WO2023231981A1 - 一种高强度石油套管及其制造方法 - Google Patents

一种高强度石油套管及其制造方法 Download PDF

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Publication number
WO2023231981A1
WO2023231981A1 PCT/CN2023/096906 CN2023096906W WO2023231981A1 WO 2023231981 A1 WO2023231981 A1 WO 2023231981A1 CN 2023096906 W CN2023096906 W CN 2023096906W WO 2023231981 A1 WO2023231981 A1 WO 2023231981A1
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Prior art keywords
strength
temperature
manufacturing
controlled
petroleum casing
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PCT/CN2023/096906
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English (en)
French (fr)
Inventor
董晓明
高展
彭黎阳
徐福昌
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Baoshan Iron and Steel Co Ltd
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Baoshan Iron and Steel Co Ltd
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Priority to JP2024570794A priority Critical patent/JP2025519284A/ja
Priority to US18/870,424 priority patent/US20250327156A1/en
Priority to DE112023002451.0T priority patent/DE112023002451T5/de
Publication of WO2023231981A1 publication Critical patent/WO2023231981A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18—Hardening; Quenching with or without subsequent tempering
    • C21D1/25—Hardening, combined with annealing between 300 degrees Celsius and 600 degrees Celsius, i.e. heat refining ("Vergüten")
    • 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
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/60—Aqueous agents
    • 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
    • C21D7/00—Modifying the physical properties of iron or steel by deformation
    • C21D7/13—Modifying the physical properties of iron or steel by deformation by hot working
    • 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 of ferrous metals or ferrous alloys by deformation combined with, or followed by, heat treatment
    • C21D8/10—Modifying the physical properties of ferrous metals or ferrous alloys 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
    • 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
    • C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L9/00—Rigid pipes
    • F16L9/02—Rigid pipes of metal
    • 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
    • C21D2211/003—Cementite
    • 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
    • C21D2211/009—Pearlite

Definitions

  • the present invention relates to a steel pipe and a manufacturing method thereof, in particular to an oil casing and a manufacturing method thereof.
  • the publication number is CN103774063A
  • the publication date is May 7, 2014
  • the Chinese patent document titled "A large-diameter petroleum casing and its TMCP production method" discloses a low carbon equivalent microalloy steel pipe and its online Normalizing process, it has stable mechanical properties and good anti-collapse performance.
  • This technical solution uses the TMCP production method, which has a simple process and high production efficiency.
  • the patent uses medium carbon CrMo steel, which is similar to conventional oil well pipe materials. There is still a risk of cracking during online quenching.
  • the publication number is CN103757561A
  • the publication number is April 30, 2014
  • the publication number is CN103757561A.
  • a large-diameter thick-walled marine seamless steel pipe and its TMCP production method were developed. It has stable mechanical properties and good low-temperature impact properties. However, its high alloy content leads to the risk of cracking during online quenching.
  • the present invention hopes to develop and obtain a new high-strength petroleum casing and its manufacturing method.
  • One of the purposes of the present invention is to provide a high-strength petroleum casing, which can obtain excellent mechanical properties through reasonable component matching and process design, and has both high strength and high toughness.
  • the strength is 552-965MPa
  • the tensile strength is ⁇ 689MPa
  • the elongation is ⁇ 20%
  • the 0°C transverse Charpy impact energy is ⁇ 80J, which can meet the performance requirements of high-strength casing in oil and gas fields.
  • the present invention provides a high-strength petroleum casing, which contains Fe and inevitable impurity elements, and also contains the following chemical elements in the following mass percentages:
  • the mass percentage of each chemical element is:
  • the balance is Fe and unavoidable impurities
  • La+Ce 0.002-0.005%.
  • C is a carbide-forming element, which can improve the strength of steel.
  • the C element content in the steel is lower than 0.06%, the hardenability of the steel will be reduced, thereby reducing the toughness of the steel; however, when the C element content in the steel is higher than 0.15%, it will significantly worsen the segregation of the steel. , prone to quenching cracks. Therefore, taking into account the impact of the C element content on the properties of steel, in order to meet the high strength requirements of the oil casing, in the high-strength oil casing of the present invention, the mass percentage content of the C element is controlled to 0.06-0.15 %between.
  • the mass percentage of the C element can be preferably controlled between 0.08-0.14%.
  • the Si element can be solid dissolved in ferrite, which can improve the yield strength of the steel.
  • Si is also a ferrite-forming element, which is beneficial to improving the toughness of steel.
  • the Si element content in the steel should not be too low. When the Si element content is less than 0.3%, the oil casing will be easily oxidized. At the same time, the addition amount of Si element in the steel should not be too high. Too high a content of Si will cause the oil casing to be easily oxidized. Elements can deteriorate the processability and toughness of steel. Therefore, in order to exert the beneficial effects of Si element, the content of Si element in steel must be strictly controlled. In the high-strength petroleum casing of the present invention, the mass percentage content of Si element is controlled between 0.3-0.5%.
