US20250027185A1 - Titanium material - Google Patents

Titanium material Download PDF

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US20250027185A1
US20250027185A1 US18/714,196 US202218714196A US2025027185A1 US 20250027185 A1 US20250027185 A1 US 20250027185A1 US 202218714196 A US202218714196 A US 202218714196A US 2025027185 A1 US2025027185 A1 US 2025027185A1
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titanium
mass
titanium material
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materials
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Norimasa NISHIYAMA
Minori Teramoto
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Assigned to SUMITOMO ELECTRIC INDUSTRIES, LTD. reassignment SUMITOMO ELECTRIC INDUSTRIES, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: NISHIYAMA, Norimasa, TERAMOTO, MINORI
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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
    • 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
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium

Definitions

  • the present disclosure relates to a titanium material.
  • the present application claims priority from Japanese application, Japanese Patent Application No. 2021-194773, filed on Nov. 30, 2021. The entire description contents of the Japanese application are hereby incorporated by reference into the present description.
  • Titanium materials since having a high specific strength, have been used in the fields of aerospace industries, automotive industries and the like. Further, titanium materials, since being excellent in biocompatibility, have been in high demand as metal materials for living bodies, such as dental implants.
  • Patent Literature 1 discloses, as a titanium material having a high strength, a titanium material having ⁇ -phases and ⁇ -phases mixedly present at normal temperature and normal pressure.
  • the titanium material of the present disclosure is a titanium material containing 91% by mass or more of titanium,
  • FIG. 1 is a coordinate system showing the relation between the strength and the ductility of conventional titanium materials and titanium materials of Embodiment 1.
  • FIG. 2 is an example of optical microscopic images of titanium materials of the present Embodiment.
  • FIG. 3 is a temperature-pressure phase diagram of titanium.
  • FIG. 4 is an example of X-ray diffraction patterns obtained by irradiation of a titanium material with X rays.
  • FIG. 5 is a coordinate system showing the relation between the 0.2% yield strength in a tensile test of conventional titanium materials and titanium materials of Embodiment 2 and the content of components other than titanium in these titanium materials.
  • FIG. 6 is a coordinate system showing the relation between the tensile strength of conventional titanium materials and titanium materials of Embodiment 3 and the content of components other than titanium in these titanium materials.
  • FIG. 7 is a schematic cross-sectional view of a high-pressure cell of an ultrahigh-pressure high-temperature generator to be used in manufacture of the titanium material of the present disclosure.
  • the present disclosure has an object to provide a titanium material having a high strength.
  • the titanium material of the present disclosure can have a high strength.
  • the titanium material of the present disclosure is a titanium material containing 91% by mass or more of titanium,
  • the titanium material of the present disclosure can have a high strength. Further, the titanium material of the present disclosure can have a high ductility.
  • the titanium material may contain 98.8% by mass or more of titanium. Thereby, the biocompatibility of the titanium material can be enhanced.
  • the titanium material of the present disclosure is a titanium material containing 91% by mass or more of titanium
  • the titanium material of the present disclosure can have a high strength.
  • the titanium material may contain 98.8% by mass or more of titanium. Thereby, the biocompatibility of the titanium material can be enhanced.
  • the titanium material of the present disclosure is a titanium material containing 91% by mass or more of titanium,
  • the titanium material of the present disclosure can have a high strength.
  • the titanium material may contain 98.8% by mass or more of titanium. Thereby, the biocompatibility of the titanium material can be enhanced.
  • the tensile strength ⁇ B MPa and a fracture elongation ⁇ % of the titanium material may have a relation of the following formula I:
  • the titanium material can have a high strength.
  • the 0.2% yield strength ⁇ 0.2 MPa in a tensile test of the titanium material and the content c % by mass of components other than titanium in the titanium material may have a relation of the following formula II.
  • the titanium material can have a high strength.
  • the average grain diameter of crystal grains constituting the titanium material is 1 ⁇ m or more and 1,000 ⁇ m or less; and the titanium material may contain 50% by mass or more of titanium having a crystal structure of an omega phase. Thereby, the titanium material can have a high strength and a high ductility.
  • the 0.2% yield strength in a compression test of the titanium material may be 570 MPa or more. Thereby the titanium material can have a high strength.
  • the Vickers hardness of the titanium material may be 200 Hv or more. Thereby, the titanium material can have a high hardness.
  • the heat-resistant temperature of the titanium material may be 100° C. or more. Thereby, the titanium material can hold a high strength even at a high temperature of 100° C. or more.
  • the volume of the titanium material may be 0.001 m 3 or more.
  • the titanium material since having a size sufficient as a metal material for living bodies, can be used in various applications such as dental implants and artificial joints.
  • the titanium material contains 98.8% by mass or more of titanium
  • the titanium material can have excellent biocompatibility.
  • a proportion D90/D10 of a cumulative 90% grain diameter D90 from a small diameter side to a cumulative 10% grain diameter D10 from the small diameter side in a cumulative grain size distribution based on volume of crystal grains constituting the titanium material may be 5 or more and 1,000 or less.
  • the strength and the ductility of the titanium material are homogenized and the titanium material can have a higher strength and a higher ductility.
  • the titanium material of the present disclosure will be described hereinafter.
  • the same reference sign represents the same part or a corresponding part.
  • the dimensional relation among length, width, thickness, depth and the like is suitably varied for clarification and simplification of the drawings, and does not always represent an actual dimensional relation.
  • the notation in the form of “A to B” means the upper limit and the lower limit in a range (that is, A or more and B or less), and in the case where A has no description of a unit and only B has a description of a unit, the unit of A and the unit of B are the same.
  • the “strength” has a meaning including at least one of the tensile strength, the 0.2% yield strength in a tensile test and the 0.2% yield strength in a compression test.
