CN110129658B - High-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel and preparation method thereof - Google Patents
High-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel and preparation method thereof Download PDFInfo
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Abstract
A high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel and a manufacturing method thereof are disclosed, wherein the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel comprises the following chemical components: c<0.05％，Si<0.50％，Mn：6～10％，Cr：12～16％，Ni：4.5～6.5％，Mo：0.5～3％，S<0.01％，P<0.03 percent, and the balance of Fe, and trace Nb, Ti, V, Al, Cu and inevitable impurity elements. The manufacturing method comprises the process steps of smelting (casting), forging (hot rolling), rolling, tempering and the like. The high-strength high-toughness stainless steel manufactured by the invention is characterized in that based on 13Cr-5Ni-2Mo/15Cr-6Ni-2Mo super martensitic stainless steel, the austenitizing is carried out by adding cheap Mn element, the high strength is realized by the back stress strengthening of residual martensite and the fine grain strengthening of austenite matrix, the high toughness is obtained by phase transformation, and the H resistance of the material is improved by austenitizing2S (hydrogen embrittlement) stress corrosion performance. The high-strength steel manufactured by the invention has extremely high toughness and hydrogen embrittlement resistance while maintaining good corrosion resistance. The invention has simple process and easy realization of industrialization, and can be used for H-containing2The oil pipe of the S oil (gas) is used in the environment with high requirements on corrosion resistance and hydrogen embrittlement resistance.
Description
Technical Field
The invention relates to high-manganese low-carbon nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel and a preparation method thereof, in particular to high-strength stainless steel which can be used as a deep well oil gas pipeline material and a crude oil and natural gas conveying equipment material.
Background
The 13Cr/15Cr type stainless steel commonly used in China is mainly martensitic stainless steel, and the main alloy elements are C and Cr. This type of steel is widely used because of its high hardness and low cost. Unfortunately, Cr is formed due to the addition of a large amount of C23C6Reducing the effective Cr content and simultaneously generating Cr23C6Easy to be segregated in the grain boundary to cause intergranular corrosion. Therefore, the corrosion resistance of the traditional martensitic stainless steel in a severer service environment faces serious challenges; meanwhile, researches show that the traditional 13Cr type martensitic stainless steel can generate H2And S stress corrosion. In order to overcome the above problems of the conventional martensitic stainless steel, the improvement of corrosion resistance and H resistance of the material by increasing the content of Cr element and adding Mo element has been developed2S stress corrosion performance, therefore, a certain amount of Ni element may need to be further added to ensure that the material is completely austenitized and a full martensite structure is ensured.
In the 90 s improved super 13Cr/15Cr stainless steels containing very little carbon, moderate amounts of nickel and molybdenum were developed abroad. However, in this steel, the highest hardness in HRC is also limited to 27 (see NACE MR 0175-2001). The improved super 13Cr/15Cr stainless steel mentioned above, several steels having high mechanical strength and excellent corrosion resistance have been proposed. For example, International patent WO 2017/162160A 1 discloses an H-resistant composition2The S stress corrosion cracked martensitic stainless steel oil casing is mainly characterized by comprising the following chemical elements in percentage by mass: c:<0.05%, Cr: 11-14%, Ni: 4-7%, Mo: 1.5-2.5%; the metal structure is mainly composed of tempered martensite and can be in high-concentration CO2、Cl-Oil wells and gas wells of crude oil or natural gas in a strongly corrosive environment in which they coexist, but H is2The applicable environment of S is limited to 0.01MPa, and the strength is only 95 ksi. International patent WO2005/007915A1 discloses a superior H resistance to super 13Cr steel2The S stress corrosion martensitic stainless steel is mainly characterized in that the maximum content of Mo is not more than 10 percent by adding, and the corrosion resistance and the H resistance are improved by controlling the content of solid-dissolved Mo to be 3.5-7 percent2S (hydrogen embrittlement) stress corrosion capability. The martensitic stainless steel toolHas high mechanical strength and is in CO2H which has excellent corrosion resistance in the environment but is suitable for use2The S partial pressure is only 0.003 MPa.