  • the mass percentage of Si element can be preferably controlled between 0.3-0.45%.
  • Mn is an austenite-forming element, which can improve the hardenability of the steel.
  • Mn element content is less than 1.5%, the hardenability of the steel will be significantly reduced, thereby reducing the proportion of martensite in the steel and reducing the toughness of the steel; and when Mn in the steel When the content is greater than 2.2%, component segregation will easily occur and quenching cracks will occur. Therefore, considering the influence of Mn element content on steel properties, in the high-strength petroleum casing of the present invention, the mass percentage content of Mn element is controlled between 1.5-2.2%.
  • the mass percentage of the Mn element can be preferably controlled between 1.6-2.0%.
  • Rare earth (La, Ce) In the high-strength petroleum casing of the present invention, both Ce and La are rare earth elements. Adding a certain proportion of the rare earth mixture to the steel can modify and refine the inclusions in the steel.
  • the rare earth modified product formed is REAlO 3 , which can remove larger inclusions, reduce oxygen content, and improve Toughness index of steel.
  • the refined inclusions serve as nucleation points for dynamic recrystallization during rolling and can also promote the formation of recrystallization, thus refining the austenite grains and inhibiting direct quenching cracking after rolling.
  • the inventor's research found that when the Ce+La content in the steel is >0.006%, coarse inclusions are likely to form, which will reduce the toughness of the material; if the Ce+La content in the steel is ⁇ 0.002%, the grains will be refined and the material will be modified. The effect of sexual inclusions is not obvious and quenching cracking is easy to occur. Therefore, in order to exert the beneficial effects of La and Ce rare earth elements, in the high-strength petroleum casing of the present invention, the content of La and Ce elements and "rare earth (La, Ce)" are controlled between 0.002-0.006% .
  • the contents of rare earth elements La and Ce can be preferably controlled between 0.0025-0.004%.
  • Ti is a strong carbon nitride-forming element, which can significantly refine the austenite grains in the steel and make up for the decrease in strength caused by the decrease in carbon content. .
  • the mass percentage content of Ti element needs to be controlled to Ti ⁇ 0.05%.
  • the mass percentage content of the Ti element can be preferably controlled to Ti ⁇ 0.03%.
  • Al In the high-strength petroleum casing of the present invention, Al is a good deoxidizing and nitrogen-fixing element, which can effectively refine the grains. Therefore, in order to exert the beneficial effects of Al element, in the present invention, the mass percentage content of Al element is controlled between 0.01-0.03%.
  • the mass percentage content of the Al element can be preferably controlled between 0.01-0.025%.
  • N In the high-strength petroleum casing of the present invention, N can form TiN with Ti to refine the austenite grains, thereby inhibiting direct quenching cracking after rolling. Therefore, in the present invention, the mass percentage content of the N element is controlled to satisfy 0 ⁇ N ⁇ 0.008%.
  • both P and S elements are impurity elements in the steel pipe.
  • they should be used as much as possible in order to obtain pipes with better performance and better quality. Reduce the content of impurity elements in high-strength petroleum casing.
  • the content of P and S elements in the steel must be strictly controlled, and controlled to P ⁇ 0.015% and S ⁇ 0.008%.
  • the contents of P and S elements can be further controlled to satisfy: P ⁇ 0.013%, S ⁇ 0.0025%.
  • the mass percentage content of each chemical element further satisfies at least one of the following items:
  • the microstructure is tempered sorbite.
  • the grain size level of its structure is greater than 8.5.
  • the yield strength is ⁇ 552MPa
  • the tensile strength is ⁇ 689MPa
  • the elongation is ⁇ 20%
  • the 0°C transverse Charpy impact energy is ⁇ 80J.
  • the yield strength is ⁇ 630MPa
  • the tensile strength is ⁇ 720MPa
  • the elongation is ⁇ 20%
  • the 0°C transverse Charpy impact energy is ⁇ 80J.
  • the yield strength is 552-965MPa
  • the tensile strength is ⁇ 689MPa
  • the elongation is ⁇ 20%
  • the 0°C transverse Charpy impact energy is ⁇ 80J.
  • the yield strength of the high-strength petroleum casing in the present invention is 630-965MPa
  • the tensile strength is 720-1040MPa
  • the elongation is 21-26%
  • the 0°C transverse Charpy impact energy is 89-150J.
  • another object of the present invention is to provide the above-mentioned manufacturing method of high-strength petroleum casing.
  • This manufacturing method utilizes the waste heat of the hot-rolled steel pipe for quenching, realizing online quenching + tempering heat treatment production, which can reduce the While reducing manufacturing costs, the above-mentioned high-strength petroleum casing of the present invention can be effectively prepared, which has good application prospects.