  • FIG. 1 is a coordinate system showing the relation between the strength and the ductility of conventional titanium materials and titanium materials of Embodiment 1.
  • the X axis indicates the tensile strength ⁇ B (MPa)
  • the Y axis indicates the fracture elongation ⁇ (%).
  • the tensile strength is one index indicating the strength of materials, and the index indicates that the higher the numerical value, the higher the strength.
  • the fracture elongation is one index indicating the ductility of materials, and the index indicates that the higher the numerical value, the higher the ductility.
  • the conventional titanium materials are shown as JIS-1 to JIS-4, Ti—Fe, Ti-3Al-2.5V and ⁇ -alloy, and the data of the tensile strength and the fracture elongation thereof were prepared by reference to FIG. 1 in Hideki Fujii, Takashi Maeda, “Titanium Alloys Developed by Nippon Steel & Sumitomo Metal Corporation”, Shinnittetsu Sumikin giho, No. 396, 2013, pp. 16-22.
  • the JIS-1 to JIS-4 and ⁇ -alloy mean industrial pure titanium described in JIS H4600:2012 “Titanium and titanium alloys—Sheets, plates and strips”.
  • the JIS-1 means JIS H4600 Class 1
  • the JIS-2 means JIS H4600 Class 2
  • the JIS-3 means JIS H4600 Class 3
  • the JIS-4 means JIS H4600 Class 4.
  • the JIS-1 to JIS-4 have a content of titanium of about 99% by mass or more, and have a crystal structure of an alpha phase.
  • pure titanium having a crystal structure of an alpha phase is referred to also as alpha pure titanium.
  • Ti—Fe, Ti-3Al-2.5V and J-alloy mean titanium alloys.
  • alpha pure titanium having a high titanium content though having a high fracture elongation (hereinafter, referred to also as ductility), is low in tensile strength (referred to also as strength).
  • titanium alloys having other metals added to titanium though having a high tensile strength, are low in fracture elongation.
  • the conventional titanium materials thus have a tradeoff relationship between the strength and the ductility, and there can be provided no titanium materials which can simultaneously satisfy both a high strength and a high ductility.
  • the titanium materials of Embodiment 1 are titanium materials containing 91% by mass or more of titanium,
  • the region having the relation of the above formula I is a region indicated by oblique lines.
  • the region indicated by oblique lines is the region where the fracture elongation is 20% or more, high in ductility, and the tensile strength is 400 MPa or more, high in strength.
  • the titanium materials of Embodiment 1 since satisfying the relation of the above formula I, have a high strength and a high ductility.
  • the conventional titanium materials all have a strength and a ductility in a region indicated by ⁇ B ⁇ 1,600 ⁇ 30 ⁇ , not satisfying the relation of the above formula I.
  • the magnitude of the fracture elongation is high. That is, the titanium materials of Embodiment 1 are, as compared with the conventional titanium materials having the same strengths, excellent in ductility.
  • the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials have a relation of the following formula I-A.
  • the titanium materials satisfying the relation of the above formula I-A can have a higher strength and a higher ductility.
  • the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials have a relation of the following formula I-B.
  • the titanium materials satisfying the relation of the above formula I-B can have a higher strength and a higher ductility.
  • the lower limit of the tensile strength ⁇ B of the titanium materials of Embodiment 1 is 400 MPa or more.
  • the lower limit of the tensile strength ⁇ B of the titanium materials is, from the viewpoint of securing excellent strength, preferably 500 MPa or more, more preferably 600 MPa or more and still more preferably 800 MPa or more.
  • the upper limit of the tensile strength ⁇ B of the titanium materials is not especially limited, and can be, for example, less than 1,550 MPa.
  • the tensile strength ⁇ B of the titanium materials is preferably 400 MPa or more and less than 1,550 MPa, preferably 500 MPa or more and less than 1,550 MPa, more preferably 600 MPa or more and less than 1,550 MPa and still more preferably 800 MPa or more and less than 1,550 MPa.
  • the measurement of the tensile strength ⁇ B of the titanium materials is carried out according to JIS Z2241:2011 “Metallic materials—Tensile testing—Method of test at room temperature”.
  • the test temperature is set at 23° C. ⁇ 5° C.
  • the fracture elongation ⁇ of the titanium materials of Embodiment 1 is 20% or more.
  • the lower limit of the fracture elongation ⁇ of the titanium materials is, from the viewpoint of securing excellent ductility, preferably 25% or more, more preferably 30% or more and still more preferably 35% or more.
  • the upper limit of the fracture elongation ⁇ of the titanium materials can be, for example, 50% or less, or 45% or less.
  • the fracture elongation ⁇ of the titanium materials is preferably 20% or more and 50% or less, preferably 25% or more and 50% or less, preferably 30% or more and 50% or less, preferably 35% or more and 50% or less, preferably 20% or more and 45% or less, preferably 25% or more and 45% or less, or preferably 30% or more and 45% or less.
  • the measurement of the fracture elongation ⁇ of the titanium materials is carried out according to JIS Z2241:2011 “Metallic materials—Tensile testing—Method of test at room temperature”.
  • the test temperature is set at 23° C. ⁇ 5° C.
  • the titanium materials of Embodiment 1 contain 91% by mass or more of titanium.
  • the lower limit of the titanium content of the titanium materials is, from the viewpoint of enhancing biocompatibility, more preferably 95% by mass or more, preferably 98% by mass or more, still more preferably 98.955% by mass or more, still more preferably 99.2% by mass or more, still more preferably 99.495% by mass or more and still more preferably 99.999% by mass or more.
  • the upper limit of the titanium content of the titanium materials is preferably 100% by mass or less. That is, the titanium materials can also be made of 100% by mass of titanium.