The domestic related patent also modifies the traditional 13Cr martensitic stainless steel. For example, CN1571858 provides a martensitic stainless steel with Mo and Cu added, which has excellent sulfide stress corrosion resistance, corrosion wear resistance and local corrosion resistance; CN102534419 provides another modification method: the C content is reduced to 0-0.03%, the Ni content is increased to 4-6%, the Mo content is increased to 1-2%, and the martensitic stainless steel has high strength and toughness and good local corrosion resistance.
The 13Cr/15Cr type super martensitic stainless steel modified above generally has low toughness due to the martensite matrix, and is also H-pair at high strength level (more than X110, X125 level and the like)2S stress corrosion is very sensitive.
Disclosure of Invention
With the development of AOD/VOD refining technology, the P, S impurity content in steel is further accurately controlled, and further optimization of alloy composition becomes possible. The strict control of the S element can realize that the content of the Mn element reaches high and does not generate MnS large-particle impurities. Aiming at the problems in the prior art, the invention is based on the existing 13Cr-5Ni-2Mo/15Cr-6Ni-2Mo type super martensitic stainless steel, relates to a preparation flow method which can reduce the Ms point by adding a cheap element Mn, realize austenitization, realize industrial production and generate huge economic benefits, and is easy to realize industrialization and industrialization.
The high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel comprises the following chemical components in percentage by mass: c < 0.05%, Si < 0.50%, Mn: 6-10%, Cr: 12-16%, Ni: 4.5-6.5%, Mo: 0.5-3%, S < 0.01%, P < 0.02%, and the balance of Fe and trace amounts of Nb, Ti, V, Al, Cu and inevitable impurity elements.
Further, when the Cr content is more than 15%, the Ni content needs to be more than 5.5% to ensure that the material is free of ferrite formation in a high-temperature solid solution state.
The preparation method of the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel comprises the following steps:
(1) smelting and casting are adopted to obtain a high-strength high-toughness austenitic stainless steel casting blank meeting the requirements of the chemical components;
(2) forging or hot rolling at 1100-1300 deg.c;
(3) cold rolling the formed high-strength high-toughness stainless steel, wherein the total reduction is 35-55%;
(4) and tempering the cold-rolled stainless steel at 600-800 ℃ to obtain the high-strength and high-toughness austenitic stainless steel with different strength levels, including 110ksi,125ksi and the like.
Further, the austenitic stainless steel is prepared on the basis of 13Cr-5Ni-2Mo/15Cr-6Ni-2Mo super martensitic stainless steel, and a cheap alloy element Mn is added to reduce the martensitic transformation temperature (Ms) for austenitizing; austenite grains are refined through a phase transformation process, and back stress strengthening is carried out on an austenite matrix through residual martensite; the fine crystal strengthening and the back stress strengthening inhibit the movement of dislocation at the initial stage of deformation, so that the material obtains extremely high yield strength.
Further, when the material enters a shaping stage, dislocation starts to propagate, the stability of an austenite matrix is damaged, martensite transformation starts to occur, and the high-strength steel manufactured by phase transformation obtains high toughness.
In the present solution, other unavoidable trace impurities are mainly S, P, O and N.
Influence of S
S is H resistance affecting steel2S (hydrogen embrittlement) is an important element of stress corrosion ability, which causes anisotropy of steel, deterioration of toughness in transverse and thickness directions, and affects low-temperature impact toughness of materials. Meanwhile, S and Mn form MnS large inclusions, the mechanical property of the material is deteriorated, and the addition threshold of Mn elements in steel grades is influenced.
Influence of P
P can obviously reduce the low-temperature impact toughness of the steel, improve the ductile-brittle transition temperature of the steel and cause the steel to be cold-brittle. Meanwhile, when the content of the P element exceeds a threshold value, the P element can be segregated in a grain boundary, and the mechanical property of the material is seriously deteriorated.