  • the present invention proposes the above-mentioned manufacturing method of high-strength petroleum casing, which includes the steps:
  • Tempering the tempering temperature is controlled to be 500-620°C, and the holding time is 40-70 minutes;
  • the inventor proposes and utilizes the waste heat of the hot-rolled steel pipe for quenching to eliminate the offline quenching process and realize online quenching + tempering heat treatment. production, which can significantly improve production efficiency, reduce production costs, reduce energy consumption and achieve green manufacturing.
  • the process adopted in the present invention requires an optimized design of the alloy type and content to prevent cracks and stress concentration in the pipe body and ensure production safety and quality stability.
  • the inventor added La and Ce rare earth elements to the steel when designing the chemical composition to modify and refine the inclusions in the steel, remove larger inclusions, reduce the oxygen content, and improve the toughness index; at the same time, The refined inclusions serve as nucleation points for dynamic recrystallization during rolling, which promotes the formation of recrystallization, thereby refining the austenite grains and obtaining a structure with a grain size of not less than 8.5, which can inhibit the formation of recrystallization directly after rolling. Quenching cracking.
  • a small amount of Ti element can also be added, and the TiN compound formed can refine the austenite grains and inhibit direct quenching cracking after rolling.
  • a rare earth alloy is added in the VD (Vacuum Degassing) or LF (Ladle Furnace refining) process, and in the casting step, the superheat of the molten steel is controlled. 40°C or less, the continuous casting speed is 1.6 ⁇ 2.4m/min, preferably 1.8- 2.4m/min.
  • the superheat degree of molten steel is between 15°C and 40°C.
  • step (2) the round billet is soaked in a furnace at 1200-1290°C, and the piercing temperature is 1120-1240°C.
  • step (3) the final rolling temperature is controlled to be 920-1000°C.
  • step (4) the sizing temperature is controlled to be 840-910°C.
  • the waste heat of the pipe body is used to directly perform step (5) before cooling down.
  • step (7) the heat straightening temperature is controlled to be 400-520°C.
  • step (5) the temperature of the casing body before cooling is controlled to 780°C-910°C, and the final cooling temperature is controlled to 30-90°C.
  • step (6) the tempering temperature is controlled to be 520°C-600°C.
  • the high-strength petroleum casing and its manufacturing method of the present invention have the following advantages and beneficial effects:
  • the inventor proposes and utilizes the waste heat of hot-rolled steel pipes for quenching to eliminate the offline quenching process and realize online quenching + tempering heat treatment production, which can significantly improve production efficiency, reduce production costs, reduce energy consumption and achieve green manufacture.
  • the steel material obtains higher strength and better toughness by using TMCP technology.
  • the process is simple to operate, easy to realize large-scale production and manufacturing, and has good Economic benefits.
  • the 80-110ksi steel grade high-strength petroleum casing finally prepared by this manufacturing process has very excellent mechanical properties, with a yield strength of 552-965MPa, a tensile strength of ⁇ 689MPa, an elongation of ⁇ 20%, and a transverse direction of 0°C.
  • the Charpy impact energy is ⁇ 80J, which can meet the performance requirements of high-strength casing in oil and gas fields and has good application prospects.
  • Figure 1 is a photo of the metallographic structure of the high-strength petroleum casing in Example 4.
  • Figure 2 is a photo of the metallographic structure of the comparative steel pipe in Comparative Example 5.
  • Tempering the tempering temperature is controlled to be 500-620°C, and the holding time is 40-70min.
  • Heat straightening Control the heat straightening temperature to 400-520°C.
  • Table 1 lists the mass percentage of each chemical element in the high-strength petroleum casing of Examples 1-6 and the comparative steel pipe of Comparative Examples 1-7.
  • Table 2-1 and Table 2-2 list the specific process parameters used in the above manufacturing process steps for the high-strength petroleum casing of Examples 1-6 and the comparative steel pipe of Comparative Examples 1-7.
  • the controlled cooling process is not used in Comparative Example 7, but an offline heat treatment process is used, that is, tempering and heat preservation at 500°C for 60 minutes.
  • Tensile test Test according to ASTM A370 standard to obtain the yield strength, tensile strength and elongation values of the steel pipes in each example and comparative example at room temperature.
  • Table 3 lists the performance test results of the high-strength petroleum casings of Examples 1-6 and the comparative steel pipes of Comparative Examples 1-7.
  • the high-strength petroleum casings of Examples 1-6 obtained by the present invention all have excellent mechanical properties, with their yield strength ranging from 630-965MPa, and their tensile strength ranging from 720-1040MPa.
  • the ratio is between 21-26%, and the transverse Charpy impact energy at 0°C is between 89-150J, that is, the casings in Examples 1-6 all have high strength and high toughness properties.
  • Comparative Examples 1 and 2 In the chemical composition design of Comparative Examples 1 and 2, the C element content exceeded the range limited by the technical solution of the present invention, and the Mn element content of Comparative Examples 3 and 4 exceeded the technical solution limited by the present invention. Range, the rare earth (La, Ce) rare earth content in Comparative Examples 5 and 6 exceeds the range limited by the technical solution of the present invention. In Comparative Example 7, no controlled cooling process is used, but an offline heat treatment process (900°C insulation Quench with water after 40 minutes, temper at 550°C and keep for 60 minutes).
