WO2022157842A1 - チタン板 - Google Patents

チタン板 Download PDF

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Publication number
WO2022157842A1
WO2022157842A1 PCT/JP2021/001764 JP2021001764W WO2022157842A1 WO 2022157842 A1 WO2022157842 A1 WO 2022157842A1 JP 2021001764 W JP2021001764 W JP 2021001764W WO 2022157842 A1 WO2022157842 A1 WO 2022157842A1
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Prior art keywords
titanium plate
phase
less
orientation
maximum value
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PCT/JP2021/001764
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English (en)
French (fr)
Japanese (ja)
Inventor
元気 塚本
知徳 國枝
一浩 ▲高▼橋
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日本製鉄株式会社
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Application filed by 日本製鉄株式会社 filed Critical 日本製鉄株式会社
Priority to CN202180086296.1A priority Critical patent/CN116635562A/zh
Priority to KR1020237020770A priority patent/KR102801567B1/ko
Priority to PCT/JP2021/001764 priority patent/WO2022157842A1/ja
Priority to JP2022576262A priority patent/JP7495645B2/ja
Publication of WO2022157842A1 publication Critical patent/WO2022157842A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon

Definitions

  • the present disclosure relates to a titanium plate, particularly a titanium plate with less processing anisotropy and excellent formability.
  • Titanium plates are used in plate heat exchangers. Since a plate heat exchanger is required to have a high heat exchange efficiency, a titanium plate is processed into a corrugated shape by press molding in order to increase the surface area when applied to the plate heat exchanger. Therefore, titanium plates for heat exchangers are required to have excellent formability in press forming.
  • titanium sheets usually have mechanical properties (strength, elongation) in the longitudinal direction (RD), which is the rolling direction, and mechanical properties (strength, elongation) in the transverse direction (TD), which is perpendicular to the RD in the sheet plane , elongation) are different (have mechanical anisotropy).
  • RD longitudinal direction
  • TD transverse direction
  • titanium sheets are usually produced by cold rolling in only one direction, and the cold rolling forms a texture oriented in a specific direction.
  • the plate thickness direction (direction perpendicular to the plate surface) is hereinafter referred to as ND.
  • an ordinary titanium plate has anisotropy in mechanical properties derived from structural anisotropy both before and after annealing.
  • the texture formed by cold rolling in the manufacturing process of the titanium plate will be described in more detail.
  • the c-axis (axis parallel to the [0001] direction) of ⁇ -grains with an hcp structure (hexagonal crystal) is , and the azimuth inclined by about 35° from ND (the direction perpendicular to the sheet surface) to TD (the sheet width direction) forms a texture with many orientations. Due to such a texture, ordinary titanium plates have working anisotropy, which is the cause of impairing the formability of titanium plates.
  • Patent Documents 1 to 7 As disclosed in Patent Documents 1 to 7, various efforts have been made to improve the formability of titanium plates.
  • Patent Documents 1 and 2 in order to improve strength and formability, there are three types of crystal orientation distribution functions that represent the grain size of the ⁇ -phase crystal grains of the titanium plate and the crystal orientation of the ⁇ -phase crystal grains. It is described that the relationship between the areas of crystal grains having orientations and the relationship between the areas are set to specific ranges.
  • intermediate annealing conditions (implemented in the recrystallization temperature range)
  • final cold rolling conditions (reduction rate of final cold rolling is 20 to 87%)
  • final annealing after cold rolling The conditions (annealing temperature above ⁇ transformation point and below 950° C.) are controlled.
  • the crystal grain size of ⁇ grains is also controlled by the final annealing conditions.
  • Patent Document 3 in order to improve the strength and formability, the grain size of the ⁇ -phase crystal grains of the titanium plate is set to a specific range, and the ⁇ -phase having a specific relationship with the axial orientation of the (0001) plane. It is described that the area ratio of crystal grains is specified.
  • the heating rate of the final annealing (10 ° C./s or more), the holding temperature ( ⁇ -phase of ⁇ -phase The temperature at which the area ratio becomes 50% or less and less than 950° C.), the holding time (300 seconds or less), and the cooling rate (10° C./s or more) are controlled.
  • the grain size of the ⁇ -phase crystal grains of the titanium plate is set to a specific range, and the 0.2% yield strength in the direction where the yield strength is minimum is set to YSR .
  • the ratio YS T /YS R is 1.17 or less, where YS T is the 0.2% proof stress in the direction orthogonal to the direction in which the proof stress is minimized.
  • the final cold rolling reduction after the final intermediate annealing is set to 20 to 87%, and the annealing temperature of the final annealing is set to the ⁇ transformation point (T ⁇ ) or higher and lower than 950°C, so that the crystal orientation of the titanium plate is , which controls the equivalent circle diameter of the ⁇ -phase grains.
  • the aspect ratio of the ⁇ -phase crystal grains of the titanium plate is set to an average value of 2.0 or more and a standard deviation of 0.70 or more, and the equivalent circle diameter is It is described that the average value is 5 ⁇ m or more and 100 ⁇ m or less, and the maximum value is 300 ⁇ m or less.