  • the titanium content of the titanium materials is preferably 91% by mass or more and 100% by mass or less, preferably 95% by mass or more and 100% by mass or less, preferably 98% by mass or more and 100% by mass or less, preferably 98.955% by mass or more and 100% by mass or less, preferably 99.2% by mass or more and 100% by mass or less, preferably 99.495% by mass or more and 100% by mass or less, or preferably 99.999% by mass or more and 100% by mass or less.
  • the upper limit of the titanium content of the titanium materials of Embodiment 1, in the case of taking inevitable impurities into consideration, can be, for example, 99.9999% by mass or less.
  • the titanium content of the titanium materials is preferably 91% by mass or more and 99.9999% by mass or less, preferably 95% by mass or more and 99.9999% by mass or less, preferably 98% by mass or more and 99.99990% by mass or less, preferably 98.955% by mass or more and 99.9999% by mass or less, preferably 99.2% by mass or more and 99.9999% by mass or less, preferably 99.495% by mass or more and 99.9999% by mass or less, or preferably 99.9990% by mass or more and 99.9999% by mass or less.
  • the titanium materials of Embodiment 1 can be made of 100% by mass of titanium. Then, the titanium materials of Embodiment 1 can contain more than 0% by mass and 9% by mass or less of components other than titanium.
  • the components other than titanium include common transition metal elements such as scandium (Sc), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), yttrium (Y), zirconium (Zr), niobium (Nb), molybdenum (Mo), silver (Ag), hafnium (Hf), tantalum (Ta), tungsten (W), platinum (Pt) and gold (Au), and as inevitable impurities, hydrogen (H), carbon (C), nitrogen (N) and oxygen (O).
  • the upper limit of the content of the components in the titanium materials, including also the inevitable impurities, other than titanium of the titanium materials is 9% by mass or less.
  • the content of the components other than titanium in the titanium materials can be a value obtained by subtracting the content of titanium from 100% by mass of the whole titanium material.
  • the content of the components other than titanium in the titanium materials is measured, in the case where the components are transition metal elements, by ICP spectrometry (radio-frequency inductively coupled plasma atomic emission spectrometry).
  • the content thereof is measured, in the case where the components are elements other than transition metal elements, such as C, N, O and H, by SIMS analysis (secondary-ion mass spectrometry).
  • the titanium content is determined by measuring the content of the components other than titanium by the above method, and, with the titanium material being taken as 100% by mass, subtracting the content of the components other than titanium from the 100% by mass.
  • the titanium materials contain 98.8% by mass or more of titanium; the titanium materials contain at least one impurity element selected from the group consisting of hydrogen, carbon, nitrogen, oxygen and iron; and the total content of titanium and the impurity element in the titanium material is 99.99% by mass or more.
  • the titanium materials contain no components harmful to living bodies, such as vanadium (V) and aluminum (Al), which are contained in the conventional titanium alloys, or even if containing the components, contain the components in a trace amount, the titanium materials can have excellent biocompatibility.
  • the total content of titanium and the impurity element in the titanium material is preferably 99.99% by mass or more and 100% by mass or less, more preferably 99.999% by mass or more and 100% by mass or less and most preferably 100% by mass.
  • the average grain diameter of crystal grains constituting the titanium materials of Embodiment 1 (hereinafter, referred to also as “average grain diameter of the titanium materials”) is preferably 1 ⁇ m or more and 1,000 ⁇ m or less. Thereby, the titanium materials can have excellent strength and ductility.
  • the lower limit of the average grain diameter of the titanium materials is, from the viewpoint of securing excellent strength, preferably 1 ⁇ m or more, preferably 3 ⁇ m or more, preferably 5 ⁇ m or more, preferably 10 ⁇ m or more, or preferably 20 ⁇ m or more.
  • the upper limit of the average grain diameter of the titanium materials is, from the viewpoint of securing excellent strength, preferably 1,000 ⁇ m or less, preferably 500 ⁇ m or less, preferably 200 ⁇ m or less, preferably 100 ⁇ m or less, or preferably 50 ⁇ m or less.
  • the average grain diameter of the titanium materials is preferably 1 ⁇ m or more and 1,000 ⁇ m or less, preferably 3 ⁇ m or more and 500 ⁇ m or less, preferably 5 ⁇ m or more and 200 ⁇ m or less, preferably 10 ⁇ m or more and 100 ⁇ m or less, preferably 10 ⁇ m or more and 50 ⁇ m or less, or preferably 20 ⁇ m or more and 50 ⁇ m or less.
  • the average grain diameter of the titanium materials is measured by an intercept procedure.
  • a specific measuring procedure is as follows. A polished faces of the titanium materials are imaged by using an optical microscope at a magnification of 100 times to obtain optical microscopic images. One example of optical microscopic images of the titanium materials of Embodiment 1 is shown in FIG. 2 .
  • a circle of 50 mm in diameter is drawn on the optical microscopic image; 8 straight lines are radially drawn from the center of the circle to the periphery thereof; and the number of the straight lines crossing grain boundaries in the circle is counted; and an average intercept length is determined by dividing the length of the straight lines by the crossing number of the straight lines; then, a value as an average grain diameter is obtained by multiplying the average intercept length by a conversion factor, 1.128, to a two-dimensional grain diameter.
  • the above measurement is carried out on three positions for one measuring sample, and an average value of average grain diameters at the three positions is taken as the average grain diameter of the titanium materials in the present description.
  • the grain diameter of crystal grains constituting the titanium materials is low in dispersion.
  • the proportion D90/D10 of a cumulative 90% grain diameter D90 from a small diameter side to a cumulative 10% grain diameter D10 from the small diameter side in a cumulative grain size distribution based on volume of crystal grains constituting the titanium is preferably 5 or more and 1,000 or less, or preferably 10 or more and 1,000 or less. It is indicated that the less the value of D90/D10, the less the dispersion in grain diameter of crystal grains.