  • Figure 1 is a photo of the metallographic structure of the high-strength petroleum casing in Example 4.
  • Example 4 the microstructure of the high-strength petroleum casing prepared is tempered sorbite, and its grain size is 8.5. It can be seen that the added rare earths La and Ce can effectively refine the grains and improve the toughness of the material.
  • Figure 2 is a photo of the metallographic structure of the comparative steel pipe in Comparative Example 5.

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Abstract

本发明公开了一种高强度石油套管，其含有Fe和不可避免的杂质元素，其还含有质量百分含量如下的下述各化学元素：C：0.06-0.15％；Si：0.3-0.5％；Mn：1.5-2.2％；稀土(La，Ce)：0.002-0.006％；Ti≤0.05％；Al：0.01-0.03％；0＜N≤0.008％。相应地，本发明还公开了上述的高强度石油套管的制造方法，其包括步骤：(1)冶炼和铸造；(2)穿孔；(3)轧制；(4)定径；(5)在线淬火：控制冷却前套管管体温度不低于780℃，对套管外表面进行水冷，冷却速度为40-100℃/S，控制终冷温度不高于100℃；(6)回火；其中控制回火温度为500-620℃，保温时间为40-70min；(7)热矫直。

Description

一种高强度石油套管及其制造方法 技术领域
本发明涉及一种钢管及其制造方法，尤其涉及一种石油套管及其制造方法。
背景技术
近年来，无缝钢管已经广泛应用于油气、能源等领域中，并起到十分重要的作用，其被誉为“工业的血管”，是不可替代的重要钢材门类。
在现有技术中，常用的油气井用无缝管钢级有API标准的N80-Q、P110等牌号。发明人研究发现，这些套管在生产过程中均采用的是热轧+调质热处理工艺进行制备，其在热轧后还需进行室温冷却，而后再经过淬火加热炉重新加热进行淬火热处理。这种工艺不仅会造成钢管轧后余热的浪费(通常轧后钢管温度在900℃以上)，同时也多了一道次的热处理工序并且带来成本的增加，其资源能源消耗大，给高品质管材的开发及高效生产带来诸多限制。
因此，为了降低能耗，并提高钢材的强度，现有的板材也常采用控轧控冷工艺进行制备。但需要注意的是，无缝钢管由于其特殊的环形断面特点，相较于板材其内应力状态更为复杂，其在利用余热的在线淬火等控冷工艺时，很容易造成钢管开裂，并且由于轧制温度较高，钢管晶粒度较大，不利于强韧性的提升。
例如：公开号为CN103774063A，公开日为2014年5月7日，名称为“一种大口径石油套管及其TMCP生产方法”的中国专利文献公开了一种低碳当量微合金钢管及其在线常化工艺，其具备稳定的机械性能和良好的抗挤毁性能。该技术方案采用的是TMCP生产方法，其工艺简单，生产效率高，但是该专利采用中碳CrMo钢材质，与常规油井管材质类似，其在线淬火时仍然存在着开裂风险。
又例如：公开号为CN103757561A，公开号为2014年4月30日，名称为“一种大口径厚壁海洋用无缝钢管及其TMCP生产方法”的中国专利文献，公 开了一种大口径厚壁海洋用无缝钢管及其TMCP生产方法，其具备稳定的机械性能和良好的低温冲击性能，但是其较高的合金含量导致在线淬火存在着开裂风险。
因此，为了解决现有技术中所存在的这种问题，本发明期望开发并获得一种新的高强度石油套管及其制造方法。
发明内容
本发明的目的之一在于提供一种高强度石油套管，该高强度石油套管通过合理的成分匹配及工艺设计，可以获得优异的力学性能，其兼具有高强度、高韧性，其屈服强度为552-965MPa，抗拉强度≥689MPa，延伸率≥20％，0℃横向夏比冲击功≥80J，可以满足油气田对高强度套管性能的使用要求。
为了实现上述目的，本发明提供了一种高强度石油套管，其含有Fe和不可避免的杂质元素，其还含有质量百分含量如下的下述各化学元素：