  • Patent Document 6 describes the Lankford value ( It describes a titanium plate material for press forming, which has an in-plane anisotropy in which the value obtained by dividing the difference between the r values) by the average r is 0.72 or less.
  • Patent Document 7 describes a titanium material with a small anisotropy of 0.2% yield strength obtained by performing cross rolling under predetermined hot rolling conditions.
  • a titanium plate manufactured by a conventional conventional method has a mechanical anisotropy with a texture having a preferential orientation in which the c-axis is tilted from ND to TD by about 35°.
  • various methods shown in the aforementioned Patent Documents 1 to 7 have been proposed as techniques for improving moldability.
  • the titanium plates described in Patent Documents 1 to 3 are not examined for mechanical anisotropy.
  • the titanium plates described in Patent Documents 4 to 7 have been examined for strength anisotropy, they have not been examined for elongation anisotropy.
  • FIG. 11A shows an SS curve (stress-strain curve) of an ⁇ -annealed material obtained by final annealing (annealing temperature 800 ° C.) in the ⁇ temperature range of a titanium plate manufactured by cold rolling. .
  • SS curve stress-strain curve
  • the c-axis is substantially aligned with the ND by asymmetric rolling described in Patent Document 6 or cross rolling described in Patent Document 7.
  • texture ( ⁇ 0, ⁇ 1 , ⁇ 2 are arbitrary) may be able to develop.
  • the anisotropy of the elongation is improved, the c-axis is oriented in the ND direction, so the tensile force is perpendicular to the c-axis regardless of which direction it is pulled, and the yield strength is the lowest.
  • Patent Documents 6 and 7 cannot sufficiently reduce the anisotropy of the titanium plate in actual operation.
  • the present disclosure aims to provide a titanium plate with high elongation and low elongation anisotropy.
  • a titanium plate according to an aspect of the present disclosure has, in mass%, Fe: 0 to 0.500%, O: 0 to 0.400%, N: 0 to 0.050%, C: 0 to 0 .080%, H: 0-0.013%, Al: 0-2.30%, Cu: 0-1.80%, Nb: 0-1.00%, Si: 0-0.50%, Zr : 0 to 0.50%, Cr: 0 to 0.50%, Mo: 0 to 0.50%, and Sn: 0 to 1.50%, and the balance is Ti and impurities.
  • the metal structure contains an ⁇ phase
  • the average crystal grain size of the ⁇ phase is 100.0 ⁇ m or less
  • the maximum value of the crystal orientation distribution function f (g) calculated by texture analysis using the spherical harmonics method of the electron beam backscattering diffraction method with an expansion index of 16 and a Gaussian half width of 5 ° is 14.0 or less.
  • the crystal orientation distribution function f(g) in the orientation group A expressed by the Euler angles, ⁇ 1 : 0 to 30°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60° 1.0 or more
  • the crystal orientation distribution function f (g ) is 1.0 or more
  • the crystal orientation in the orientation group C expressed by the Euler angles, ⁇ 1 : 60 to 90°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°
  • the maximum value of the distribution function f(g) is 1.0 or more.
  • the chemical composition is, in mass%, O: 0.030 to 0.200%, Fe: 0.020 to 0.200%, one or two May contain seeds.
  • the titanium plate according to [1] or [2] above has the chemical composition, in mass%, of Al: 0.10 to 2.30% and Cu: 0.10 to 1.80%. 1 type or 2 types may be included.
  • the chemical composition is, in mass%, Fe: 0.100% or less, Nb: 0.10 to 1.00%, Si: 0.10 to 0 .50%, and Zr: one or more selected from 0.10 to 0.50%.
  • the titanium plate according to [3] or [4] above has the chemical composition, in mass%, of Cr: 0.05 to 0.50%, Mo: 0.05 to 0.50%, and Sn: May contain one or more selected from 0.05 to 1.50%.
  • the average crystal grain size of five crystal grains from the largest ⁇ phase may be 250 ⁇ m or less.
  • the ⁇ -phase may have an average crystal grain size of 2.0 to 100.0 ⁇ m.
  • the ⁇ -phase may have an average crystal grain size of 8.0 to 100.0 ⁇ m.
  • the titanium plate according to any one of [1] to [8] above has a ratio of total elongation in the rolling direction to total elongation in the plate width direction, El RD /El TD , of 0.70 to It may be 1.30.
  • a titanium plate with high elongation hereinafter, total elongation unless otherwise specified
  • This titanium plate is excellent in formability, and is useful for manufacturing titanium products of complicated shapes by press forming.
  • FIG. 4 is a contour diagram of the crystal orientation distribution function ODF in the space of Euler angles for the titanium plate of the present disclosure.
  • FIG. 10 is a contour line representation of the crystal orientation distribution function ODF in a space of Euler angles for a titanium plate of a conventional example ( ⁇ -annealed material).
  • FIG. 10 is a contour line representation of the crystal orientation distribution function ODF in a space of Euler angles for a titanium plate of a conventional example ( ⁇ -annealed material).
  • FIG. 10 is a contour line representation of the crystal orientation distribution function ODF in a space of Euler angles for a titanium plate of a conventional example ( ⁇ -annealed material).