  • the grain diameter of each crystal grain for calculating the D90/D10 is determined by carrying out image processing using a commercially available image analysis software on an optical microscopic image taken under the same condition as in the above intercept procedure, to measure an equivalent circle diameter of each crystal grain.
  • a measuring visual field of 50 mm ⁇ 50 mm is set in the optical microscopic image, and a volume-base cumulative grain size distribution is formed based on all crystal grains observed in the measuring visual field.
  • the D90/D10 is calculated based on the cumulative grain size distribution.
  • the titanium materials of Embodiment 1 contain 50% by mass or more of titanium having a crystal structure of an omega phase. Thereby, the titanium materials can have excellent strength and ductility.
  • the crystal structure of titanium will be described.
  • alpha titanium having a crystal structure of an alpha phase
  • beta titanium having a crystal structure of a beta phase
  • omega titanium having a crystal structure of an omega phase
  • the alpha titanium is in a stable phase at normal temperature and normal pressure, and has a crystal structure of a hexagonal close-packed (hcp).
  • the beta titanium is a stable phase on the higher temperature side, and has a crystal structure of a body-centered cubic (bcc).
  • the omega titanium is a metastable transition phase formed when the alpha titanium is crystallized from the beta titanium, and has a simple hexagonal crystal structure.
  • omega titanium causes alpha pure titanium to become brittle. Accordingly, it has conventionally been considered that it is preferable to reduce the content of omega titanium in the alpha pure titanium.
  • the present inventors have produced titanium materials containing 50% by volume or more of omega titanium.
  • the titanium materials have been confirmed to have excellent strength and ductility.
  • the lower limit of the content of titanium having a crystal structure of an omega phase of the titanium materials is, from the viewpoint of improving strength and ductility, preferably 50% by mass or more, or, preferably, 55% by mass or more, 60% by mass or more, 65% by mass or more, 70% by mass or more, 75% by mass or more, 80% by mass or more, 85% by mass or more, 90% by mass or more, 95% by mass or more, 98.8% by mass or more, 99% by mass or more, 99.2% by mass or more, 99.5% by mass or more, or 99.999% by mass or more.
  • the upper limit of omega titanium of the titanium materials is preferably 100% by mass or less.
  • the titanium materials can be made of 100% by mass of omega titanium.
  • the omega titanium content of the titanium materials is preferably, 50% by mass or more and 100% by mass or less, 55% by mass or more and 100% by mass or less, 60% by mass or more and 100% by mass or less, 65% by mass or more and 100% by mass or less, 70% by mass or more and 100% by mass or less, 75% by mass or more and 100% by mass or less, 80% by mass or more and 100% by mass or less, 85% by mass or more and 100% by mass or less, 90% by mass or less and 100% by mass or less, 95% by mass or less and 100% by mass or less, 98.8% by mass or more and 100% by mass or less, 99% by mass or more and 100% by mass or less, 99.2% by mass or more and 100% by mass or less, or 99.999% by mass or more and 100% by mass or less.
  • the upper limit of the omega titanium content of the titanium materials of Embodiment 1, in the case of taking inevitable impurities into consideration, can be, for example, 99.9999% by mass or less.
  • the omega titanium content of the titanium materials is preferably, 50% by mass or more and 99.9999% by mass or less, 55% by mass or more and 99.9999% by mass or less, 60% by mass or more and 99.9999% by mass or less, 65% by mass or more and 99.9999% by mass or less, 70% by mass or more and 99.9999% by mass or less, 75% by mass or more and 99.9999% by mass or less, 80% by mass or more and 99.9999% by mass or less, 85% by mass or more and 99.99990% by mass or less, 90% by mass or more and 99.9999% by mass or less, 95% by mass or more and 99.9999% by mass or less, 98.8% by mass or more and 99.9999% by mass or less, 99% by mass or more and 99.9999% by mass or less, 99.2% by mass or more and 99.9999% by mass or less, or
  • the titanium materials of Embodiment 1 are allowed to contain, in addition to omega titanium, either or both of alpha titanium and beta titanium in the range of exhibiting the advantageous effect of the present disclosure.
  • the upper limit of the total content of alpha titanium and beta titanium in the titanium materials is preferably 50% by mass or less, 45% by mass or less, 40% by mass or less, 35% by mass or less, 30% by mass or less, 25% by mass or less, 20% by mass or less, 15% by mass or less, 10% by mass or less, 5% by mass or less, 1.2% by mass or less, or 1% by mass or less.
  • the lower limit of the total content of alpha titanium and beta titanium in the titanium materials is not especially limited, and is preferably, for example, 0% by mass or more, but may be 0.01% by mass or more.
  • the total content of alpha titanium and beta titanium in the titanium materials is preferably, 0% by mass or more and 50% by mass or less, 0% by mass or more and 45% by mass or less, 0% by mass or more and 40% by mass or less, 0% by mass or more and 35% by mass or less, 0% by mass or more and 30% by mass or less, 0% by mass or more and 25% by mass or less, 0% by mass or more and 20% by mass or less, 0% by mass or more and 15% by mass or less, 0% by mass or more and 10% by mass or less, 0% by mass or more and 5% by mass or less, 0% by mass or more and 1.2% by mass or less, 0% by mass or more and 1% by mass or less, 0.01% by mass or more and 50% by mass or less, 0.01% by mass or more and 45% by mass or less, 0.01% by mass or more and 40% by mass or less, 0.01% by mass or more and 35% by mass or less, 0.01% by mass or more and 30% by mass or less, 0.01%
  • omega titanium, alpha titanium and beta titanium in the titanium materials are calculated from intensity ratios of X-ray diffraction peaks characteristic to omega titanium, alpha titanium and beta titanium.
