US20150101711A1 - High-strength seamless stainless steel tube for oil country tubular goods and method of manufacturing the same - Google Patents

High-strength seamless stainless steel tube for oil country tubular goods and method of manufacturing the same Download PDF

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US20150101711A1
US20150101711A1 US14/403,731 US201314403731A US2015101711A1 US 20150101711 A1 US20150101711 A1 US 20150101711A1 US 201314403731 A US201314403731 A US 201314403731A US 2015101711 A1 US2015101711 A1 US 2015101711A1
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steel tube
mass
chemical composition
stainless steel
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Yukio Miyata
Yasuhide Ishiguro
Kazutoshi Ishikawa
Tetsu Nakahashi
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JFE Steel Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/54—Ferrous alloys, e.g. steel alloys containing chromium with nickel with boron
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
    • C21D8/105—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies of ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • C21D9/085—Cooling or quenching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/46—Ferrous alloys, e.g. steel alloys containing chromium with nickel with vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/50—Ferrous alloys, e.g. steel alloys containing chromium with nickel with titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/001—Austenite
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/005—Ferrite
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D2211/00—Microstructure comprising significant phases
    • C21D2211/008—Martensite

Definitions

  • This disclosure relates to a seamless steel tube for oil country tubular goods, in particular, to a high-strength seamless stainless steel tube with both excellent low-temperature toughness and excellent corrosion resistance.
  • duplex stainless tubes have been used.
  • duplex stainless tubes contain a large amount of alloying chemical elements and are poor in terms of hot formability, duplex stainless tubes can be manufactured by only using particular kinds of hot processing and are expensive.
  • Japanese Unexamined Patent Application Publication No. 2005-336595 describes a method of manufacturing a high-strength stainless steel tube for oil country tubular goods with excellent corrosion resistance, the method including making a steel tube material having a chemical composition including, by mass %, C: 0.005% to 0.05%, Si: 0.05% to 0.5%, Mn: 0.2% to 1.8%, Cr: 15.5% to 18%, Ni: 1.5% to 5%, Mo: 1% to 3.5%, V: 0.02% to 0.2%, N: 0.01% to 0.15%, and O: 0.006% or less, in which relational expressions (1) and (2) below are satisfied, into a steel tube having a specified size by performing hot processing for tube making, cooling the tube down to room temperature at a cooling rate equal to or more than an air-cooling rate after tube making has been performed and performing quenching-tempering on the tube by reheating the tube up to a temperature of 850° C. or higher, subsequently cooling the heated tube down to
  • Japanese Patent No. 4577457 describes a method of manufacturing a stainless steel tube, the method including making a billet having a chemical composition containing, by mass %, C: 0.001% to 0.05%, Si: 0.05% to 1%, Mn: 2% or less, Cr: 16% to 18%, Ni: 3.5% to 7%, Mo: more than 2% and 4% or less, Cu: 1.5% to 4%, rare-earth element: 0.001% to 0.3%, sol.
  • a method of manufacturing a high-strength seamless stainless steel tube for oil country tubular goods having a wall thickness of more than 25.4 mm including heating a steel material; hot rolling including piercing rolling the steel material into a seamless steel tube; and cooling the seamless steel tube down to room temperature at a cooling rate equal to or more than an air-cooling rate, the steel material having a chemical composition containing, by mass %, C: 0.005% or more and 0.06% or less, Si: 0.05% or more and 0.5% or less, Mn: 0.2% or more and 1.8% or less, P: 0.03% or less, S: 0.005% or less, Cr: 15.5% or more and 18.0% or less, Ni: 1.5% or more and 5.0% or less, V: 0.02% or more and 0.2% or less, Al: 0.002% or more and 0.05% or less, N: 0.01% or more and 0.15% or less, O: 0.006% or less, and further containing one, two or more selected from among Mo: 1.0% or more and 3.