  • FIG. 3 is a diagram for explaining regions of orientation groups A to orientation groups C in a three-dimensional display of Euler angles;
  • the ODF of the area including the position where the ODF becomes the maximum value in each orientation group is displayed by contour lines, (A) is orientation group A, (B) is orientation group B, ( C) contains the points of ODF maxima in orientation group C;
  • the ODF of the area including the position where the ODF is the maximum value in each orientation group is displayed by contour lines, (A) is orientation group A, (B) is orientation group B, and (C) is Contains the point of ODF maxima in orientation group C.
  • FIG. 4 is a diagram showing an SS curve of an annealed titanium plate produced by conventional cold rolling.
  • FIG. 4 is a diagram showing an example of an SS curve of a titanium plate according to the present embodiment;
  • FIG. 3 is a diagram showing the structure (needle-like structure) of a titanium plate subjected to final annealing at a temperature equal to or higher than the ⁇ transformation temperature; It is the figure which showed the manufacturing process of the titanium plate which concerns on this embodiment.
  • FIG. 4 is a diagram for explaining a method of obtaining flow stress from an SS curve;
  • titanium plate according to an embodiment of the present disclosure (titanium plate according to the present embodiment) will be described below.
  • Metal structure ⁇ contains ⁇ phase, average crystal grain size of ⁇ phase is 100.0 ⁇ m or less>
  • the main crystal structure is the ⁇ phase.
  • the crystal structure mainly composed of ⁇ phase means that the ⁇ phase fraction in the entire evaluation surface is 95% or more in terms of area ratio. This fraction is preferably 97% or more, more preferably 99% or more.
  • the residual structure other than the ⁇ -phase includes ⁇ -phase, Ti 2 Cu, TiFe, Ti 3 Al, and silicide. Also, the average crystal grain size of the ⁇ phase is set to 100.0 ⁇ m or less.
  • the average crystal grain size of the ⁇ phase is preferably 90.0 ⁇ m or less, more preferably 80.0 ⁇ m or less.
  • the lower limit of the average crystal grain size of the ⁇ -phase is not limited, but if the average crystal grain size is to be made finer, it is necessary to increase the rolling reduction in cold rolling, and cold rolling tends to develop texture. Therefore, the average crystal grain size of the ⁇ phase may be 2.0 ⁇ m or more, 5.0 ⁇ m or more, or 8.0 ⁇ m or more.
  • the area ratio of ⁇ -phase is obtained by the following method. Since the ⁇ -phase is uniformly distributed, the area ratio of each phase constituting the metallographic structure of the titanium plate may be measured in any cross section of the titanium plate. In the present disclosure, for example, by observing a plane (L cross section) perpendicular to the plate width direction at a position of 1/2 the plate width of the titanium plate (a position of 1/2 the plate width from the end in the width direction: the center of the width) Measure.
  • the L cross section at the position of 1/2 the plate width of the titanium plate is polished and used as an observation surface, and SEM (Scanning Electron Microscopy) / EPMA (Electron Probe Microanalyzer) is used in a 500 ⁇ m ⁇ 500 ⁇ m field of view to 1.0 ⁇ m.
  • the concentration distribution of Fe and Cu is measured at a pitch (step: 1.0 ⁇ m). Since Fe and Cu are concentrated in the ⁇ phase or the Ti 2 Cu portion, the region where the concentration of these elements is 1.7 times or more the average of the entire field of view is defined as the ⁇ phase or the Ti 2 Cu portion, and the entire field of view of this region is calculated as the area ratio of the ⁇ phase or Ti 2 Cu. Also, the area ratio of the ⁇ phase is calculated by subtracting these area ratios from 100%.
  • the average crystal grain size of the ⁇ -phase may be measured at any cross section of the titanium plate. For example, it is measured by observing a plane perpendicular to the plate width direction (L section) at a position of 1/2 of the plate width of the titanium plate. Specifically, the L cross section at the position of 1/2 the plate width of the titanium plate is polished and used as an observation surface, and the EBSD pattern is measured with a SEM at a pitch of 2.0 ⁇ m in a field of view of the total plate thickness of this surface ⁇ 10 mm.
  • the boundary with a misorientation of 15° or more is recognized as a crystal grain boundary, and the region surrounded by this crystal grain boundary is defined as a crystal grain.
  • the average crystal grain size is evaluated by arithmetic mean of the average value of equivalent circle diameters (equivalent circle diameters) of the crystal grains.
  • This field of view is preferably set so that approximately 1000 or more crystal grains are present. However, if the average crystal grain size obtained by the above method is 5.0 ⁇ m or less, in order to improve accuracy, the field of view of the total plate thickness ⁇ 1 mm is measured again at a pitch of 0.5 ⁇ m to obtain the average crystal grain size. .
  • ⁇ ⁇ 1 , ⁇ , ⁇ 2 ⁇
  • ⁇ Orientation group A ⁇ 1 : 0 to 30°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°
  • orientation group B ⁇ 1 : 30 to 60°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°
  • the maximum value of the crystal orientation distribution function f(g) in the orientation group C is 1.
  • the notation method using Euler angles is used in order to express the crystal orientation in the texture in three dimensions.
  • the notation method using Euler angles (Bunge notation method)
  • a crystal coordinate system a coordinate system based on the direction of the hcp structure in the case of the ⁇ phase of titanium
  • the Z-axis is the [0001] direction.