  • the 0.2% yield strength in a compression test of the titanium materials of Embodiment 1 is preferably 570 MPa or more. Thereby, the titanium materials can have a high strength.
  • the lower limit of the 0.2% yield strength in a compression test of the titanium materials is, from the viewpoint of securing excellent strength, preferably 600 MPa or more, more preferably 700 MPa or more and still more preferably 800 MPa or more.
  • the upper limit of the 0.2% yield strength in a compression test of the titanium materials is, since a higher one is better, not especially limited, and can be, for example, 5,000 MPa or less.
  • the 0.2% yield strength in a compression test of the titanium materials is preferably 570 MPa or more and 5,000 MPa or less, preferably 600 MPa or more and 5,000 MPa or less, more preferably 700 MPa or more and 5,000 MPa or less and still more preferably 800 MPa or more and 5,000 MPa or less.
  • the measurement of the 0.2% yield strength in a compression test of the titanium materials is carried out according to JIS R1608:2003 “Testing methods for compressive strength of fine ceramics”.
  • the test temperature is set at 23° C. ⁇ 5° C.
  • the Vickers hardness of the titanium materials of Embodiment 1 is preferably 200 Hv or more. Thereby, the titanium materials can have excellent hardness. The titanium materials hardly generate wear.
  • the lower limit of the Vickers hardness of the titanium materials is, from the viewpoint of securing excellent hardness, preferably 200 Hv or more and more preferably 220 Hv or more.
  • the upper limit of the Vickers hardness of the titanium materials is, since a higher one is better, not especially limited, and can be, for example, 400 Hv or less.
  • the Vickers hardness of the titanium materials is preferably 200 Hv or more and 400 Hv or less and more preferably 220 Hv or more and 400 Hv or less.
  • the measurement of the Vickers hardness of the titanium materials is carried out according to JIS Z2244:2009 “Vickers hardness test—Test method”.
  • the test temperature is set at 23° C. ⁇ 5° C.
  • the heat-resistant temperature of the titanium materials of Embodiment 1 is preferably 100° C. or more. Thereby, the titanium materials can hold excellent strength even at a high temperature of 100° C. or more.
  • the lower limit of the heat-resistant temperature of the titanium materials of Embodiment 1 is, from the viewpoint of securing excellent strength, preferably 100° C. or more, more preferably 120° C. or more and still more preferably 140° C. or more.
  • the upper limit of the heat-resistant temperature of the titanium materials is, since a higher one is better, not especially limited, and can be, for example, 190° C. or less.
  • the heat-resistant temperature of the titanium materials is preferably 100° C. or more and 190° C. or less, more preferably 120° C. or more and 190° C. or less and still more preferably 140° C. or more and 190° C. or less.
  • the heat-resistant temperature of the titanium materials is measured by X-ray diffractometry and comparing an X-ray diffraction pattern at 25° C. with X-ray diffraction patterns at predetermined temperatures.
  • a specific measuring method for the measurement is as follows.
  • a measuring sample is prepared by polishing the surface of the titanium materials.
  • the measuring sample is irradiated with X rays under the following condition by using an X-ray diffraction device to obtain X-ray diffraction patterns.
  • a plurality of temperatures of 25° C. and exceeding 25° C. in the measurement are suitably selected and X-ray diffraction patterns are obtained at respective temperatures.
  • An X-ray diffraction pattern at 25° C. and X-ray diffraction patterns at predetermined temperatures exceeding 25° C. are compared; and in the case where shapes of both of the X-ray diffraction patterns coincide, it is determined that the crystal structure of the measuring sample is held at the predetermined temperatures, and the measuring sample has heat resistance.
  • predetermined temperatures X-ray diffraction patterns at 25° C. and X-ray diffraction patterns at predetermined temperatures exceeding 25° C.
  • the above X-ray diffraction measurement is carried out by raising the temperature condition until X-ray diffraction patterns at the predetermined temperatures exceeding 25° C. assume a shape different from the ray diffraction pattern at 25° C. Among a plurality of X-ray diffraction patterns obtained, an X-ray diffraction pattern at a highest temperature coinciding with the X-ray diffraction pattern at 25° C. is specified. The highest temperature is taken as the heat-resistant temperature of the measuring sample.
  • FIG. 4 One example of X-ray diffraction patterns obtained by irradiating the titanium materials of Embodiment 1 with X rays is shown in FIG. 4 .
  • the X axis indicates 2 ⁇ (deg); and the Y axis indicates the intensity (cps).
  • the X-ray diffraction measurement is carried out at 25° C. and at a temperature condition of from 40° C. to 210° C. at 10° C. intervals on the same titanium material, and in FIG. 4 , X-ray diffraction patterns at respective temperatures thereby obtained are shown.
  • the volume of the titanium materials of Embodiment 1 is preferably 0.001 mm 3 or more.
  • the titanium materials since having a sufficiently large volume as a metal material for living bodies, can be used in various applications such as dental implants and artificial joints.
  • the lower limit of the volume of the titanium materials is preferably 0.001 mm 3 or more, more preferably 10 mm 3 or more and still more preferably 100 mm 3 or more.
  • the upper limit of the volume of the titanium materials is, since a larger volume is better, not especially limited, and is preferably, for example, 100,000 mm 3 or less.
  • the volume of the titanium materials is preferably 0.001 mm 3 or more and 100,000 mm 3 or less, more preferably 10 mm 2 or more and 100,000 mm 3 or less and still more preferably 100 mm 3 or more and 100,000 mm 3 or less.
  • the volume of the titanium materials is measured by the Archimedes method.
