CN116145051A - High-corrosion-resistance economic oil well pipe steel and preparation method thereof - Google Patents

High-corrosion-resistance economic oil well pipe steel and preparation method thereof Download PDF

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CN116145051A
CN116145051A CN202211593652.1A CN202211593652A CN116145051A CN 116145051 A CN116145051 A CN 116145051A CN 202211593652 A CN202211593652 A CN 202211593652A CN 116145051 A CN116145051 A CN 116145051A
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oil well
well pipe
steel
percent
corrosion resistant
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宋志刚
丰涵
何建国
朱玉亮
郑文杰
王宝顺
钱炯
王曼
潘平伟
苏诚
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Central Iron and Steel Research Institute
Zhejiang Jiuli Hi Tech Metals Co Ltd
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Central Iron and Steel Research Institute
Zhejiang Jiuli Hi Tech Metals Co Ltd
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Priority to CN202211593652.1A priority Critical patent/CN116145051A/en
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Priority to PCT/CN2023/137477 priority patent/WO2024125407A1/en
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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
    • C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B39/00—Arrangements for moving, supporting, or positioning work, or controlling its movement, combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • 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
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • 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
    • C22C38/02—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
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention discloses high-corrosion-resistance economic oil well pipe steel and a preparation method thereof, belongs to the technical field of corrosion-resistance steel, and solves the problems of high alloy element content and high cost of the oil well pipe steel in the prior art. The high corrosion resistant economic oil well pipe steel comprises the following components in percentage by mass: c: less than or equal to 0.03 percent, cr:17.3% -18.4%, mo:0.5 to 2.0 percent of Ni:1.0 to 2.8 percent of Mn:1.0% -3.5%, si:0.1% -0.5%, N:0.1% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities. The oil well pipe steel has high strength, good plasticity and toughness, and excellent corrosion resistance.

Description

High-corrosion-resistance economic oil well pipe steel and preparation method thereof
Technical Field
The invention relates to the technical field of corrosion-resistant steel, in particular to high corrosion-resistant economic oil well pipe steel and a preparation method thereof.
Background
The oil well pipe is an important consumable in the petroleum and natural gas exploration and development process, accounts for about 40% of the total steel for the oil and gas industry, and is an important component in petroleum and natural gas exploitation equipment. As an important petroleum equipment material, the oil well pipe accounts for 20% -30% of the total well construction cost on average. Therefore, the whole petroleum engineering can be smoothly carried out, and the petroleum engineering is indistinguishable from the quality of oil well pipes. The oil well pipe is arranged in the casing pipe and is used for collecting oil and gas. Because of the flow of corrosive liquid in the oil well pipe, various corrosion resistant products are selected according to the corrosion condition. In China, sichuan gas field contains H 2 S, sichuan, north China and Western oil and gas fields some oil and gas wells contain CO 2 H and H 2 S、CO 2 、C1 - And coexist. Under such oil recovery conditions, higher demands are also put on the corrosion resistance properties of the oil well pipe. At presentCO resistance 2 The material for corroded oil well pipe is mainly 13Cr martensitic stainless steel, but martensitic steel cannot contain H 2 S environmental use. Although the use requirement of oil well pipes can be met by selecting the 22Cr (or 25Cr, 27Cr, with higher Cr content and better corrosion resistance) duplex stainless steel with higher alloy content, the material cost is high, and the method is not suitable for large-batch industrial application in oil and gas exploitation scenes. Aiming at the actual conditions of Chinese oil and gas exploitation and mineral resource limitation, the development of economic high corrosion resistant oil well pipe materials is imperative.
At present, various oil well pipe steel with good comprehensive performance and corresponding technological processes at home and abroad have a lot of patents, but most of the problems of overhigh cost or complex process exist, and the requirements of mass production and practical application cannot be met.
Disclosure of Invention
In view of the above, the invention aims to provide the high corrosion-resistant economic oil well pipe steel and the preparation method thereof, which are used for solving the problems of higher alloy element content and higher cost of the existing oil well pipe steel.
The aim of the invention is mainly realized by the following technical scheme:
on one hand, the invention provides high corrosion-resistant economic oil well pipe steel, which comprises the following components in percentage by mass: c: less than or equal to 0.03 percent, cr:17.3% -18.4%, mo:0.5 to 2.0 percent of Ni:1.0 to 2.8 percent of Mn:1.0% -3.5%, si:0.1% -0.5%, N:0.1% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities.