  • a high-strength seamless stainless steel tube for oil country tubular goods having a wall thickness of more than 25.4 mm the steel tube having a chemical composition containing, by mass %, C: 0.005% or more and 0.06% or less, Si: 0.05% or more and 0.5% or less, Mn: 0.2% or more and 1.8% or less, P: 0.03% or less, S: 0.005% or less, Cr: 15.5% or more and 18.0% or less, Ni: 1.5% or more and 5.0% or less, V: 0.02% or more and 0.2% or less, Al: 0.002% or more and 0.05% or less, N: 0.01% or more and 0.15% or less, O: 0.006% or less, and further containing one, two or more selected from among Mo: 1.0% or more and 3.5% or less, W: 3.0% or less and Cu: 3.5% or less and the balance being Fe and inevitable impurities, in which relational expressions (1) and (2) below are satisfied, having a microstructure including a martensite phase as a main phase
  • FIG. 1 is a graph illustrating the relationship between absorbed energy vE ⁇ 10 in a Charpy impact test and a GSI value.
  • a microstructure was observed using an optical microscope (at a magnification of 400 times).
  • a GSI value was determined as an index representing the degree of a decrease in the grain diameter of a microstructure.
  • the GSI value was determined by counting the number of ferrite-martensite grain boundaries per unit length (line/mm) in the wall thickness direction using the obtained microstructure photograph.
  • FIG. 1 indicates that it is necessary to decrease the grain diameter of a microstructure to GSI: 120 or more to achieve toughness of vE ⁇ 10 : 40 J or more. From the results of other experiments, we confirmed that a decrease in the grain diameter of a microstructure to GSI: 120 or more can be achieved by performing hot rolling under conditions such that the total rolling reduction in a temperature of 1100° C. to 900° C. is 30% or more.
  • hot rolling including piercing rolling where a slab is heated at an ordinary heating temperature (1100° C. to 1250° C.), a temperature of 1100° C. to 900° C. corresponds to rolling using an elongator mill and a plug mill or an mandrel mill.
  • a seamless steel tube is manufactured by heating a steel material and by performing hot rolling including piercing rolling.
  • the steel material has a chemical composition containing C: 0.005% or more and 0.06% or less, Si: 0.05% or more and 0.5% or less, Mn: 0.2% or more and 1.8% or less, P: 0.03% or less, S: 0.005% or less, Cr: 15.5% or more and 18.0% or less, Ni: 1.5% or more and 5.0% or less, V: 0.02% or more and 0.2% or less, Al: 0.002% or more and 0.05% or less, N: 0.01% or more and 0.15% or less, O: 0.006% or less, and further containing one, two or more selected from among Mo: 1.0% or more and 3.5% or less, W: 3.0% or less and Cu: 3.5% or less and the balance being Fe and inevitable impurities, in which (1) and (2) are satisfied:
  • C is a chemical element related to an increase in the strength of martensitic stainless steel. It is necessary that the C content be 0.005% or more in the present invention. On the other hand, when the C content is more than 0.06%, there is a significant deteriorate in corrosion resistance. Therefore, the C content is limited to 0.005% or more and 0.06% or less, preferably 0.01% or more and 0.04% or less.
  • Si 0.05% or More and 0.5% or Less
  • Si is a chemical element which functions as a deoxidation agent, and Si is added in the amount of 0.05% or more.
  • the Si content is limited to 0.05% or more and 0.5% or less, preferably 0.1% or more and 0.4% or less.
  • Mn is a chemical element which increases strength, and Mn is added in the amount of 0.2% or more to achieve the desired high strength.
  • Mn content is more than 1.8%, there is a negative influence on toughness. Therefore, the Mn content is limited to 0.2% or more and 1.8% or less, preferably 0.2% or more and 0.8% or less.
  • the P content be as small as possible. However, since the P content is controlled at comparatively low cost without deteriorating corrosion resistance when the P content is 0.03% or less, it is acceptable that the P content is about 0.03% or less. Therefore, the P content is limited to 0.03% or less. Since there is an increase in manufacturing cost when the P content is excessively small, it is preferable that the P content be 0.005% or more.