  • FIG. 5 is a coordinate system showing the relation between the 0.2% yield strength in a tensile test of conventional titanium materials and titanium materials of Embodiment 2 and the content of components other than titanium in these titanium materials.
  • the X axis indicates the content c (% by mass) of components other than titanium in the titanium materials
  • the Y axis indicates the 0.2% yield strength ⁇ 0.2 (MPa) in a tensile test.
  • the 0.2% yield strength in a tensile test is one index indicating the strength of materials, and the index indicates that the higher the numerical value, the higher the strength.
  • the conventional titanium materials are shown as ASTM Gr. 1 to ASTM Gr. 4, and for each titanium material, the upper limit and the lower limit of the 0.2% yield strength in a tensile test are indicated.
  • ASTM Gr.1 to ASTM Gr.4 mean pure titanium described in ASTM.
  • the pure titanium has a content of titanium of about 99% by mass or more, and are alpha pure titanium having a crystal structure of an alpha phase.
  • the titanium materials of Embodiment 2 are titanium materials containing 91% by mass or more of titanium,
  • the region having the relation of the above formula II is a region indicated by oblique lines.
  • the 0.2% yield strength in a tensile test is high. That is, the titanium materials of Embodiment 2 satisfying the relation of the above formula II are, as compared with the conventional titanium materials having the same contents of components other than titanium, high in strength. Then, the conventional titanium materials have all a 0.2% yield strength in a tensile test and a content of components other than titanium in the region indicated by ⁇ 0.2 ⁇ 600c+180, not satisfying the relation of the above formula II.
  • the 0.2% yield strength ⁇ 0.2 MPa in a tensile test of the titanium materials and the content c % by mass of components other than titanium in the titanium materials have a relation of the following formula II-A:
  • the titanium materials satisfying the relation of the above formula II-A, as compared with the conventional titanium materials having the same contents of components other than titanium, can have a higher strength.
  • the 0.2% yield strength ⁇ 0.2 MPa in a tensile test of the titanium materials and the content c % by mass of components other than titanium in the titanium materials have a relation of the following formula II-B:
  • the titanium materials satisfying the relation of the above formula II-B, as compared with the conventional titanium materials having the same contents of components other than titanium, can have a higher strength.
  • the 0.2% yield strength ⁇ 0.2 in a tensile test of the titanium materials of Embodiment 2 is more than 180 MPa.
  • the lower limit of the 0.2% yield strength ⁇ 0.2 in a tensile test of the titanium materials is, from the viewpoint of securing excellent strength, preferably 250 MPa or more, more preferably 400 MPa or more and still more preferably 550 MPa or more.
  • the upper limit of the 0.2% yield strength ⁇ 0.2 in a tensile test of the titanium materials is, since a higher one is better, not especially limited.
  • the measurement of the 0.2% yield strength in a tensile test of the titanium materials is carried out according to JIS Z2241:2011 “Metallic materials—Tensile testing—Method of test at room temperature”.
  • the test temperature is set at 23° C. ⁇ 5° C.
  • the ranges, of the composition of the titanium materials, the average grain diameter of crystal grains constituting the titanium materials, the content of titanium having a crystal structure of an omega phase of the titanium materials, the 0.2% yield strength in a compression test of the titanium materials, the Vickers hardness of the titanium materials, the heat-resistant temperature of the titanium materials and the volume of the titanium materials, can be the same as the ranges described in Embodiment 1.
  • the titanium materials may contain 98.8% by mass or more of titanium.
  • the strength and the ductility of the titanium materials are more improved.
  • the relation between the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials can be the same as in Embodiment 1. That is, it is preferable that the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials have the relation of the formula I, the formula I-A or the formula I-B described in Embodiment 1. Thereby, the strength and the ductility of the titanium materials are more improved.
  • FIG. 6 is a coordinate system showing the relation between the tensile strength of conventional titanium materials and titanium materials of Embodiment 3 and the content of components other than titanium in these titanium materials.
  • the X axis indicates the amount c (% by mass) of components other than titanium in the titanium materials
  • the Y axis indicates the tensile strength ⁇ B (MPa) of the titanium materials.
  • the tensile strength is one index indicating the strength of materials, and the index indicates that the higher the numerical value, the higher the strength.
  • the conventional titanium materials are shown as JIS-1 to JIS-4, and for the each titanium material, the upper limit and the lower limit of the tensile strength are indicated.
  • JIS-1 to JIS-4 the upper limit and the lower limit of the tensile strength are indicated.
  • the present inventors could produce titanium materials having, with the content of components other than titanium being held, a high tensile strength, that is, a high strength.
  • a high tensile strength that is, a high strength.
  • the titanium materials of Embodiment 3 are titanium materials containing 91% by mass or more of titanium,
  • the region having the relation of the above formula III is a region indicated by oblique lines.
  • the tensile strength is higher. That is, the titanium materials of Embodiment 3 satisfying the relation of the above formula III are, as compared with the conventional titanium materials having the same contents of components other than titanium, higher in tensile strength.
  • the conventional titanium materials have all a tensile strength and a content of components other than titanium in the region indicated by ⁇ B ⁇ 600c+280, not satisfying the relation of the above formula III.
  • the tensile strength ⁇ B MPa of the titanium materials and the content c % by mass of components other than titanium in the titanium materials have a relation of the following formula III-A:
  • the titanium materials satisfying the relation of the above formula III-A, as compared with the conventional titanium materials having the same contents of components other than titanium, can have a higher strength.
  • the tensile strength ⁇ B MPa of the titanium materials and the content c % by mass of components other than titanium in the titanium materials have a relation of the following formula III-B:
  • the titanium materials satisfying the relation of the above formula III-B, as compared with the conventional titanium materials having the same contents of components other than titanium, can have a higher strength.