In one possible design, cr+3.3Mo+16N is greater than or equal to 26 in the composition of the high corrosion resistant economic oil well pipe steel.
In one possible design, 60Ni+17Mn-12Mo-800N is less than or equal to 0 in the components of the high corrosion resistant economic oil well pipe steel.
In one possible design, the high corrosion resistant economic oil well pipe steel may have the following composition in mass percent: c:0.01% -0.03%, cr:17.4% -18.4%, mo:1.0% -2.0%, ni:1.0 to 2.7 percent of Mn:1.4 to 3.2 percent of Si:0.1% -0.5%, N:0.13% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities.
In one possible design, the microstructure of the highly corrosion resistant economical oil well pipe steel is a mixed structure of ferrite + austenite + martensite.
In one possible design, the high corrosion resistant economic oil well pipe steel microstructure has austenite in the volume percent of 20-40% and martensite in the volume percent of 10-40%.
In one possible design, the austenitic grain size is < 3 μm in the microstructure of the highly corrosion resistant economical oil well pipe steel.
On the other hand, the invention also provides a preparation method of the high corrosion-resistant economic oil well pipe steel, which is used for preparing the high corrosion-resistant economic oil well pipe steel and comprises the following steps:
step 1: smelting a metal raw material into molten steel;
step 2: smelting molten steel into a continuous casting blank or an ingot by adopting a continuous casting or die casting method;
step 3: forging and cogging a continuous casting blank or an ingot to prepare a forging blank;
step 4: rolling the forging stock into a tube blank, and controlling the technological parameters of hot rolling and cooling to obtain the high corrosion resistant economic oil well tube steel.
In one possible design, in step 3, the forging cogging temperature is 1150-1250 ℃.
In one possible design, in step 4, controlling hot rolling and cooling process parameters includes: the initial rolling temperature is controlled to be higher than 1050 ℃, the final rolling temperature is controlled to be higher than 950 ℃, the deformation of the first rolling pass is not higher than 30%, and the deformation of the final rolling pass is not higher than 50%.
Compared with the prior art, the invention has the following beneficial effects:
a) The high corrosion resistant economic oil well pipe steel of the invention precisely controls the mass percent of Cr, ni, mn, mo, N element in the steel, and can obtain the mixed structure of ferrite, austenite and martensite by combining the thermal deformation process of rolling control and cooling control, thereby greatly improving the corrosion resistance and strength of the oil well pipe steel. Due to the superfine martensite in the 17Cr material of the present inventionThe tensile strength of the material is superior to that of the duplex stainless steel with higher Cr content, and the high strength is obtained by using lower Cr content. Compared with the martensitic stainless steel in the prior art, the stainless steel of the invention introduces ferrite and austenite to obtain better intergranular corrosion resistance and H resistance 2 S stress corrosion performance. The austenitic stainless steel of the invention has the austenitic content far higher than that of martensitic stainless steel, and the martensitic stainless steel is difficult to obtain the austenitic with the austenitic content more than 20 percent, so that the material of the invention has better hydrogen embrittlement resistance.
b) The steel of the invention not only ensures high strength, good ductility and toughness and excellent corrosion resistance, but also ensures that the yield strength of the steel of the invention is more than 600MPa (for example, 601-648 MPa), the tensile strength is more than 910MPa (for example, 911-1010 MPa), and the elongation is more than 22% (for example, 23-24%). (180 ℃ C.) CO 2 Corrosion rate of 0.028g/m 2 h is less than or equal to (e.g., 0.0203-0.0275 g/m) 2 h)；(200℃)CO 2 Corrosion rate of 0.1g/m 2 h is less than or equal to (e.g., 0.078 to 0.099 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the Pitting corrosion rate 2.5g/m 2 h is less than or equal to (e.g., 1.693-2.433 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the The crevice corrosion rate was 5.9g/m 2 h is less than or equal to (for example, 3.303-5.852 g/m) 2 h)；H 2 The S stress corrosion test is passed.
c) The steel has good toughness and excellent corrosion resistance, and has the high strength of the super martensitic stainless steel oil well pipe material and the stress corrosion resistance, the intergranular corrosion resistance and the small amount of H resistance of the duplex stainless steel 2 S stress corrosion capability. Because the Cr and Ni contents of the steel are low, the raw material cost is equivalent to or even slightly lower than that of the super 13Cr martensitic stainless steel in the prior art, and the hot workability is good, the steel has low comprehensive cost, economy and practicability.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims thereof as well as the appended drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, like reference numerals being used to refer to like parts throughout the several views.