  • the S content be as small as possible. However, it is acceptable that the S content is 0.005% or less, because it is possible to manufacture a pipe using normal processes when the S content is 0.005% or less. Therefore, the S content is limited to 0.005% or less. Since there is an increase in manufacturing cost when the S content is excessively small, it is preferable that the S content be 0.0005% or more.
  • Cr is a chemical element which enhances corrosion resistance as a result of forming a protective film and, in particular contributes to an enhancement in CO 2 corrosion resistance. It is necessary that the Cr content be 15.5% or more to enhance corrosion resistance at a high temperature. On the other hand, when the Cr content is more than 18%, there is a deterioration in hot formability and there is a decrease in strength. Therefore, the Cr content is limited to 15.5% or more and 18.0% or less, preferably 16.0% or more and 17.5% or less, more preferably 16.5% or more and 17.0% or less.
  • Ni is a chemical element effective in increasing corrosion resistance by strengthening a protective film and which increases the strength of steel as a result of forming a solid solution. These effects become noticeable when the Ni content is 1.5% or more. On the other hand, when the Ni content is more than 5.0%, since there is a decrease in the stability of a martensite phase, there is a decrease in strength. Therefore, the Ni content is limited to 1.5% or more and 5.0% or less, preferably 3.0% or more and 4.5% or less.
  • V 0.02% or More and 0.2% or Less
  • V contributes to an increase in strength through solid solution strengthening and is effective in increasing resistance to stress corrosion cracking. It is necessary that the V content be 0.02% or more to realize these effects. On the other hand, when the V content is more than 0.2%, there is a deterioration in toughness. Therefore, the V content is limited to 0.02% or more and 0.2% or less, preferably 0.03% or more and 0.08% or less.
  • Al is a chemical element which functions as a deoxidation agent, and it is necessary that the Al content be 0.002% or more to realize this effect.
  • the Al content is more than 0.05%, since there is an increase in the amount of alumina containing inclusions, there is a deterioration in ductility and toughness. Therefore, the Al content is limited to 0.002% or more and 0.05% or less, preferably 0.01% or more and 0.04% or less.
  • N is a chemical element which markedly enhances pitting corrosion resistance, and it is necessary that the N content be 0.01% or more.
  • the N content is more than 0.15%, various nitrides are formed and there is a deterioration in toughness. Therefore, the N content is limited to 0.01% or more and 0.15% or less, preferably 0.02% or more and 0.08% or less.
  • O is present in the form of an oxide in steel and has a negative effect on ductility, toughness and so forth. Therefore, it is preferable that the O content be as small as possible. In particular, when the O content is more than 0.006%, there is a significant deterioration in hot formability, toughness and corrosion resistance. Therefore, the O content is limited to 0.006% or less.
  • Mo is a chemical element which contributes to an enhance in corrosion resistance by increasing resistance to pitting corrosion caused by and it is necessary that the Mo content be 1.0% or more.
  • Mo content when the Mo content is more than 3.5%, there is a deterioration in strength and toughness and an increase in material cost. Therefore, when Mo is added, the Mo content is limited to 1.0% or more and 3.5% or less, preferably 1.5% or more and 3.0% or less.
  • W is a chemical element which contributes to an enhance in corrosion resistance like Mo, and it is preferable that the W content be 0.5% or more.
  • the W content is more than 3.0%, there is a deterioration in toughness and there is an increase in material cost. Therefore, when W is added, the W content is limited to 3.0% or less, preferably 0.5% or more and 2.5% or less.
  • Cu Since Cu is effective in suppressing penetration of hydrogen into steel by strengthening a protective film, Cu contributes to an enhancement in corrosion resistance. It is preferable that the Cu content be 0.5% or more to realize these effects. However, when the Cu content is more than 3.5%, there is a deterioration in hot formability. Therefore, when Cu is added, the Cu content is limited to 3.5% or less, preferably 0.5% or more and 2.5% or less.