  • the composition of the titanium materials, the average grain diameter of crystal grains constituting the titanium materials, the content of titanium having a crystal structure of an omega phase of the titanium materials, the 0.2% yield strength in a compression test of the titanium materials, the Vickers hardness of the titanium materials, the heat-resistant temperature of the titanium materials and the volume of the titanium materials can be the same as in Embodiment 1.
  • the titanium materials may contain 98.8% by mass or more of titanium.
  • the strength and the ductility of the titanium materials are more improved.
  • the relation between the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials can be the same as in Embodiment 1. That is, it is preferable that the tensile strength ⁇ B MPa and the fracture elongation ⁇ % of the titanium materials have the relation of the formula I, the formula I-A or the formula I-B described in Embodiment 1. Thereby, the strength and the ductility of the titanium materials are more improved.
  • the relation between the 0.2% yield strength ⁇ 0.2 MPa in a tensile test of the titanium materials and the content c % by mass of components other than titanium in the titanium materials can be the same as in Embodiment 2. That is, it is preferable that the 0.2% yield strength ⁇ 0.2 MPa in a tensile test of the titanium materials and the content c % by mass of components other than titanium in the titanium materials have the relation of the formula II, the formula II-A or the formula II-B described in Embodiment 2. Thereby, the strength and the ductility of the titanium materials are more improved.
  • Embodiment 4 A method for manufacturing the titanium materials of Embodiment 1 to Embodiment 3 (hereinafter, referred to also as “Embodiment 4”) will be described hereinafter. Then, the titanium material of the present disclosure is not limited to those produced by the following manufacturing method, and includes those produced by other methods.
  • Patent Literature 1 a titanium material is manufactured by subjecting pure titanium, an ⁇ -titanium alloy and an ⁇ + ⁇ -titanium alloy to plastic working of a working strain of 0.5 or more under a pressure of 1.5 GPa or more. It is presumed that since the grain size of the crystal grains constituting the titanium material of Patent Literature 1 is as small as several hundreds of nanometers, the ductility is low. Then, since the titanium material is produced with a working strain being imparted to a raw material, strain gradients are present between the center part and edge parts of the titanium materials and the titanium material is heterogeneous, so the titanium material is inappropriate as an object for measuring mechanical properties such as tensile strength.
  • FIG. 7 is a schematic cross-sectional view of a high-pressure cell of an ultrahigh-pressure high-temperature generator to be used in Embodiment 4.
  • a high-pressure cell 10 is equipped with a pressure medium 1 having a regular octahedral shape, a sample container 2 disposed inside pressure medium 1 , and a heating element 3 disposed in the circumference of the sample container.
  • Sample container 2 is composed of hexagonal boron nitride.
  • Heating element 3 is composed of graphite.
  • a raw material 4 is enclosed inside sample container 2 .
  • the maximum load of the ultrahigh-pressure high-temperature generator to be used in Embodiment 4 is, for example, 2,800 tons.
  • a conventional titanium alloy or pure titanium containing 98.8% by mass or more of titanium is prepared.
  • the titanium in the titanium alloy or pure titanium is an alpha titanium having a crystal structure of an alpha phase.
  • the above raw material is put in a sample container made of a polycrystalline hexagonal boron nitride, and by using an ultrahigh-pressure high-temperature generator, pressurized up to 6 to 11 GPa, thereafter heated up to 200 to 600° C. and held for 1 to 5 hours. Thereby, the titanium material of the present disclosure is obtained.
  • the titanium material of the present disclosure obtained by the above method has a high strength and a high ductility. The reason therefor is presumably as follows.
  • the phase transformation from the alpha titanium to the omega titanium is carried out.
  • the rearrangement of atoms needs an energy. Accordingly, the phase transformation from the alpha titanium to the omega titanium is initiated at a pressure and a temperature beyond the dotted line indicated by the ⁇ -> ⁇ hysteresis of FIG. 3 , due to the effect of hysteresis.
  • the high-pressure high temperature treatment is carried out under the pressure and temperature condition in the vicinity of the dotted line indicated by the ⁇ -> ⁇ hysteresis of FIG. 3 .
  • the overpressure is low, and crystal nuclei of the omega titanium are generated only at limited places such as grain boundary junction points and excess generation of crystal nuclei hardly occurs. Accordingly, it is presumed that the grain diameter of the crystal grains constituting obtained titanium materials easily becomes large and the titanium materials have a high ductility.
  • Embodiment 4 for the heating element of the ultrahigh-pressure high-temperature generator, a graphite having a high thermal conductivity (thermal conductivity: 2,000 W/(m ⁇ K)) is used; and for the sample container, a hexagonal boron nitride having a high thermal conductivity (thermal conductivity: 600 W/(m ⁇ K)) is used.
  • thermo conductivity 2,000 W/(m ⁇ K)
  • a hexagonal boron nitride having a high thermal conductivity thermal conductivity: 600 W/(m ⁇ K)
  • the manufacturing method of Embodiment 4 since the synthesis pressure is 6 to 11 GPa and the maximum load of the manufacturing apparatus is 2,800 tons, there can be produced, for example, cylindrical large-sized titanium materials of 10 mm or more in diameter, 6 mm or more in height and 471 mm 3 or more in volume. Since the titanium materials have a sufficient diameter, test pieces for carrying out a tensile test can be produced therefrom.
  • the ⁇ -Ti is treated at 12 GPa and 400° C., which sufficiently exceed the dotted line indicated by the ⁇ -> ⁇ hysteresis of FIG. 3 . Since this pressure and temperature condition is away from the dotted line indicated by the ⁇ -> ⁇ hysteresis of FIG. 3 , and the overpressure is high, many crystal nuclei of the omega titanium are generated. Accordingly, it is presumed that the grain diameter of crystal grains constituting the obtained titanium materials is small and is about several tens to several hundreds of nanometers.