FIG. 1 is a microstructure view of the steel of example 1 of the present invention after hot rolling;
FIG. 2 is a transmission electron microscope image at M in FIG. 1 according to the present invention;
FIG. 3 is a microstructure view of the steel of example 2 of the present invention;
FIG. 4 is a microstructure of the steel of example 3 of the present invention;
FIG. 5 is a microstructure of the steel of example 4 of the present invention;
FIG. 6 is a photograph of a hot rolled sheet of example 1 of the present invention.
Detailed Description
Preferred embodiments of the present invention are described in detail below with reference to the attached drawing figures, which form a part of the present application and, together with the embodiments of the present invention, serve to explain the principles of the invention.
The invention provides high corrosion-resistant economic oil well pipe steel, which comprises the following components in percentage by mass: c: less than or equal to 0.03 percent, cr:17.3% -18.4%, mo:0.5 to 2.0 percent of Ni:1.0 to 2.8 percent of Mn:1.0% -3.5%, si:0.1% -0.5%, N:0.1% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities.
Specifically, cr+3.3Mo+16N (namely PREN) is more than or equal to 26, and 60Ni+17Mn-12Mo-800N is less than or equal to 0; wherein Cr, mo, N, ni, mn refers to the mass percent of these elements x 100. For example, the mass percentage of Cr element is 18.4%, and Cr is 18.4 here.
The following is a specific description of the action and the selection of the amounts of the components contained in the invention:
c: although the addition of carbon can obviously improve the hardness and strength of steel, the carbon is easy to combine with Cr to form M due to the high diffusion capability of carbon element 23 C 6 Carbide of the type which precipitates rapidly (not more than 0.5 hours) mainly in the temperature range of 700 to 900 ℃ or for a longer period of time at 550 to 700 DEG CAnd separating out during heat preservation. The precipitation of carbide causes partial lean Cr, increases the intergranular corrosion sensitivity of the material and worsens the corrosion resistance, so the comprehensive effect of strength and corrosion resistance is comprehensively considered, and the content of the carbide is controlled to be less than or equal to 0.03 percent.
Cr: the main elements of the corrosion resistance of the stainless steel are ensured, meanwhile, the main elements are ferrite forming elements, the ferrite content in the structure can be increased due to improper control of the Cr content, the strength is reduced, and the content of the ferrite is comprehensively considered to be controlled to be 17.3% -18.4%.
Ni: ni is an element which strongly forms and stabilizes austenite and enlarges an austenite phase region, ni is an element which improves the toughness and the corrosion resistance of a reducing medium of stainless steel, and Ni is an important element which improves the corrosion resistance of the austenite phase to various medium through crystal type stress, meanwhile, compared with Mn element, ni element can reduce the cold work hardening tendency of the austenite phase, and the content of the Ni element is controlled to be 1.0-2.8 percent under the condition of considering cost control.
Mn: the invention can improve the solubility of N in steel and inhibit precipitation of chromium nitride as a harmful phase, but Mn reduces the toughness of stainless steel, compared with Ni, mn is an economic austenite forming element, and Mn is different from the hardening effect of the austenitic phase of stainless steel and the whole material, so the content of Mn is controlled to be 1.0-3.5%.
Mo: besides improving the corrosion resistance of stainless steel in an oxidation medium, the alloy has good effect on improving the corrosion resistance of the stainless steel in a reducing medium, and meanwhile, in order to ensure the pitting corrosion resistance, alloy elements such as Cr, mo and the like for improving the PREN value are not too low, and meanwhile, the alloy cost control and phase balance are also required to be considered, and the content of the alloy is controlled to be 0.5% -2.0% by comprehensive consideration.
Si: the deoxidizer is added in the smelting process, so that the deoxidizer can play a role in deoxidizing, and the excessive addition can deteriorate the intergranular corrosion resistance of the material. The content of the invention is controlled to be 0.1-0.5%.
N: like Ni, N is an element that strongly forms and stabilizes austenite and enlarges the austenite phase region, and N can also significantly improve the pitting corrosion resistance of the austenite phase in stainless steel, thereby improving the pitting corrosion resistance of the stainless steel as a whole, and in some media, N has a good effect on the stress resistance of stainless steel, and there is an optimum value, further improving the N content, and its stress corrosion resistance is reduced. N is an economic alloy element at the same time, but N reduces the hot workability of stainless steel, so the content of the alloy is controlled to be 0.1-0.25%.
