an intermediate way to two successive press forging steps. [7] 7/8 than six reductions, in which the radial forging temperature range is 1100 ° F to 1400 ° F. 23. Method according to claim 13, CHARACTERIZED by the fact that the radial forging comprises a multiple series of at least two and no more than six reductions in radial forging temperatures to no more than 1400 ° F and decreasing to no less than 1000 ° F, with a reheat step before each reduction. 24. Method, according to claim 13, CHARACTERIZED by the fact that it further comprises: before forging the titanium alloy at the first forging temperature, heat the alpha-beta titanium alloy in beta to a beta heat treatment temperature, where the beta heat treatment temperature is a beta transus temperature of the alloy alpha-beta titanium at a temperature 300 ° F higher than the beta transus temperature of the alpha-beta titanium alloy; and tempering the alpha-beta titanium alloy. 25. Method according to claim 24, CHARACTERIZED by the fact that the beta heat treatment of the alpha-beta titanium alloy further comprises working the alpha-beta titanium alloy at the beta heat treatment temperature. 26. Method according to claim 25, CHARACTERIZED by the fact that working the alpha-beta titanium alloy at beta heat treatment temperature comprises one or more laminated forging, stamping, rough lamination, open die forging, forging in printing die, press forging, automatic hot forging, radial forging, turning forging, stretch forging and multiaxial forging. 27. Method according to claim 1, CHARACTERIZED by the fact that the alpha-beta titanium alloy comprises a particle microstructure of Petition 870190084256, of 08/28/2019, p. 46/77 7. Method according to claim 6, CHARACTERIZED by the fact that the reheating of the alpha-beta titanium alloy comprises heating the alpha-beta titanium alloy to the first, second or third working temperature and maintaining the titanium alloy alpha-beta at the respective first, second or third working temperature for 30 minutes to 12 hours. 8. Method according to claim 5, CHARACTERIZED by the fact that the at least one step of forging in an open die press comprises at least one of turning forging and stretching forging. 9. Method according to claim 5, CHARACTERIZED by the fact that working the alpha-beta titanium alloy at the third working temperature comprises radial forging of the alpha-beta titanium alloy. 10. Method, according to claim 1, CHARACTERIZED by the fact that it further comprises: beta heat treatment of the alpha-beta titanium alloy at a beta heat treatment temperature before working the alpha-beta titanium alloy at the first Petition 870190084256, of 08/28/2019, p. 42/77 [8] 8/8 alpha globularized phase and, where working the workpiece at the first temperature comprises at least one pass of both turning forging and stretching forging, where the first temperature is 500 ° F to 350 ° F below temperature beta transus; and in which the alpha-beta titanium alloy is worked at a third working temperature in a third temperature range, in which the alpha-beta titanium alloy in the third temperature range comprises radial forging, in which the third temperature is 1000 ° F to 1400 ° F and, where the third working temperature is lower than the first and second working temperatures.
类似技术:
公开号 | 公开日 | 专利标题 BR112015015681B1|2020-02-11|METHOD FOR REFINING ALPHA-BETA GRAIN SIZE IN AN ALPHA-BETA TITANIUM ALLOY WORK PIECE JP6386599B2|2018-09-05|Alpha / beta titanium alloy processing US9624567B2|2017-04-18|Methods for processing titanium alloys JP6734890B2|2020-08-05|Method for treating titanium alloy CA2810388C|2018-09-18|Processing routes for titanium and titanium alloys JP2016517471A5|2017-03-30| CN103045974B|2015-03-04|Hot working method for improving strength of wrought aluminium alloy and keeping plasticity of wrought aluminium alloy
同族专利:
公开号 | 公开日 CA2892936C|2021-08-10| PT2971200T|2018-06-26| SG11201506118TA|2015-10-29| MX2015006543A|2015-07-23| US20170321313A1|2017-11-09| RU2015121129A3|2018-03-01| EP2971200B1|2018-04-11| KR20150129644A|2015-11-20| AU2014238051B2|2017-12-07| ES2674357T3|2018-06-29| JP6467402B2|2019-02-13| RU2675886C2|2018-12-25| CN105026587B|2018-05-04| US9777361B2|2017-10-03| CA2892936A1|2014-09-25| AU2014238051A1|2015-06-11| US10370751B2|2019-08-06| PL2971200T3|2018-11-30| HUE038607T2|2018-10-29| WO2014149518A1|2014-09-25| JP2016517471A|2016-06-16| IL239028A|2019-12-31| MX366990B|2019-08-02| IL239028D0|2015-07-30| KR102344014B1|2021-12-28| SG10201707621UA|2017-11-29| BR112015015681A2|2017-07-11| US20140261922A1|2014-09-18| CN105026587A|2015-11-04| NZ708494A|2020-07-31| EP2971200A1|2016-01-20| DK2971200T3|2018-06-18| RU2015121129A|2017-04-24| UA119844C2|2019-08-27| TR201808937T4|2018-07-23|
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2017-10-03| B25D| Requested change of name of applicant approved|Owner name: ATI PROPERTIES LLC (US) | 2018-11-13| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]| 2019-06-04| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]| 2019-12-24| B09A| Decision: intention to grant [chapter 9.1 patent gazette]| 2020-02-11| 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 28/02/2014, OBSERVADAS AS CONDICOES LEGAIS. |
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申请号 | 申请日 | 专利标题 US13/844,196|2013-03-15| US13/844,196|US9777361B2|2013-03-15|2013-03-15|Thermomechanical processing of alpha-beta titanium alloys| PCT/US2014/019252|WO2014149518A1|2013-03-15|2014-02-28|Thermomechanical processing of alpha-beta titanium alloys| 相关专利
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