  • a heating element of the ultrahigh-pressure high-temperature generator a lanthanum chromite oxide (LaCr 2 O 3 , thermal conductivity: 5 W/(m ⁇ K) or less) is used; and as a sample container, a magnesia (MgO: 60 W/(m ⁇ K)) is used.
  • LaCr 2 O 3 thermal conductivity: 5 W/(m ⁇ K) or less
  • MgO magnesia
  • the titanium materials obtained in the above literatures are small (cylindrical with 4 mm in diameter, 3 mm in height, and 37.7 mm 3 in volume), and cannot be processed to a test piece for measuring mechanical properties such as tensile strength. Since the manufacturing condition of the above literatures uses a pressure of as high as 12 GPa, the upsizing of the titanium materials is difficult.
  • alpha pure titanium having the following composition was prepared. N: 0.03% by mass, C: 0.08% by mass, H: 0.015% by mass, O: 0.18% by mass, Fe: 0.20% by mass, Ti (having a crystal structure of an alpha phase): balance.
  • the alpha pure titanium was put in a sample container made of a polycrystalline hexagonal boron nitride, and pressurized up to 8 GPa and thereafter heated up to 400° C., and held for 3 hours, by using a multianvil ultrahigh-pressure high-temperature generator (“mavo press LPR 1000-400/50”, manufactured by Voggenreiter Verlag GmbH, heating element: made of graphite, maximum load: 2,800 tons), to thereby obtain a titanium material.
  • the obtained titanium material was cylindrical and had a size of 10 mm in diameter, 6 mm in height and 471 mm 3 in volume.
  • the titanium material was produced by the above manufacturing method; and there were measured the composition, the tensile strength ⁇ B, the fracture elongation ⁇ %, the 0.2% yield strength ⁇ 0.2 in a tensile test, the content of omega titanium, the content c of components other than titanium in the titanium material, the average grain diameter of crystal grains constituting the titanium material, the 0.2% yield strength in a compression test, the Vickers hardness and the heat-resistant temperature. Since the measuring methods of respective measurement items were as described in Embodiment 1 and Embodiment 2, the description thereof is not repeated. The results are as follows.
  • the titanium material of Example 1 contained 91% by mass or more of titanium, and as shown in FIG. 1 , FIG. 5 and FIG. 6 , the titanium material satisfied the relations of the above formula I, formula II and formula III, and had a high strength and a high ductility.
  • alpha pure titanium having the following composition was prepared. N: 0.05% by mass, C: 0.08% by mass, H: 0.015% by mass, O: 0.40% by mass, Fe: 0.50% by mass, Ti (having a crystal structure of an alpha phase): balance.
  • the alpha pure titanium was put in a sample container made of a polycrystalline hexagonal boron nitride, and pressurized up to 8 GPa and thereafter heated up to 400° C., and held for 3 hours, by using a multianvil ultrahigh-pressure high-temperature generator (“mavo press LPR 1000-400/50”, manufactured by Voggenreiter Verlag GmbH, heating element: made of graphite, maximum load: 2,800 tons), to thereby obtain a titanium material.
  • the obtained titanium material was cylindrical and had a size of 10 mm in diameter, 6 mm in height and 471 mm 3 in volume.
  • the titanium material was produced by the above manufacturing method; and there were measured the composition, the tensile strength ⁇ B, the fracture elongation ⁇ %, the 0.2% yield strength ⁇ 0.2 in a tensile test, the content of omega titanium, the content c of components other than titanium in the titanium material, the average grain diameter of crystal grains constituting the titanium material, the 0.2% yield strength in a compression test, the Vickers hardness and the heat-resistant temperature. Since the measuring methods of respective measurement items were as described in Embodiment 1 and Embodiment 2, the description thereof is not repeated. The results are as follows.
  • the titanium material of Example 2 contained 91% by mass or more of titanium, and as shown in FIG. 1 , FIG. 5 and FIG. 6 , the titanium material satisfied the relations of the above formula I, formula II and formula III, and had a high strength and a high ductility.
  • alpha pure titanium having the following composition was prepared.
  • the alpha pure titanium was put in a sample container made of a polycrystalline hexagonal boron nitride, and pressurized up to 8 GPa and thereafter heated up to 400° C., and held for 3 hours, by using a multianvil ultrahigh-pressure high-temperature generator (“mavo press LPR 1000-400/50”, manufactured by Voggenreiter Verlag GmbH, heating element: made of graphite, maximum load: 2,800 tons), to thereby obtain a titanium material.
  • the obtained titanium material was cylindrical and had a size of 10 mm in diameter, 6 mm in height and 471 mm 3 in volume.
  • the titanium material was produced by the above manufacturing method; and there were measured the composition, the tensile strength ⁇ B, the fracture elongation ⁇ %, the 0.2% yield strength ⁇ 0.2 in a tensile test, the content of omega titanium, the content c of components other than titanium in the titanium material, the average grain diameter of crystal grains constituting the titanium material, the 0.2% yield strength in a compression test, the Vickers hardness and the heat-resistant temperature. Since the measuring methods of respective measurement items were as described in Embodiment 1 and Embodiment 2, the description thereof is not repeated. The results were as follows.
  • the titanium material of Example 3 contained 91% by mass or more of titanium, and as shown in FIG. 1 , FIG. 5 and FIG. 6 , the titanium material satisfied the relations of the above formula I, formula II and formula III, and had a high strength and a high ductility.
  • Embodiments and Examples of the present disclosure have been described, but it is contemplated from the beginning to suitably combine and variously modify the above-mentioned constitutions of the Embodiments and Examples.

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