S: the hot workability of the steel is obviously reduced, mnS inclusions are easily generated by reaction with Mn, and the pitting corrosion resistance and the crevice corrosion resistance of the material are reduced. So the content is controlled to be less than or equal to 0.01 percent.
P: belongs to harmful impurity elements, not only can deteriorate the plasticity of the material, but also can reduce the corrosion resistance of the material, so the content of the material is controlled to be less than or equal to 0.03 percent.
Specifically, in the invention, 3 aspects of ensuring corrosion resistance, raw material cost caused by alloy element matching, precipitation of harmful phases caused by alloy element matching, cost change caused by hot working yield and the like are comprehensively considered, besides the control of the content of a single element of main alloy element Cr, ni, mn, N in steel, cr+3.3Mo+16N is more than or equal to 26, the highest precipitation temperature of the harmful phases is lower than 750 ℃ to ensure that the material has good hot working performance, and simultaneously, the three-phase proportion is considered to be controllable in the hot working process between 900 ℃ and 1180 ℃, and the content of Ni, mn, mo, N elements is required to be controlled to satisfy: 60Ni+17Mn-12Mo-800N is less than or equal to 0.
In order to further improve the comprehensive performance of the high corrosion resistant economic oil well pipe steel, the high corrosion resistant economic oil well pipe steel comprises the following components in percentage by mass: c:0.01% -0.03%, cr:17.4% -18.4%, mo:1.0% -2.0%, ni:1.0 to 2.7 percent of Mn:1.4 to 3.2 percent of Si:0.1% -0.5%, N:0.13% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities. Wherein Cr+3.3Mo+16N (namely PREN) is 26.1-27.8, and 60Ni+17Mn-12Mo-800N is less than or equal to-0.42.
Specifically, the microstructure of the high corrosion resistant economic oil well pipe steel is a mixed structure of ferrite, austenite and martensite, wherein the volume percentage of austenite is 20% -40% (for example, 20% -35%), the volume percentage of martensite is 10% -40% (for example, 30% -40%), the martensite is dispersed in the austenite in an ultrafine flake form, and the martensite is alternately laminated with the austenite and mutually divided, so that the austenite has smaller grain size (for example, the grain size of the austenite is less than 3 mu m), and the thickness of the martensite sheet is less than 100nm.
Compared with the prior art, the high corrosion-resistant economic oil well pipe steel is of a three-phase structure, has the characteristics of low Cr and low alloy element content and higher strength, can simultaneously have the characteristics of high strength, intergranular corrosion resistance, stress corrosion resistance, high toughness, good welding performance and the like, and has excellent comprehensive performance. Meanwhile, the martensite austenitic composite structure can improve the interface density in the structure, so that the high-strength mechanical property superior to that of the traditional duplex stainless steel is obtained. The balanced phase ratio of the hot working temperature range (900-1180 ℃) brings excellent hot working performance, and the multiphase composite structure form after hot working has better corrosion resistance than single-phase martensitic stainless steel while ensuring certain cold working performance.
The invention also provides a preparation method of the high corrosion-resistant economic oil well pipe steel, which comprises the following steps:
step 1: smelting a metal raw material into molten steel;
step 2: smelting molten steel into a continuous casting blank or an ingot by adopting a continuous casting or die casting method;
step 3: heating a continuous casting blank or an ingot at 1150-1250 ℃ to forge and cogge the continuous casting blank or the ingot to prepare a forging blank;
step 4: the forging stock is heated at 1050-1250 ℃ and rolled into a tube blank, and the high corrosion resistant economic oil well tube steel is obtained by controlling the hot rolling and cooling process parameters. The three-phase structure content of the high corrosion-resistant economic oil well pipe steel is as follows: 10-40% of martensite, 20-40% of austenite and the balance of ferrite.
Specifically, in the step 1 and the step 2, a converter or an electric furnace is adopted for smelting, LF refining and casting into a casting blank.
Specifically, in the step 3, the forging cogging temperature is 1150-1250 ℃, because the material of the invention is ferrite and austenite two phases at the temperature higher than 800 ℃, the ratio of the ferrite and austenite two phases changes along with the heating temperature, and the higher the heating temperature is, the more the ferrite content is, and the corresponding austenite content is reduced. The temperature range is selected for heating, meanwhile, the sufficient redissolution of harmful precipitated phases is ensured, the ferrite phase content in the material is also more than 70%, the steel is forged and cogged in a single-phase region with better thermoplasticity, and forging cracking caused by inconsistent deformation of two phases in the forging process due to different heat deformation capacities of ferrite and austenite is avoided.