C：0.06-0.15％；
Si：0.3-0.5％；
Mn：1.5-2.2％；
La+Ce：0.002-0.006％；
Ti≤0.05％；
Al：0.01-0.03％；
0＜N≤0.008％。
进一步地，在本发明所述的高强度石油套管中，其各化学元素质量百分比为：
C：0.06-0.15％；
Si：0.3-0.5％；
Mn：1.5-2.2％；
La+Ce：0.002-0.006％；
Ti≤0.05％；
Al：0.01-0.03％；
0＜N≤0.008％；
余量为Fe和不可避免的杂质；
优选地，La+Ce：0.002-0.005％。
在本发明所述的高强度石油套管中，各化学元素的设计原理如下所述：
C：在本发明所述的高强度石油套管中，C是碳化物形成元素，其可以提高钢的强度。当钢中C元素含量低于0.06％时，会使得钢材的淬透性降低，从而降低钢的韧性；然而，当钢中C元素含量高于0.15％时，则又会显著地恶化钢的偏析，易产生淬火裂纹。因此，考虑到C元素含量对钢材性能的影响，为了达到石油套管的高强度的要求，在本发明所述的高强度石油套管中，将C元素的质量百分含量控制在0.06-0.15％之间。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将C元素的质量百分含量控制在0.08-0.14％之间。
Si：在本发明所述的高强度石油套管中，Si元素能够固溶于铁素体，其可以提高钢材的屈服强度。此外，Si同时也是铁素体形成元素，其有利于提高钢材的韧性。需要注意的是，钢中Si元素含量不宜过低，当Si元素含量低于0.3％时，会使得石油套管容易氧化；同时钢中Si元素的添加量也不宜过高，太高含量的Si元素会恶化钢材的加工性能和韧性。因此，为了发挥Si元素的有益效果，必须严格控制钢中Si元素含量，在本发明所述的高强度石油套管中，将Si元素的质量百分含量控制在0.3-0.5％之间。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将Si元素的质量百分含量控制在0.3-0.45％之间。
Mn：在本发明所述的高强度石油套管中，Mn为奥氏体的形成元素，其可以提高钢材的淬透性。在本发明所设计的这种钢材体系中，当Mn元素含量小于1.5％时，钢材的淬透性会显著降低，从而降低钢中马氏体的比例，降低钢的韧性；而当钢中Mn含量大于2.2％时，则易产生成分偏析，产生淬火裂纹。因此，考虑到Mn元素含量对于钢材性能的影响，在本发明所述的高强度石油套管中，将Mn元素的质量百分含量控制在1.5-2.2％之间。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将Mn元素的质量百分含量控制在1.6-2.0％之间。
稀土(La、Ce)：在本发明所述的高强度石油套管中，Ce和La均为稀土元素，钢中添加一定比例的稀土混合物，可对钢中夹杂物进行改性并细化，所形成的稀土改性产物为REAlO3，其能够去除较大的夹杂物，降低氧含量，提高 钢材的韧性指标。同时，细化的夹杂物作为轧制时动态再结晶的形核质点，还能够促进再结晶的形成，从而细化了奥氏体晶粒，可以抑制轧后直接淬火开裂。发明人研究发现，当钢中Ce+La量＞0.006％时，则容易形成粗大的夹杂物，这样会降低材料的韧性；若钢中Ce+La含量＜0.002％，则细化晶粒和改性夹杂物效果不显著，易产生淬火开裂。因此，为了发挥La、Ce稀土元素的有益效果，在本发明所述的高强度石油套管中，将La和Ce元素含量的和“稀土(La，Ce)”控制在0.002-0.006％之间。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将稀土元素La和Ce的含量控制在0.0025-0.004％之间。
Ti：在本发明所述的高强度石油套管中，Ti是强碳氮化物的形成元素，其能够显著地细化钢中奥氏体晶粒，可以弥补因碳含量降低而引起的强度下降。当钢中Ti元素含量大于0.05％时，则容易形成粗大的TiN，这样会降低材料的韧性。因此，在本发明所述的高强度石油套管中，需要将Ti元素的质量百分含量控制为Ti≤0.05％。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将Ti元素的质量百分含量控制为Ti≤0.03％。
Al：在本发明所述的高强度石油套管中，Al是良好的脱氧固氮元素，其可以有效细化晶粒。因此，为发挥Al元素的有益效果，在本发明中，将Al元素的质量百分含量控制在0.01-0.03％之间。