  • the X-axis may be taken in the [10-10] direction (the normal direction of the cylindrical surface) or in the [1-210] direction.
  • the X-axis is the [1-210] direction.
  • the Y-axis is the [10-10] direction (the normal direction of the cylindrical surface).
  • the result obtained is the same regardless of which orientation is adopted as the X-axis.
  • the notation method using Euler angles as shown in FIG. match) is considered first. From there, the crystal coordinate system is rotated by ⁇ 1 ° around the Z axis (X′, Y′, Z) as shown in FIG. 1(B), and then by ⁇ 1 ° as shown in FIG.
  • FIG. 2 shows a notation diagram in which the preferred orientation of the conventional material is three-dimensionally represented by Euler angles.
  • the crystal orientation distribution of a polycrystal is represented by a function f ( ⁇ 1 , ⁇ , ⁇ 2 ) using the above-mentioned Euler angles ( ⁇ 1 , ⁇ , ⁇ 2 ), and this function is called a crystal orientation distribution function (Orientation Distribution Function (ODF).
  • ODF Orientation Distribution Function
  • the ODF can be expressed as f(g).
  • the value of f(g), which represents the orientation density, is 1 for random orientations (see Non-Patent Document 1).
  • the crystal orientation distribution function can be determined by an electron backscattered diffraction (EBSD) method. Measure and analyze the EBSD pattern by the electron beam backscatter diffraction (EBSD) method while scanning an electron beam on the inspection surface with a scanning electron microscope (SEM), and convert it into an angle with respect to the plate surface by calculation on a computer. to obtain the Euler angles ( ⁇ 1 , ⁇ , ⁇ 2 ) of the crystal orientation at each measurement point. ODF (f( ⁇ 1 , ⁇ , ⁇ 2 )) can be calculated based on the data of the measurement points within the measured field of view.
  • EBSD electron backscattered diffraction
  • the crystal orientation distribution function is obtained by the following method. Since the ⁇ phase is uniformly distributed, the crystal orientation distribution function may be measured in any cross section of the titanium plate. For example, the surface perpendicular to the plate width direction at the position of 1/2 of the plate width of the titanium plate (hereinafter also referred to as "L section") is polished and used as a measurement surface, and 5
  • the EBSD pattern was measured and analyzed by the electron beam backscatter diffraction (EBSD) method while scanning the electron beam with a scanning electron microscope (SEM) at a pitch of .0 ⁇ m (step 5.0 ⁇ m), and by calculation on a computer, By converting the ⁇ -phase crystal of titanium to the angle with respect to the plate surface in FIG.
  • the Euler angle at each measurement point is obtained.
  • OIM Analysis software TM version 8.1.0 manufactured by TSL Solutions is used to calculate the ⁇ -phase ODF.
  • EBSD electron beam backscatter diffraction
  • the maximum value of f(g) of the ⁇ phase, which is the main phase, is 14.0 or less, the structure becomes random and the anisotropy of the mechanical properties of the titanium plate can be reduced. Furthermore, since the c-axes are oriented in various directions, the yield strength can be increased compared to the cross-rolled material.
  • the maximum value of the crystal orientation distribution function f(g) is preferably 12.0 or less, 10.0 or less, and more preferably 9.0 or less.
  • the three -dimensional orientation distribution function f( ⁇ 1 , ⁇ , ⁇ 2 ) are shown in FIG.
  • f(g) at a specific ⁇ 2 is represented by contour lines in the horizontal axis: ⁇ 1 ( 0 to 90°) and the vertical axis: ⁇ (0 to 90°) space. Select up to 55° pitch and put together in one drawing.
  • Concerning the notation of the value of the contour line of f(g) in FIG. Numerical values shown with leading lines in the drawings are rounded to one decimal place for the sake of convenience. These points also apply to FIGS. 4, 5, 7 and 8 below.
  • a cold-rolled titanium plate is finally annealed in the ⁇ temperature range (annealing temperature 800 ° C).
  • the texture of ⁇ 2 is selected from 0 ° to 55° with a pitch of 5° in the same manner as in FIG.
  • the texture of a conventional example ( ⁇ -annealed material) obtained by final annealing (annealing temperature 920°C) of a titanium plate manufactured by cold rolling at a temperature higher than the ⁇ transformation point is shown in the same manner as FIGS.
  • Fig. 5 is a single sheet of drawing in which ⁇ 2 is selected from 0 ° to 55° with a pitch of 5°.
  • the titanium plate according to the present embodiment has, in addition to the above-mentioned provisions, orientation group A ( ⁇ 1 : 0 to 30°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°), orientation group B ( ⁇ 1 : 30-60°, ⁇ : 30-90°, ⁇ 2 : 0-60°), crystal in orientation group C ( ⁇ 1 : 60-90°, ⁇ : 30-90°, ⁇ 2 : 0-60°)
  • orientation group A ⁇ 1 : 0 to 30°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°
  • orientation group B ⁇ 1 : 30-60°, ⁇ : 30-90°, ⁇ 2 : 0-60°
  • crystal in orientation group C ⁇ 1 : 60-90°, ⁇ : 30-90°, ⁇ 2 : 0-60°
  • the maximum value of the orientation distribution function f(g) is set to 1.0 or more.