Specifically, in the step 4, the pipe blank is hot-rolled and then cooled to room temperature, so that precipitation of harmful phases is avoided.
Specifically, in the step 4, since the oil well pipe steel of the present invention has an excellent hot working window, the control of hot rolling and cooling process parameters includes: the initial rolling temperature is controlled to be above 1050 ℃ (for example, 1050-1200 ℃), the final rolling temperature is controlled to be above 950 ℃ (for example, 950 ℃ -1050 ℃), the deformation of the initial rolling pass is not more than 30%, and the deformation of the final rolling pass is not more than 50%.
Compared with the prior art, the high corrosion resistant economic oil well pipe steel of the invention precisely controls the mass percent of Cr, ni, mn, mo, N element in the steel, and can obtain the mixed structure of ferrite, austenite and martensite by combining the thermal deformation process of rolling control and cooling control, thereby greatly improving the corrosion resistance and the toughness of the oil well pipe steel. In stainless steel, the increase of Cr content can improve the strength of the material, but the 17Cr material has superfine martensite, so that the tensile strength of the material is superior to that of duplex stainless steel with higher Cr content. Compared with the duplex stainless steel in the prior art, the 17Cr three-phase structure stainless steel provided by the invention has the advantages that the three-phase structure with adjustable martensite content is obtained after hot rolling by controlling the content combination of Cr, ni, mn, mo, N, and the high strength is obtained by using the lower Cr content. Compared with the martensitic stainless steel in the prior art, the stainless steel of the invention introduces ferrite and austenite to obtain better intergranular corrosion resistance and H resistance 2 S stress corrosion performance. The austenitic stainless steel of the invention has the austenitic content far higher than that of martensitic stainless steel, and the martensitic stainless steel is difficult to obtain the austenitic with the austenitic content more than 20 percent, so that the material of the invention has better hydrogen embrittlement resistance.
The steel of the invention not only ensures high strength, good ductility and toughness and excellent corrosion resistance, but also ensures that the yield strength of the steel of the invention is more than 600MPa (for example, 601-648 MPa), the tensile strength is more than 910MPa (for example, 911-1010 MPa), and the elongation is more than 22% (for example, 23-24%). (180 ℃ C.) CO 2 Corrosion rate of 0.028g/m 2 h is less than or equal to (e.g., 0.0203-0.0275 g/m) 2 h)；(200℃)CO 2 Corrosion rate of 0.1g/m 2 h is less than or equal to (e.g., 0.078 to 0.099 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the Pitting corrosion rate 2.5g/m 2 h is less than or equal to (e.g., 1.693-2.433 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the The crevice corrosion rate was 5.9g/m 2 h is less than or equal to (for example, 3.303-5.852 g/m) 2 h)；H 2 The S stress corrosion test is passed.
The steel has good toughness and excellent corrosion resistance, and has the high strength of the super martensitic stainless steel oil well pipe material and the stress corrosion resistance, the intergranular corrosion resistance and the small amount of H resistance of the duplex stainless steel 2 S stress corrosion capability. Because the Cr and Ni contents of the steel are low, the raw material cost is equivalent to or even slightly lower than that of the super 13Cr martensitic stainless steel in the prior art, and the hot workability is good, the steel has low comprehensive cost, economy and practicability.
Examples 1 to 4
The following shows the advantages of the precise control of the composition and process parameters of the steel according to the invention in the specific examples and comparative examples. 13Cr was selected as a comparison object of corrosion performance.
Examples 1-4 of the present invention provide a highly corrosion resistant economical oil well pipe steel and a method for preparing the same, and the chemical compositions of the steels of examples 1-4 are shown in Table 1.
The preparation method of the example 1 comprises the following steps:
step 1: smelting a metal raw material into molten steel; smelting molten steel into steel ingots by adopting a die casting method to obtain casting blanks;
step 2: heating a casting blank to 1150 ℃, preserving heat for 2 hours, and forging and cogging to prepare a forging blank;
step 3: the forging stock is kept at 1050 ℃ for 2 hours, rolled into a tube blank, and the three-phase structure content, the ferrite content, the martensite content and the austenite content are adjusted to be 20% by controlling the hot rolling and cooling process parameters (the deformation of the first pass is 25%, the deformation of the final pass is 48%, the thickness of the final rolling plate is controlled to be about 3.5mm and water cooling) and controlling the final rolling temperature to be 960 ℃.