  • the chemical composition described above is a base chemical composition and, in addition to the base chemical composition, one or more selected from among Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less and B: 0.01% or less and/or Ca: 0.01% or less may be added.
  • Nb 0.2% or Less
  • Ti 0.3% or Less
  • Zr 0.2% or Less
  • B 0.01% or Less
  • Nb, Ti, Zr and B are all chemical elements which increase the strength of steel and enhance resistance to stress corrosion cracking, one or more selected from among these chemical elements may be added as needed. It is preferable that the contents of these chemical elements be respectively Nb: 0.02% or more, Ti: 0.04% or more, Zr: 0.02% or more and B: 0.001% or more to realize these effects. On the other hand, when the contents of these chemical elements are respectively Nb: more than 0.2%, Ti: more than 0.3%, Zr: more than 0.2% and B: more than 0.01%, there is a deterioration in toughness. Therefore, the contents of these chemical elements are respectively limited to Nb: 0.2% or less, Ti: 0.3% or less, Zr: 0.2% or less and B: 0.01% or less.
  • Ca is a chemical element which contributes to a morphology control function of sulfides as a result of spheroidizing sulfide containing inclusions
  • Ca may be added as needed.
  • the Ca content be 0.0005% or more to realize this effect.
  • the Ca content when the Ca content is more than 0.01%, there is an increase in the amount of oxide containing inclusions, which deteriorates corrosion resistance. Therefore, when Ca is added, it is preferable that the Ca content be 0.01% or less.
  • the remainder of the chemical composition other than the constituent chemical elements described above consists of Fe and inevitable impurities.
  • molten steel having a specified chemical composition be smelted using a common refining method such as one using a steel converter and that the smelted steel be made into a cast material such as a billet using a common casting method such as a continuous casting method.
  • a cast material such as a billet may be manufactured using an ingot casting-blooming method.
  • a seamless steel tube is manufactured by heating a steel material having the chemical composition described above, by performing ordinary hot rolling including piercing rolling using a Mannesmann-plug mill method or a Mannesmann-mandrel mill method, and further performing cooling down to room temperature at a cooling rate equal to or more than an air-cooling rate.
  • the wall thickness of the seamless steel tube is set to be more than 25.4 mm.
  • the size of a steel material which is a starting material is controlled to be within an appropriate range to achieve a seamless steel tube having such a wall thickness. Heating temperature of a steel material: 1100° C. or higher and 1300° C. or lower
  • the heating temperature of a steel material When the heating temperature of a steel material is lower than 1100° C., there is an enhancement in deformation resistance due to the heating temperature being excessively low and it is difficult to perform hot rolling due to a load on rolling mills being excessively large. On the other hand, when the heating temperature is higher than 1300° C., there is a deterioration in toughness due to an increase in crystal grain diameter and there is a decrease in yield due to an increase in the amount of scale loss. Therefore, it is preferable that the heating temperature of a steel material be 1100° C. or higher and 1300° C. or lower, more preferably 1200° C. or higher and 1280° C. or lower.
  • the steel material which has been heated up to the heating temperature descried above is subjected to hot rolling including piercing rolling.
  • hot rolling any of an ordinary Mannesmann-plug mill method, in which the steel material is subjected to processing using a piercer mill for performing piercing rolling, a subsequent elongator mill, a plug mill and a realer mill or, further, a sizing mill in this order, and an ordinary Mannesmann-mandrel mill method, in which the steel material is subjected to processing using a piercer mill to perform piercing rolling, a subsequent mandrel mill and reducer mill in this order, may be used.
  • the hot rolling including piercing rolling described above is performed under conditions such that the total rolling reduction in a temperature range of 1100° C. to 900° C. is 30% or more.
  • rolling reduction in this temperature range to be within an appropriate range, the spacing between ferrite-austenite (martensite) grain boundaries can be controlled to be small and a decrease in grain diameter can be achieved, which results in an enhancement in toughness.