当然，在一些优选的实施方式中，为了获得更优的实施效果，可以优选地将Al元素的质量百分含量控制在0.01-0.025％之间。
N：在本发明所述的高强度石油套管中，N可以与Ti形成TiN，细化奥氏体晶粒，从而抑制轧后直接淬火开裂。因此，在本发明中，将N元素的质量百分含量控制满足0＜N≤0.008％。
进一步地，在本发明所述的高强度石油套管中，在不可避免的杂质中，P≤0.015％，S≤0.008％。
进一步地，在本发明所述的高强度石油套管中，在不可避免的杂质中，P≤0.013％，S≤0.0025％。
在本发明所述的高强度石油套管中，P元素和S元素均为钢管中的杂质元素，在技术条件允许情况下，为了获得性能更好且质量更优的管材，应尽可能 降低高强度石油套管中杂质元素的含量。
因此，在本发明中，必须严格地控制钢中P、S元素的含量，并控制为P≤0.015％，S≤0.008％。当然，在一些优选的实施方式中，为了获得更优的实施效果，可以进一步控制P、S元素的含量满足：P≤0.013％，S≤0.0025％。
进一步地，在本发明所述的高强度石油套管中，其各化学元素质量百分含量进一步满足下述各项的至少其中之一：
C：0.08-0.14％；
Si：0.3-0.45％；
Mn：1.6-2.0％；
La+Ce：0.0025-0.004％；
Ti≤0.03％；
Al：0.01-0.025％。
进一步地，在本发明所述的高强度石油套管中，其微观组织为回火索氏体。
进一步地，在本发明所述的高强度石油套管中，其组织的晶粒度级别大于8.5级。
进一步地，在本发明所述的高强度石油套管中，其屈服强度≥552MPa，抗拉强度≥689MPa，延伸率≥20％，0℃横向夏比冲击功≥80J。
进一步地，在本发明所述的高强度石油套管中，其屈服强度≥630MPa，抗拉强度≥720MPa，延伸率≥20％，0℃横向夏比冲击功≥80J。
进一步地，在本发明所述的高强度石油套管中，其屈服强度为552-965MPa，抗拉强度≥689MPa，延伸率≥20％，0℃横向夏比冲击功≥80J。
进一步地，在本发明所述的高强度石油套管的屈服强度为630-965MPa，抗拉强度为720-1040MPa，延伸率为21-26％，0℃横向夏比冲击功为89-150J。
相应地，本发明的另一目的在于提供上述的高强度石油套管的制造方法，该制造方法利用了热轧后的钢管余热进行淬火，实现了在线淬火+回火热处理生产，其可以在降低制造成本的同时，有效制备本发明上述的高强度石油套管，其具有良好的应用前景。
为了实现上述目的，本发明提出了上述的高强度石油套管的制造方法，其包括步骤：
(1)冶炼和铸造；
(2)穿孔；
(3)轧制；
(4)定径；
(5)在线淬火：控制冷却前套管管体温度不低于780℃，对套管外表面进行水冷，冷却速度为40-100℃/S，控制终冷温度不高于100℃；
(6)回火；其中控制回火温度为500-620℃，保温时间为40-70min；
(7)热矫直。
在现有技术中，常规的高强度套管通常采用离线淬火+回火热处理的工艺进行制备，其在热轧后需进行室温冷却，而后经过淬火加热炉重新加热进行淬火热处理。这种针对无缝钢管的处理工艺不仅造成了钢管轧后余热的浪费，同时也多了一道次的热处理工序，并且会带来成本的增加，其资源消耗大，给高品质管材的开发及高效生产带来诸多限制。
不同于现有技术，在本发明所述的高强度石油套管的制造方法中，发明人提出并利用了热轧后的钢管余热进行淬火，以去除离线淬火工序，实现在线淬火+回火热处理生产，进而可以显著提高生产效率降低生产成本，降低能耗实现绿色制造。
但需要注意的是，套管在热轧后直接淬火时因晶粒畸变储存了较高的能量，其在淬火过程中易发生开裂；同时，由于套管的轧制温度较高，轧后套管的晶粒度较大，一般在5-7级，容易产生淬火开裂。因此，本发明所采用的此种工艺需要对合金种类及含量进行优化设计，以防止管体裂纹和应力集中，保证生产的安全和质量的稳定。为此，发明人在化学成分设计时，在钢中加入La和Ce稀土元素，对钢中夹杂物进行改性并细化，去除较大的夹杂物，降低氧含量，提高韧性指标；同时，细化的夹杂物作为轧制时动态再结晶的形核质点促进了再结晶的形成，从而可以细化奥氏体晶粒，得到晶粒度不低于8.5级的组织，可以抑制轧后直接淬火开裂。
另外，在本发明所设计的这种高强度石油套管中，还可加入少量的Ti元素，并依靠形成的TiN化合物，细化奥氏体晶粒，抑制轧后直接淬火开裂。