  • orientation group A, the orientation group B, and the orientation group C when the maximum value of the crystal orientation distribution function f(g) is 1.0 or more, the c-axis is oriented in various directions, and the crystal The orientation becomes random and the anisotropy is reduced.
  • Orientation group A, orientation group B, and orientation group C are each within 30° from TD, 30° to 60°, and 60° to 90° in the plate plane, and the c-axis is 30° or more from ND.
  • a group of tilted orientations is shown. That is, if the maximum value of f(g) in these orientation groups is 1.0 or more, it means that there are more than a certain amount of orientations in which the c-axis is tilted with respect to each direction.
  • FIG. 6 shows the regions of orientation group A, orientation group B, and orientation group C in the space ⁇ 1 , ⁇ , ⁇ 2 ⁇ expressed as a three-dimensional space.
  • FIG. 7 and 8 show the orientation group A for the titanium plate according to the present embodiment and the titanium plate of the conventional example (a texture in which the c-axis is tilted about 35° to TD as a preferential orientation). , orientation group B, and orientation group C, respectively.
  • the point at which f(g) is maximized in the entire ( ⁇ 1 , ⁇ , ⁇ 2 ) region and the point at which f(g) is maximized in orientation group A are the same.
  • FIG. 7 (titanium plate according to this embodiment) and FIG. 8 respectively show three diagrams (A), (B) and (C).
  • ⁇ 2 is fixed at a specific angle, and the distribution of f(g) within the range ( ⁇ 1 : 0 to 90°, ⁇ : 0 to 90°) is illustrated by contour lines.
  • (A) is in the orientation group A
  • (B) is in the orientation group B
  • (C) is in the orientation group C
  • ⁇ 2 at the position where f(g) is maximized is selected.
  • the point at which f(g) has the maximum value in each of orientation group A, orientation group B, and orientation group C is illustrated.
  • FIG. 7 The maximum value of the crystal orientation distribution function f(g) is 1.0 or more at both 15° and the maximum value of f(g) 2.7).
  • FIG. 11B shows an example of the SS curve of the titanium plate according to this embodiment.
  • the titanium plate according to the present embodiment has less anisotropy in elongation (total elongation) and flow stress than the conventional titanium plate (FIG. 11A).
  • the average crystal grain size of the five crystal grains from the largest crystal grain size of the ⁇ phase is 250 ⁇ m or less>
  • the average crystal grain size (equivalent circle diameter) of the five largest crystal grains among the crystal grains contained in the ⁇ phase, which is the main phase is 250 ⁇ m or less. is preferred.
  • the average crystal grain size of the five largest crystal grains is 250 ⁇ m or less, the occurrence of wrinkles due to the presence of coarse grains can be suppressed.
  • the average crystal grain size of the five largest crystal grains is obtained by measuring the crystal grain size in the field of view in the same manner as the measurement of the average crystal grain size of the ⁇ phase described above, and measuring the circles of the five largest crystal grains. It is obtained by averaging the equivalent diameters. (When there are multiple crystal grains with the same grain size, each is counted as one crystal grain.)
  • the titanium plate according to the present embodiment has Fe: 0 to 0.500%, O: 0 to 0.400%, N: 0 to 0.050%, C: 0 to 0.080%, H: 0 to 0 .013%, the balance being Ti and impurities, and further replacing part of the above Ti, further optional elements Al, Cu, Nb, Si, Zr, It may have a chemical composition containing one or more of Cr, Mo, and Sn.
  • Impurities are elements that can be mixed from raw materials or manufacturing processes, and examples thereof include Cl, Na, Mg, Ca, Ta, and V. These elements are permissible as long as they do not interfere with the effects of the titanium plate according to this embodiment. If each impurity is limited to less than 0.1% by mass and the total amount of impurities is limited to 0.5% by mass or less, there is no problem. Moreover, the arbitrary elements described above may be contained as impurities.
  • the chemical composition without any optional elements corresponds to the standard for industrial pure titanium (classes 1 to 4) of Japanese Industrial Standards JIS H4600 (2007) "Titanium and titanium alloys - plates and strips".
  • a pure titanium plate has a low content of alloying elements and is therefore easy to form.
  • the lower limit is 0% because the optional element does not necessarily have to be included.
  • the Fe content is set to 0.500% or less. From the viewpoint of texture control, the Fe content is preferably 0.350% or less, more preferably 0.250% or less, still more preferably 0.200% or less, and still more preferably 0.150%. It is below. Moreover, when the Fe content exceeds 0.100%, there is a concern that the oxidation resistance may decrease. Therefore, when considering oxidation resistance, the Fe content is preferably 0.100% or less.
  • the Fe content may be 0%, but Fe is an element that can be contained in titanium, and if the Fe content is less than 0.001%, the refining cost will increase, so the Fe content should be 0.001%. It is good as above. Moreover, Fe is also an element having the effect of improving the 0.2% proof stress. To obtain this effect, the Fe content is preferably 0.020% or more, more preferably 0.030% or more.
  • the O content is set to 0.400% or less.