  • rolling reduction is controlled in a temperature range out of 1100° C. to 900° C., if rolling reduction in the temperature range of 1100° C. to 900° C. is out of the appropriate range described above, a decrease in grain diameter cannot be achieved.
  • the rolling reduction in this temperature range is 30% or more.
  • the spacing between ferrite-austenite (martensite) grain boundaries is equal to or less than the specified value, a decrease in grain diameter can be realized even in a steel tube having a thick wall, which results in an enhance in toughness. Note that there is no particular limitation on the upper limit of rolling reduction in this temperature range.
  • the seamless steel tube which has been manufactured by performing hot rolling for tube making as described above is subsequently subjected to cooling down to room temperature at a cooling rate equal to or more than an air-cooling rate.
  • a microstructure including a martensite phase as a main phase can be achieved by performing cooling at a cooling rate equal to or more than an air-cooling rate.
  • the cooled steel tube is subsequently subjected to a heat treatment including quenching-tempering.
  • the steel tube In quenching, the steel tube is heated up to a heating temperature for quenching at 850° C. or higher and 1000° C. or lower, and then cooled with water.
  • a heating temperature for quenching When the heating temperature for quenching is lower than 850° C., transformation into a martensite does not sufficiently progress, and the desired high strength cannot be achieved. Further, there is concern that intermetallic compounds may be formed and toughness and corrosion resistance may deteriorate.
  • the heating temperature for quenching when the heating temperature for quenching is higher than 1000° C., the fraction of a martensite formed becomes excessively high, and strength becomes excessively high. Therefore, it is preferable that the heating temperature for quenching be 850° C. or higher and 1000° C. or lower.
  • a holding time when heating is performed for quenching there is no particular limitation on a holding time when heating is performed for quenching.
  • the holding time be 10 to 30 minutes from the viewpoint of productivity.
  • the heating temperature for quenching be 920° C. or higher and 980° C. or lower.
  • tempering is further performed.
  • the steel tube is heated up to a tempering temperature of 400° C. or higher and 700° C. or lower, and then cooled at a cooling rate equal to or more than an air-cooling rate.
  • a tempering temperature 400° C. or higher and 700° C. or lower.
  • the tempering temperature be 400° C. or higher and 700° C. or lower. Note that there is no particular limitation on a holding time when heating for tempering is performed. However, it is preferable that the holding time be 20 to 60 minutes from the viewpoint of productivity. Further, it is more preferable that the tempering temperature be 550° C. or higher and 650° C. or lower.
  • tempering described above may be performed without performing quenching on the steel tube which has been subjected to tube making.
  • the seamless steel tube manufactured using the manufacturing method described above has a chemical composition described above and a microstructure including a martensite phase as a main phase and a second phase consisting of, at volume ratio, 10% or more and 60% or less of a ferrite phase and 0% or more and 10% or less of an austenite phase.
  • the steel tube is a thick high-strength seamless stainless steel tube for oil country tubular goods having a wall thickness of more than 25.4 mm and having a microstructure in which a GSI value, which is defined as the number of ferrite-martensite grain boundaries per unit length of a line segment drawn in the wall thickness direction, is 120 or more in the central portion in the wall thickness direction.
  • a microstructure includes a martensite phase as a main phase and a second phase consisting of, at volume ratio, 10% or more and 60% or less of a ferrite phase and 0% or more and 10% or less of an austenite phase in order to achieve the desired high strength.
  • the volume ratio of a ferrite phase When the volume ratio of a ferrite phase is less than 10%, there is a deterioration in hot formability. On the other hand, when the volume ratio of a ferrite phase is more than 60%, there is a deterioration in strength and toughness.
  • the second phase may include 10% or less of an austenite phase other than a ferrite phase, it is preferable that the volume ratio of an austenite phase be as small as possible, including 0%, to achieve sufficient strength. When the volume ratio of an austenite phase is more than 10%, it is difficult to achieve the desired high strength.