进一步地，在本发明所述的制造方法中，在步骤(1)的冶炼步骤中，在VD(Vacuum Degassing)或LF(Ladle Furnace refining)工序加入稀土合金，在铸造步骤中，控制钢水过热度小于等于40℃，连铸拉速为1.6～2.4m/min，优选1.8- 2.4m/min。优选地，钢水过热度在15～40℃之间。
进一步地，在本发明所述的制造方法中，在步骤(2)中，圆坯在1200-1290℃的炉内均热，穿孔温度为1120-1240℃。
进一步地，在本发明所述的制造方法中，在步骤(3)中，控制终轧温度为920-1000℃。
进一步地，在本发明所述的制造方法中，在步骤(4)中，控制定径温度为840-910℃。优选地，步骤(4)完成后，在降温前利用管体的余热直接进行步骤(5)。
进一步地，在本发明所述的制造方法中，在步骤(7)中，控制热矫直温度为400-520℃。
进一步地，在步骤(5)中，控制冷却前套管管体温度为780℃-910℃，控制终冷温度为30-90℃。
进一步地，在步骤(6)中，控制回火温度为520℃-600℃。
相较于现有技术，本发明所述的高强度石油套管及其制造方法具有如下所述的优点以及有益效果：
在本发明中，发明人提出并利用了热轧后的钢管余热进行淬火，以去除离线淬火工序，实现在线淬火+回火热处理生产，进而可以显著提高生产效率降低生产成本，降低能耗实现绿色制造。
在本发明所述的高强度石油套管的制造方法中，其通过采用TMCP技术使得钢材获得较高的强度和较好的韧性，其过程操作简单，易于实现大规模的生产制造，具有良好的经济效益。采用这种制造工艺最终所制备的80-110ksi钢级的高强度石油套管具有十分优异的力学性能，其屈服强度为552-965MPa，抗拉强度≥689MPa，延伸率≥20％，0℃横向夏比冲击功≥80J，可以满足油气田对高强度套管性能的使用要求，具有良好的应用前景。
附图说明
图1为实施例4的高强度石油套管的金相组织照片。
图2为对比例5的对比钢管的金相组织照片。
具体实施方式
下面将结合说明书附图和具体的实施例对本发明所述的高强度石油套管及其制造方法做进一步的解释和说明，然而该解释和说明并不对本发明的技术方案构成不当限定。
实施例1-6和对比例1-7
本发明所述实施例1-6的高强度石油套管和对比例1-7的对比钢管均采用以下步骤制得：
(1)按照表1所示的化学元素的质量百分配比进行冶炼和铸造：在冶炼过程中，控制实施例1-6的高强度石油套管和对比例1-7的对比钢管中的各化学元素的质量百分配比如表1所示，并在VD或LF工序加入稀土合金；冶炼完成后再连铸制成管坯，并控制钢水过热度低于40℃，连铸拉速为1.8-2.4m/min。
(2)穿孔：将经过连铸获得的圆坯在1200-1290℃的环形炉内均热，并控制穿孔温度为1120-1240℃。
(3)轧制：控制终轧温度为920-1000℃。
(4)定径：控制定径温度为840-910℃。
(5)在线淬火：控制冷却前套管管体温度不低于780℃，对套管外表面进行水冷，冷却速度为40-100℃/S，控制终冷温度不高于100℃。
(6)回火；其中控制回火温度为500-620℃，保温时间为40-70min。
(7)热矫直：控制热矫直温度为400-520℃。
需要说明的是，本发明所述实施例1-6的高强度石油套管的化学元素成分和相关工艺设计均满足本发明设计规范要求。而对比例1-7的对比钢管虽然也采用上述工艺步骤制得，但其化学元素成分和/或相关工艺参数存在不符合本发明设计的参数。
表1列出了实施例1-6的高强度石油套管和对比例1-7的对比钢管中各化学元素质量百分比。
表1.(余量为Fe和除P、S外其他的不可避免的杂质)

注：在上述表1之中并未单独列出La、Ce各自的含量是因为稀土属于混合物，无法精确确定La和Ce的单独含量。
表2-1和表2-2列出了实施例1-6的高强度石油套管和对比例1-7的对比钢管在上述制造工艺步骤中所采用的具体工艺参数。
表2-1.
表2-2.

在上述实施条例和对比例中，对比例7中未采用控冷工艺，其采用的是离线热处理工艺，即在500℃回火保温60min。
将制备的成品实施例1-6的高强度石油套管和对比例1-7的对比钢管分别取样，并对各实施条例和对比例的钢管进行各项性能测试，所得的测试结果列于表3中。
相关性能检测手段如下所述：
(1)拉伸试验：按照ASTMA370标准测试，以获得各实施例和对比例的钢管在室温下的屈服强度、抗拉强度和延伸率数值。
(2)冲击试验：按照ASTM E23标准测试，以获得各实施例和对比例的钢管在0℃下的横向冲击韧性。
表3列出了实施例1-6的高强度石油套管和对比例1-7的对比钢管的性能测试结果。
表3.