  • the O content is preferably 0.350% or less, more preferably 0.250% or less, still more preferably 0.200% or less, and still more preferably 0.150%. % or less.
  • the O content may be 0%, but O is an element that can be contained in titanium, and if the O content is less than 0.001%, the refining cost will increase, so the O content is set to 0.001%. It is good as above. O is also an element that improves the 0.2% proof stress. In order to obtain the above effects, the O content is preferably 0.020% or more. The O content is more preferably 0.030% or more.
  • N 0-0.050% C: 0-0.080% H: 0-0.013% If the N content, C content, and H content are excessive, the elongation will decrease. Therefore, the N content is 0.050% or less, the C content is 0.080% or less, and the H content is 0.013% or less.
  • the C content is preferably less than 0.050%.
  • the content of these elements may be 0%, but in order to make the N content less than 0.0001%, the C content less than 0.0001%, and the H content less than 0.00001%, the smelting There will be a cost. Therefore, the N content may be 0.0001% or more, the C content may be 0.0001% or more, and/or the H content may be 0.00001% or more.
  • the N content may be 0.001% or more, the C content may be 0.001% or more, and/or the H content may be 0.001% or more.
  • Al 0-2.30%
  • Al is an element that improves the 0.2% proof stress, and the higher the Al content, the higher the 0.2% proof stress. Therefore, it may be contained.
  • the Al content is preferably 0.10% or more, more preferably 0.30% or more.
  • the Al content is set to 2.30% or less.
  • the Al content is preferably 2.00% or less, more preferably 1.95%, still more preferably 1.60%.
  • Cu 0-1.80% Cu is an element that improves the 0.2% proof stress without suppressing twinning deformation, and the higher the Cu content, the higher the 0.2% proof stress. Therefore, it may be contained.
  • the Cu content is preferably 0.10% or more, more preferably 0.30% or more.
  • Al 0.10% or more and 2.30% or less
  • Cu 0.10% or more and 1.80% or less.
  • Nb 0-1.00%
  • Nb is an element that improves oxidation resistance, and may be contained when use at high temperatures is expected.
  • the Nb content is preferably 0.10% or more, more preferably 0.15% or more.
  • the Nb content is set to 1.00% or less.
  • the Nb content is preferably 0.85% or less, more preferably 0.80% or less.
  • Si 0-0.50% Si is an element that improves oxidation resistance, and may be contained when use at high temperatures is expected.
  • the Si content is preferably 0.05% or more, more preferably 0.10% or more.
  • the Si content is set to 0.50% or less.
  • the Si content is preferably 0.45% or less, more preferably 0.40% or less.
  • Zr 0-0.50%
  • Zr is an element that improves oxidation resistance, and may be contained when use at high temperatures is expected.
  • the Zr content is preferably 0.10% or more, more preferably 0.15% or more.
  • the Zr content should be 0.50% or less.
  • the Zr content is preferably 0.45% or less, more preferably 0.40% or less.
  • Nb 0.10 to 1.00%
  • Si 0.10 to 0.50%
  • Zr 0.10 to 0.50%
  • Cr 0-0.50% Cr is an element that improves the 0.2% proof stress. Therefore, it may be contained.
  • the Cr content is preferably 0.05% or more, more preferably 0.10% or more.
  • the Cr content is set to 0.50% or less.
  • the Cr content is preferably 0.45% or less, more preferably 0.40% or less.
  • Mo 0-0.50% Mo is an element that improves the 0.2% proof stress. Therefore, it may be contained.
  • the Mo content is preferably 0.05% or more, more preferably 0.10%.
  • the Mo content is set to 0.50% or less.
  • the Mo content is preferably 0.45% or less, more preferably 0.40% or less.
  • Sn 0-1.50% Sn is an element that improves the 0.2% proof stress. Therefore, it may be contained.
  • the Sn content is preferably 0.05% or more, and more preferably 0.10% or more.
  • the Sn content is set to 1.50% or less.
  • the Sn content is preferably 1.30% or less, more preferably 1.10% or less, and even more preferably 1.00% or less.
  • one or more selected from Cr: 0.05 to 0.50%, Mo: 0.05 to 0.50%, and Sn: 0.05 to 1.50% is preferably included.
  • the titanium plate according to the present embodiment is preferably a cold-rolled annealed plate obtained by final annealing a cold-rolled plate.
  • the sheet may be tempered by a tension leveler, a skin pass, or the like after the final annealing.
  • it is preferable that it is a thin plate, and the plate thickness is preferably 1.5 mm or less. More preferably, the thin plate has a thickness of 1.2 mm or less, more preferably 1.0 mm or less, and still more preferably 0.8 mm or less.
  • the titanium plate according to the present embodiment has sufficient elongation and small elongation anisotropy.
  • the elongation (total elongation) when pulled in the RD (rolling direction) and TD (plate width direction) is preferably 20% or more.
  • the ratio of elongation El RD when pulled in RD (rolling direction) to elongation El TD when pulled in TD (plate width direction) (El RD /El TD ) is 0. It is preferably between 0.70 and 1.30.
  • (El RD /El TD ) is more preferably 0.75 or more, still more preferably 0.80 or more, and even more preferably 0.85 or more.