The preparation method of example 2 comprises:
step 1: smelting a metal raw material into molten steel; smelting molten steel into steel ingots by adopting a die casting method to obtain casting blanks;
step 2: heating a casting blank to 1180 ℃, preserving heat for 1.5 hours, and forging and cogging to prepare a forging blank;
step 3: the forging stock is kept at 1150 ℃ for 2 hours, rolled into a tube blank, and the three-phase structure content, the ferrite content, the martensite content and the austenite content are adjusted by controlling the hot rolling and cooling process parameters (the first pass deformation amount is 28%, the final pass deformation amount is 45%, the final rolling plate thickness is controlled to be about 3.5mm and water cooling) and controlling the final rolling temperature to be 1000 ℃ to be 45%, respectively.
The preparation method of example 3 comprises:
step 1: smelting a metal raw material into molten steel; smelting molten steel into steel ingots by adopting a die casting method to obtain casting blanks;
step 2: heating a casting blank to 1200 ℃ and preserving heat for 1h, and forging and cogging to prepare a forging blank;
step 3: the forging stock is kept at 1200 ℃ for 2 hours, rolled into a tube blank, hot rolling and cooling process parameters (23% of deformation of a first pass, 46% of deformation of a final pass and water cooling of a final rolling plate thickness of about 3.5 mm) are controlled, and the final rolling temperature is 1050 ℃ (three-phase structure content is adjusted, ferrite content is 40%, martensite content is 30% and austenite content is 30%) is controlled.
The preparation method of example 4 comprises:
step 1: smelting a metal raw material into molten steel; smelting molten steel into cast ingots by adopting a die casting method to obtain cast blanks;
step 2: heating the cast ingot to 1250 ℃, preserving heat for 1h, and forging and cogging to prepare a forging stock;
step 3: the forging stock is kept at 1200 ℃ for 2 hours, rolled into a tube blank, and the three-phase structure content, the ferrite content, the martensite content and the austenite content are adjusted to 35% by controlling the hot rolling and cooling process parameters (the deformation of the first pass is 26%, the deformation of the final pass is 45%, the thickness of the final rolling plate is controlled to be about 3.5mm and water cooling) and controlling the final rolling temperature to 1050 ℃.
The specific process parameters of examples 1-4 are shown in Table 2, the mechanical properties of examples 1-4 are shown in Table 3, FIG. 1 is a microstructure of the steel of example 1 of the present invention, FIG. 2 is a transmission electron microscopy image at M in FIG. 1 of the present invention, wherein the upper left corner is the diffraction spots of the martensite and austenite matrix at A, and it can be demonstrated that the crystal structure of the black martensite sheet and the thickness of the martensite sheet is < 100nm.
FIGS. 3 to 5 are microstructure diagrams of steels according to examples 2 to 4 of the present invention, respectively; the microstructures of examples 1-4 are shown in Table 4 below. The microstructure of the high corrosion resistant economic oil well pipe steel is a mixed structure of ferrite, austenite and martensite, wherein the volume percentage of austenite is 20% -40% (for example, 20% -35%), the volume percentage of martensite is 10% -40% (for example, 30% -40%), the martensite is dispersed in the austenite in an ultrafine flake form, and the martensite is alternately laminated with the austenite and mutually divided, so that the austenite has smaller grain size (for example, the grain size of the austenite is less than 3 mu m), and the thickness of the martensite sheet is less than 100nm.
TABLE 1 chemical Components wt% of examples 1-4
Figure BDA0003995980270000121
Table 2 specific process parameters for examples 1-4
Numbering device Forging cogging temperature, DEG C Hot rolling temperature (initial rolling, final rolling), DEG C
Example 1 1150 1050、950
Example 2 1180 1150、1000
Example 3 1200 1200、1050
Example 4 1250 1200、1050
TABLE 3 mechanical Properties of examples 1-4
Figure BDA0003995980270000122
TABLE 4 microstructure of the steels of examples 1-4
Figure BDA0003995980270000131
To illustrate the corrosion resistance of the steels of the present invention, the steels of examples 1 to 4 were evaluated for corrosion resistance by 5 different conditions and compared with 13Cr under the same test conditions, and the corrosion resistance of the steels of the present invention in different corrosion environments was evaluated by this experiment. The results of the corrosion resistance test are shown in Table 5, and the corresponding test conditions are as follows:
CO (180 ℃ or 200 ℃) 2 The corrosion conditions for the corrosion rate were as follows:
1. medium (formation water) mg/L: CO 3 2- /0，HCO 3 - /189,OH - /0,Cl - /128000,SO 4 2- /430,Ca 2+ /8310,Mg 2+ /561,K + /6620,Na + /76500)；
2、CO 2 Partial pressure: 4.48MPa, total test pressure: 10MPa;
3. test temperature 180 ℃ or 200 ℃;
4. the test time was 720 hours.