由表3可以看出，相较于对比例1-7的对比钢管，本发明所述实施例1-6的高强度石油套管的综合性能明显更优。
参阅表3可知，本发明所获得的实施例1-6的高强度石油套管均具有优异的力学性能，其屈服强度在630-965MPa之间，其抗拉强度在720-1040MPa之间，延伸率在21-26％之间，其在0℃的横向夏比冲击功在89-150J之间，即实施例1-6中的套管均具有高强度和高韧性性能。
而对比例1和对比例2在化学成分设计时，C元素含量超出了本发明的技术方案所限定的范围，对比例3和对比例4的Mn元素含量超出了本发明的技术方案所限定的范围，对比例5和6中的稀土(La，Ce)稀土含量超出了本发明的技术方案所限定的范围，对比例7中未采用控冷工艺，其采用的是离线热处理工艺(900℃保温40min后水淬，550℃回火保温60min)。
这种设计使得对比例1-6所制备的对比钢管的至少一项力学性能并未能达到本专利提出的高强度、高韧性的要求。
图1为实施例4的高强度石油套管的金相组织照片。
如图1所示，在实施例4中，其所制备的高强度石油套管的微观组织为回火索氏体，且其晶粒度为8.5级。由此可见，加入的稀土La和Ce能够有效细化晶粒，提高材料的韧性。
图2为对比例5的对比钢管的金相组织照片。
如图2所示，在对比例5所制备的对比钢管中，其晶粒度为7级，稀土含量小于本发明所设定的下限值，无明显晶粒细化效果，材料韧性降低。
上述晶粒度级别依照GB/T 6394-2017标准测定。
需要说明的是，本案中各技术特征的组合方式并不限本案权利要求中所记载的组合方式或是具体实施例所记载的组合方式，本案记载的所有技术特征可以以任何方式进行自由组合或结合，除非相互之间产生矛盾。
还需要注意的是，以上所列举的实施例仅为本发明的具体实施例。显然本发明不局限于以上实施例，随之做出的类似变化或变形是本领域技术人员能从本发明公开的内容直接得出或者很容易便联想到的，均应属于本发明的保护范围。

Claims (15)

  1. 一种高强度石油套管，其含有Fe和不可避免的杂质元素，其特征在于，其还含有质量百分含量如下的下述各化学元素：
    C：0.06-0.15％；
    Si：0.3-0.5％；
    Mn：1.5-2.2％；
    La+Ce：0.002-0.006％；
    Ti≤0.05％；
    Al：0.01-0.03％；
    0＜N≤0.008％。
  2. 如权利要求1所述的高强度石油套管，其特征在于，其各化学元素质量百分比为：
    C：0.06-0.15％；
    Si：0.3-0.5％；
    Mn：1.5-2.2％；
    La+Ce：0.002-0.006％；
    Ti≤0.05％；
    Al：0.01-0.03％；
    0＜N≤0.008％；
    余量为Fe和不可避免的杂质；
    优选地，La+Ce：0.002-0.005％。
  3. 如权利要求1或2所述的高强度石油套管，其特征在于，在不可避免的杂质中，P≤0.015％，S≤0.008％。
  4. 如权利要求3所述的高强度石油套管，其特征在于，在不可避免的杂质中，P≤0.013％，S≤0.0025％。
  5. 如权利要求1或2所述的高强度石油套管，其特征在于，其各化学元素质量百分含量进一步满足下述各项的至少其中之一：
    C：0.08-0.14％；
    Si：0.3-0.45％；
    Mn：1.6-2.0％；
    La+Ce：0.0025-0.004％；
    Ti≤0.03％；
    Al：0.01-0.025％。
  6. 如权利要求1或2所述的高强度石油套管，其特征在于，其微观组织为回火索氏体。
  7. 如权利要求6所述的高强度石油套管，其特征在于，其晶粒度的级别大于等于8.5级。
  8. 如权利要求1或2所述的高强度石油套管，其特征在于，其屈服强度≥552MPa，抗拉强度≥689MPa，延伸率≥20％，0℃横向夏比冲击功≥80J；优选地，其屈服强度为630-965MPa，抗拉强度为720-1040MPa，延伸率为21-26％，0℃横向夏比冲击功为89-150J。
  9. 一种如权利要求1-8中任意一项所述的高强度石油套管的制造方法，其特征在于，包括步骤：
    (1)冶炼和铸造；
    (2)穿孔；
    (3)轧制；
    (4)定径；
    (5)在线淬火：控制冷却前套管管体温度不低于780℃，对套管外表面进行水冷，冷却速度为40-100℃/S，控制终冷温度不高于100℃；
    (6)回火；其中控制回火温度为500-620℃，保温时间为40-70min；
    (7)热矫直。
  10. 如权利要求9所述的制造方法，其特征在于，在步骤(1)的冶炼步骤中，在VD或LF工序加入稀土合金，在铸造步骤中，控制钢水过热度低于40℃，优选为15～40℃，连铸拉速为1.6-2.4m/min。
  11. 如权利要求9所述的制造方法，其特征在于，在步骤(2)中，圆坯在1200-1290℃的炉内均热，穿孔温度为1120-1240℃。
  12. 如权利要求9所述的制造方法，其特征在于，在步骤(3)中，控制终轧温度为920-1000℃。
  13. 如权利要求9所述的制造方法，其特征在于，在步骤(4)中，控制定径温度为840-910℃；优选地，步骤(4)完成后，在降温前利用管体的余热直接进行步骤(5)。
  14. 如权利要求9所述的制造方法，其特征在于，在步骤(7)中，控制热矫直温度为400-520℃。
  15. 如权利要求9所述的制造方法，其特征在于，在步骤(5)中，控制冷却前套管管体温度为780℃-910℃，控制终冷温度为30-90℃；在步骤(6)中，控制回火温度为520℃-600℃。
PCT/CN2023/096906 2022-05-30 2023-05-29 一种高强度石油套管及其制造方法 Ceased WO2023231981A1 (zh)

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