  • (El RD /El TD ) is more preferably 1.25 or less, still more preferably 1.20 or less.
  • the titanium plate according to the present embodiment has the smaller total elongation (at break) in the SS curve when pulled in the RD (rolling direction) and TD (plate width direction) It is preferable that the flow stress ratio is 0.90 to 1.10 at each of the 1/4 position, 1/2 position and 3/4 position of the one strain.
  • the tensile test was performed according to JIS Z2241 (1998) "Metal material tensile test method", using No. 13B test piece specified in JIS Z2201 (1998) “Metal material tensile test piece", RD, TD elongation to measure. Specifically, the gauge length is 50 mm, the strain rate is 0.5%/min up to 2% strain, and 30%/min after that, and the sample is pulled until it breaks. In addition, at each of the 1/4 position, 1/2 position, and 3/4 position of the smaller strain to full elongation (at break) in the SS curve, the flow stress ratio is calculated by the following method. Ask for For example, in a tensile test, when an SS curve as shown in FIG.
  • a titanium raw material manufactured to a predetermined purity is melted by a known method to form a predetermined ingot. Specifically, a vacuum arc melting method (VAR method) or an electron beam melting method (EB method) can be applied.
  • VAR method vacuum arc melting method
  • EB method electron beam melting method
  • Hot rolling process A known method is used. For example, a slab is heated to 700-1000° C. and rolled at a rolling rate of 60-98% to obtain a hot-rolled sheet. At this time, if heated to a temperature higher than the ⁇ transformation point temperature, scale formation becomes severe, so the heating temperature is preferably set to the ⁇ transformation point temperature or less.
  • annealing may be performed as necessary.
  • the temperature is maintained at 600° C. or above and below the ⁇ transformation temperature, and annealing is performed for a certain period of time.
  • the ⁇ transformation point temperature can be obtained from the phase diagram.
  • the phase diagram can be obtained, for example, by the CALPHAD (Computer Coupling of Phase Diagrams and Thermochemistry) method, for which Thermo-Calc, an integrated thermodynamic calculation system of Thermo-Calc Software AB, and a predetermined database ( TI3) can be used.
  • CALPHAD Computer Coupling of Phase Diagrams and Thermochemistry
  • the most characteristic feature is the combination of the conditions of the cold rolling process, the intermediate annealing during the cold rolling process, and the final annealing process. Therefore, among the cold rolling steps, the conditions for the final cold rolling and the conditions for the intermediate annealing immediately before the final cold rolling (hereinafter referred to as "final intermediate annealing") are predetermined conditions.
  • FIG. 13 schematically shows the steps of cold rolling, final intermediate annealing, final cold rolling, and final annealing in the manufacturing process of the titanium plate according to this embodiment.
  • Cold rolling up to final intermediate annealing may be performed under known conditions. Intermediate annealing may be performed between each pass of cold rolling.
  • ⁇ Heating temperature of final intermediate annealing ⁇ transformation point temperature or higher
  • ⁇ phase transforms to ⁇ phase once, and ⁇ phase is cooled
  • the texture is randomized.
  • the anisotropy of the titanium plate can be reduced. If the heating temperature is lower than the ⁇ transformation temperature, the maximum value of the crystal orientation distribution function f(g) will exceed 14.0 in the final product. As a result, the anisotropy of the titanium plate increases. Therefore, the heating temperature of the final intermediate annealing is set to the ⁇ transformation point temperature or higher.
  • the final intermediate annealing temperature is preferably 1000° C. or less.
  • the annealing time is preferably 0 to 10 minutes.
  • the annealing time of 0 min means that cooling is started immediately after reaching the annealing temperature.
  • ⁇ Final cold rolling Rolling rate is 5 to 50% When the rolling reduction in the final cold rolling (the rolling reduction in the cold rolling performed after the final intermediate annealing until the final annealing) is 5 to 50%, in addition to the slip deformation, the twinning deformation is actively activated, and the texture is randomized. If the rolling reduction in the final cold rolling is less than 5%, coarse acicular non-recrystallized grains remain in the subsequent annealing, and the maximum value of the crystal orientation distribution function f(g) exceeds 14.0. . Also, the average crystal grain size exceeds 100.0 ⁇ m.
  • the rolling reduction in the final cold rolling exceeds 50%, twin crystals are not generated so much, and the orientation in a specific direction is strengthened due to slip deformation, and the orientation in a specific direction is observed even after the final annealing.
  • the maximum value of the crystal orientation distribution function f(g) exceeds 14.0.
  • the rolling reduction is set to 5% or more and 50% or less.
  • the rolling reduction is preferably 10% or more and 40% or less. Cold rolling at this rolling rate may be performed in one pass or in multiple passes.
  • the total rolling reduction of cold rolling (without annealing between passes) performed between the final intermediate annealing and the final annealing should be a predetermined rolling reduction. If the crystal orientation is made random before the final cold rolling, it will eventually become more random. Therefore, it is preferable to perform the intermediate annealing in the ⁇ region (temperature equal to or higher than the ⁇ transformation point) to make the orientation uneven.
  • the heating time of the final annealing is not particularly limited, but is preferably 0.5 min or longer from the viewpoint of structural stability for ensuring recrystallization. On the other hand, from the viewpoint of preventing coarsening of crystal grains, the time is preferably 480 min or less.