The corrosion conditions for the pitting corrosion rate were as follows:
1. test temperature: 22+/-2 ℃;
2. medium: 100g of reagent grade ferric trichloride FeCl 3 ·6H 2 O is dissolved in 900mL of IV type reagent grade water (mass ratio is about 6%);
3. test time: 72 hours;
4. sample size: 50X 25X 3mm was sanded to 2000# sandpaper.
The etching conditions for the crevice etching rate were as follows:
1. the test temperature is 22+/-2 ℃;
2. 100g of reagent grade ferric trichloride FeCl 3 ·6H 2 O is dissolved in 900mL of IV type reagent grade water (mass ratio is about 6%);
3. test time: 72 hours;
4. sample size: 50X 25X 3mm was sanded to 2000# sandpaper.
H 2 The corrosion conditions for the S stress corrosion test are as follows:
1. the test temperature is 22+/-2 ℃;
2、50g NaCl、25g[23.8mL]CH 3 COOH、4.1g CH 3 COONa was dissolved in 921mL type IV reagent grade water (mass ratio of about 5wt% sodium chloride, 2.5wt% glacial acetic acid, and 0.41wt% sodium acetate);
3. test time: 720 hours;
4. sample size: polishing 50X 5X 2mm to 2000# sand paper;
5. the four-point bending test, the loading force was 80% yield stress.
As can be seen from Table 5, the (180 ℃) CO of the high corrosion resistant economical well pipe steels of examples 1 to 4 2 Corrosion rate of 0.028g/m 2 h is less than or equal to (e.g., 0.0203-0.0275 g/m) 2 h)；(200℃)CO 2 Corrosion rate of 0.1g/m 2 h is less than or equal to (e.g., 0.078 to 0.099 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the Pitting corrosion rate 2.5g/m 2 h is less than or equal to (e.g., 1.693-2.433 g/m) 2 h) The method comprises the steps of carrying out a first treatment on the surface of the The crevice corrosion rate was 5.9g/m 2 h is less than or equal to (for example, 3.303-5.852 g/m) 2 h)；H 2 The S stress corrosion test is passed. The corrosion resistance of examples 1-4 of the invention is better than that of 13Cr, especially CO resistance at 200 DEG C 2 The corrosion performance of the invention is far superior to super 13Cr, and the invention can be used in more severe environment, namely, environment with larger well depth. As shown in FIG. 5, H of example 1 2 S stress corrosion test results.
TABLE 5 Corrosion test data
Figure BDA0003995980270000141
Figure BDA0003995980270000151
In order to illustrate the hot workability of the steels of the present invention, the edge quality of the hot rolled steel sheet of examples 1 to 4 was counted, taking example 1 as an example. FIG. 6 is a photograph of a hot rolled sheet of example 1, showing that there is no cracking at the edges, and the steel of the example of the present invention has a yield of 90% or more in the actual production process.
The inventors have conducted intensive studies in the study, and some of these poorly effective schemes are now exemplified as comparative examples as follows:
comparative example 1
The comparative example provides a corrosion-resistant oil well pipe steel and a preparation method thereof, wherein the corrosion-resistant oil well pipe steel is 13Cr and is prepared by adopting the existing 13Cr mature technology. The corrosion resistant oil well pipe steel of this comparative example has the composition C:0.03%, cr:13%, ni:5%, mo:2%, mn:0.5%, si:0.5 percent of the preparation method: after being heated and forged at 1150 ℃, the steel is cooled by water, and then is heated to 860 ℃ again for 2 hours, quenched and tempered at 620 ℃ for 1 hour.
The microstructure of the steel of this comparative example was martensitic (93%) + austenitic (7%). The mechanical properties are shown in Table 3, and the corrosion resistance results are shown in Table 5.
Comparative example 2
The comparative example provides a corrosion-resistant oil well pipe steel and a preparation method thereof, and the corrosion-resistant oil well pipe steel comprises the following components: 0.03%, cr:16%, mo:1.21%, N:0.22%, mn:2.11%, si:0.5% by weight, and the preparation method was the same as in example 1.