  • the steel tube has a microstructure including a martensite and a ferrite phase and, further, a retained austenite phase as described above, in which a GSI value, which is defined as the number of ferrite-martensite grain boundaries per unit length of a line segment drawn in the wall thickness direction, is 120 or more in the central portion in the wall thickness direction.
  • a GSI value which is defined as the number of ferrite-martensite grain boundaries per unit length of a line segment drawn in the wall thickness direction, is 120 or more in the central portion in the wall thickness direction.
  • a GSI value is a value which can be determined by counting the number (line/mm) of ferrite-martensite grain boundaries in the wall thickness direction using a microstructure photograph taken through the observation of a sample, which has been etched with a vilella's reagent, using an optical microscope (magnification of 100 to 1000 times).
  • Molten steels having the chemical compositions given in Table 1 were smelted using a steel converter, and then cast into billets (steel materials having an outer diameter of 260 mm) using a continuous casting method.
  • the obtained steel materials were heated at the temperatures given in Table 2, and then made into seamless steel tubes (having an outer diameter of 168.3 to 297 mm ⁇ and a wall thickness of 26 to 34 mm) by performing hot rolling using an ordinary Mannesmann-plug mill method in which the steel material is subjected to hot processing using a piercing mill, an elongator mill, a plug mill and realer mill or, further, a sizing mill in this order under conditions such that the rolling reduction in a temperature range of 1100° C. to 900° C. satisfied the conditions given in Table 2. Further, after hot rolling had been performed, cooling was performed under the conditions given in Table 2. The obtained seamless steel tubes were subjected to quenching-tempering under the conditions given in Table 2.
  • a microstructure in a cross section in the wall thickness direction which had been polished and etched with a vilella's reagent, was observed using an optical microscope (at a magnification of 100 to 1000 times).
  • the kinds of microstructures were identified, and the fraction (volume ratio) of a ferrite phase was calculated by performing image analysis.
  • I ⁇ integrated intensity of a ⁇ phase
  • test piece for microstructure observation was etched with a vilella's reagent and observed using an optical microscope (at a magnification of 400 times). Using the taken photograph, the number (line/mm) of ferrite-martensite grain boundaries was counted in the wall thickness direction in order to calculate a GSI value.
  • a strip specimen specified by API standard (having a gage length of 50.8 mm) was cut out of the central portion in the wall thickness direction of the obtained steel tube in accordance with API standard so that the tensile direction is the direction of the tube axis.
  • tensile properties yield strength YS, tensile strength TS and elongation El
  • V-notch test piece (having a thickness of 10 mm) which was cut out of the central portion in the wall thickness direction of the obtained steel tube in accordance with ISO standard so that the longitudinal direction of the test piece was the circumferential direction of the tube
  • Charpy impact test was performed under a condition of a test temperature of ⁇ 10° C. in order to determine absorbed energy vE ⁇ 10 (J).
  • the number of the test pieces was 3 for each steel tube, the average value of the three was used as the value for the steel tube.
  • a test specimen for a corrosion test (having a thickness of 3 mm, a width of 25 mm and a length of 50 mm) was cut out of the central portion in the wall thickness direction of the obtained steel tube and used for a corrosion test.
  • the test specimen was immersed in a 20% NaCl aqueous solution (having a temperature of 230° C. with carbon dioxide gas of 3.0 MPa being dissolved in the saturated state) which was contained in an autoclave, for 14 days. After the corrosion test had been performed, by determining the weight of the test specimen, a corrosion rate was calculated from a decrease in weight. In addition, after the corrosion test had been performed, the test specimen was observed using a loupe at a magnification ratio of 50 times to observe whether or not pitting corrosion occurred. Pitting corrosion of a diameter of 0.2 mm or more was observed and evaluated.
  • Comparative Examples corresponded to one or more of when the desired high strength was not achieved, when a GSI value was less than 120 and vE ⁇ 10 (J) was less than 40 J, which means high toughness was not stably achieved, and when a decrease in weight due to corrosion was more than 0.127 mm/year, which means there was a deteriorate in corrosion resistance.

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