  • the crystal orientation of the product varies, the texture becomes random, and the anisotropy of strength and elongation decreases.
  • a slab having a thickness of 150 mm, a width of 800 mm, and a length of 5000 mm is formed by blooming or forging. manufactured.
  • these slabs were then heated to 850° C. and hot rolled to prepare 4.0 mm thick titanium plate materials having the composition shown in Tables 1 and 2.
  • Some of the titanium sheet materials were subjected to hot-rolled sheet annealing at 780° C. for 2 minutes.
  • This titanium plate material was subjected to cold rolling, final intermediate annealing, final cold rolling, and final annealing under the conditions shown in Tables 1 and 2 to obtain a titanium plate (cold-rolled annealed plate) having a thickness of 0.5 mm. manufactured.
  • the surface (L section) perpendicular to the plate width direction at the position of 1/2 of the plate width of the titanium plate is used as an observation surface, and the area ratio of ⁇ phase and the average of ⁇ phase are measured by the method described above.
  • the crystal grain size and the average crystal grain size of five crystal grains from the largest ⁇ phase were measured.
  • the surface (L section) perpendicular to the plate width direction at the position was used as the observation surface, and was determined by the method described above.
  • orientation group A expressed by the Euler angles ⁇ 1 : 0 to 30°, ⁇ : 30 to 90°, ⁇ 2 : 0 to 60°, ⁇ 1 : 30 to 60°, ⁇ : 30 to 90 °, ⁇ 2 : 0 to 60°
  • orientation group B expressed by ⁇ 1 : 60 to 90°, ⁇ : 30 to 90°, ⁇ 2 : crystal orientation distribution in orientation group C expressed by 0 to 60°
  • the maximum value of the function f(g) was obtained by the method described above.
  • a No. 13B test piece specified in JIS Z2201 (1998) "Metal material tensile test piece” was sampled and subjected to JIS Z2241 (1998) “Metal material tensile test method”.
  • a tensile test was performed to measure the elongation in RD and TD (El RD , El TD ). Specifically, the distance between the gauge points is 50 mm, the strain rate is 0.5%/min up to 2% strain, and 30%/min after that, and the tension is applied until breakage. The amount of change in the point-to-point distance (50 mm before stretching) was measured to obtain the total elongation. Also, the anisotropy was evaluated by the value of El RD /El TD .
  • a No. 13B test piece specified in JIS Z2201 (1998) “Metal material tensile test piece” was further collected, and according to JIS Z2241 (1998) “Metal material tensile test method” Accordingly, a tensile test was performed in the rolling direction at a strain rate of 30%/min up to a strain amount of 20%.
  • the wrinkles referred to here are rough skin caused by unevenness caused by plastic deformation. Specifically, the surface was observed, and when conspicuous wrinkles were visually confirmed, it was determined to be wrinkled.
  • the total elongation is 20% or more in both RD and TD, and the value of El RD /El TD is sufficiently close to 1.00, and the anisotropy is small.
  • Comparative Example 101 since the temperature of the final intermediate annealing was low, the structure had a strong orientation in which the maximum value of f( g ) exceeded 14.0 . The anisotropy of the plate was large.
  • Comparative Example 102 the rolling reduction in the final cold rolling was low, resulting in a structure in which non-recrystallized grains remained, and a highly oriented structure with a maximum value of f(g) exceeding 14.0.
  • the value of El RD /El TD was also large, and the anisotropy of the titanium plate was large.
  • the average crystal grain size exceeded 100.0 ⁇ m, and wrinkles occurred during deformation.
  • Comparative Example 103 since the rolling reduction in the final cold rolling was high, the structure had a strong orientation in which the maximum value of f( g ) exceeded 14.0 . Anisotropy was large.
  • Comparative Example 104 since the final annealing temperature was low, the structure was such that non-recrystallized grains remained. As a result, the value of El RD /El TD was large and the anisotropy of the titanium plate was large.
  • Comparative Examples 105 and 109 since the temperature of the final annealing was high, an acicular structure with a small degree of circularity including a coarse structure was obtained.
  • Comparative Example 110 the maximum value of f(g) exceeded 14.0, resulting in a strongly oriented structure because the final cold rolling was not performed.
  • the value of El RD /El TD was also large, and the anisotropy of the titanium plate was large.
  • the ⁇ phase was a needle-like structure with a small average circularity, and as a result, wrinkles were generated.
  • Comparative Example 111 did not undergo a final anneal. As a result, the elongation decreased and the value of El RD /El TD increased.
  • Comparative Example 112 the Fe content exceeds the upper limit, and the maximum value of f( g ) exceeds 14.0 , resulting in a strongly oriented structure. Anisotropy was large.
  • Comparative Example 113 the O content exceeded the upper limit, the maximum value of f(g) in the orientation group C was less than 1.0, and the elongation was also reduced.
  • Comparative Example 114 the Al content exceeded the upper limit, and the elongation decreased.
  • Comparative Example 115 the Cu content exceeded the upper limit, and the elongation decreased.
  • this titanium plate is excellent in formability, and is useful for manufacturing titanium products of complicated shapes by press forming.

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