The microstructure of the steel of this comparative example was ferrite (15%) +martensite (65%) +austenite (20%). The mechanical properties are shown in Table 3, and the corrosion resistance results are shown in Table 5.
Comparative example 3
The comparative example provides a corrosion-resistant oil well pipe steel and a preparation method thereof, and the corrosion-resistant oil well pipe steel comprises the following components: 0.04%, cr:16.5%, ni:1.12%, mo:1.32%, N:0.16%, mn:2.82%, si:0.5% by weight, and the preparation method was the same as in example 1.
The microstructure of the steel of this comparative example was ferrite (20%) +martensite (60%) +austenite (20%). The mechanical properties are shown in Table 3, and the corrosion resistance results are shown in Table 5.
As can be seen from the comparison examples and comparative examples, the high corrosion resistant economic oil well pipe steel of the invention precisely controls the mass percent of Cr, ni, mn, mo, N element in the steel, and can obtain the mixed structure of ferrite, austenite and martensite by combining the hot deformation process of controlled rolling and controlled cooling, thereby greatly improving the corrosion resistance and toughness of the oil well pipe steel, the raw material cost is equivalent to or even slightly lower than that of the super 13Cr martensitic stainless steel in the prior art, and the hot workability is good, and the corrosion resistance of the high corrosion resistant economic oil well pipe steel of the invention is superior to that of the super 13Cr martensitic stainless steel, so that the steel of the invention has low comprehensive cost, economy and practicability.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.

Claims (10)

1. The high corrosion resistant economic oil well pipe steel is characterized by comprising the following components in percentage by mass: c: less than or equal to 0.03 percent, cr:17.3% -18.4%, mo:0.5 to 2.0 percent of Ni:1.0 to 2.8 percent of Mn:1.0% -3.5%, si:0.1% -0.5%, N:0.1% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities.
2. The high corrosion resistant economical oil well pipe steel according to claim 1, wherein Cr+3.3Mo+16N is not less than 26 in the composition of the high corrosion resistant economical oil well pipe steel.
3. The high corrosion resistant economical oil well pipe steel according to claim 1, wherein 60ni+17mn-12Mo-800N is 0 or less among the components of the high corrosion resistant economical oil well pipe steel.
4. The high corrosion resistant economical oil well pipe steel according to claim 1, wherein the high corrosion resistant economical oil well pipe steel comprises the following components in percentage by mass: c:0.01% -0.03%, cr:17.4% -18.4%, mo:1.0% -2.0%, ni:1.0 to 2.7 percent of Mn:1.4 to 3.2 percent of Si:0.1% -0.5%, N:0.13% -0.25%, P: less than or equal to 0.03 percent, S: less than or equal to 0.01 percent, and the balance of Fe and unavoidable impurities.
5. The high corrosion resistant economical oil well pipe steel of claim 1, wherein the microstructure of the high corrosion resistant economical oil well pipe steel is a mixed structure of ferrite + austenite + martensite.
6. The high corrosion resistant economical oil well pipe steel according to claim 5, wherein the microstructure of the high corrosion resistant economical oil well pipe steel has a volume percentage of austenite of 20% to 40% and a volume percentage of martensite of 10% to 40%.
7. The high corrosion resistant economical oil well pipe steel of claim 5, wherein the austenitic grain size in the microstructure of said high corrosion resistant economical oil well pipe steel is < 3 μm.
8. A method for preparing a high corrosion resistant economical oil well pipe steel according to any one of claims 1 to 7, comprising:
step 1: smelting a metal raw material into molten steel;
step 2: smelting molten steel into a continuous casting blank or an ingot by adopting a continuous casting or die casting method;
step 3: forging and cogging a continuous casting blank or an ingot to prepare a forging blank;
step 4: rolling the forging stock into a tube blank, and controlling the technological parameters of hot rolling and cooling to obtain the high corrosion resistant economic oil well tube steel.
9. The method according to claim 8, wherein in the step 3, the forging cogging temperature is 1150 to 1250 ℃.
10. The method according to any one of claims 7 to 9, wherein in the step 4, controlling hot rolling and cooling process parameters comprises: the initial rolling temperature is controlled to be higher than 1050 ℃, the final rolling temperature is controlled to be higher than 950 ℃, the deformation of the first rolling pass is not higher than 30%, and the deformation of the final rolling pass is not higher than 50%.
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