Influence of O
The element O is present in the steel mainly in the form of oxides, which have a negative effect on the hot workability, impact toughness and corrosion resistance of the steel.
Influence of N
N is a beneficial element added into the steel, can improve the pitting corrosion resistance of the stainless steel, and can be used as an austenite performance element to balance Cr equivalent, so that the stainless steel has no ferrite generation in a high-temperature solid solution state. However, the high-strength high-toughness austenitic stainless steel provided by the invention relates to a tempering process at 600-800 ℃, the temperature range is a CrN strong aging precipitation temperature range, and CrN rapidly deteriorates the mechanical property of the material, so that the content of N element needs to be strictly controlled.
After the manufacturing process, the typical structures of the high-strength high-toughness austenitic stainless steel at room temperature are residual martensite and recrystallized fine-grained austenite, wherein the fine-grained austenite is mainly divided into equiaxed austenite growing in a diffusion property and lath-shaped austenite growing in a cutting deformation manner.
Compared with the 13Cr-5Ni-2Mo/15Cr-6Ni-2Mo super martensitic stainless steel in the prior art, the invention has the following beneficial effects:
1. the high-strength high-toughness austenitic stainless steel related by the invention is austenitized by adding the cheap Mn element, compared with the Ni element, the cost is only one tenth of the cost, the mechanical property of the material is greatly improved while little cost is increased, and the production cost is strictly controlled.
2. The high-strength high-toughness austenitic stainless steel can reach extremely high strength levels (110ksi,125ksi and the like), has good corrosion resistance and excellent H resistance2S (hydrogen embrittlement) stress corrosion capability.
3. The high-strength high-toughness austenitic stainless steel related by the invention has simple production process, is easy to realize industrialization and industrialization, and generates great economic benefit.
Drawings
FIG. 1 is an example EBSD contrast map;
FIG. 2 is a graph of engineering stress-strain for an example;
figure 3 is a potentiodynamic polarization curve for the examples and comparative examples in four solutions,
a)0.2M NaSO4；b)0.1M HNO3；c)0.2M NaOH；d)3.5％NaCl；
FIG. 4 shows examples and comparative examples CO2The surface appearance after the corrosion test is finished,
a) and b) USTB13 Cr; c) and d) S13Cr.;
FIG. 5 shows the results of the step-by-step loading test in examples and comparative examples,
a)USTB13Cr；b)S13Cr.。
Detailed Description
Examples and comparative examples
Table 1 shows the chemical composition proportion of the high-strength high-toughness austenitic stainless steel (marked as USTB13Cr) and 13Cr-5Ni-2Mo super martensitic stainless steel (marked as S13Cr) produced commercially by factories.
TABLE 1 examples and comparative examples chemical compositions
The balance in table 1 is Fe and inevitable impurity elements.
The heat treatment processes of the examples were hot forging (forging temperature 1200 ℃), cold rolling (total rolling amount 44%), and tempering (holding at 700 ℃ for 1 hour).
Example electron backscatter diffraction patterns (EBSDs) are shown in figure 1. Examples the main microstructures were fine crystalline regions and coarse crystalline regions. Wherein the fine crystalline region is a mixed state of nano-scale austenite and residual martensite. The coarse crystal region is residual austenite which is not recrystallized, the residual austenite is rolled to form a strip structure, and martensite is distributed among the strip austenite.
Example engineering stress-strain curves are shown in figure 2. Example USTB13Cr gave 932MPa of yield strength (to 125ksi strength grade), 1085MPa of tensile strength, 33.2% elongation, 29% uniform elongation. Comparative example S13Cr super martensitic stainless steel has a yield strength of 912MPa, a tensile strength of 1030MPa, and an elongation of 16.3%. Under the same strength range, the toughness of the embodiment is greatly improved.
The zeta potential polarization curves of the examples and comparative examples in acid base salts are shown in figure 3. In alkaline and neutral solutions, USTB13Cr showed a better self-corrosion potential than S13Cr, showing a lesser tendency to corrode. In the strongly acidic solution, the self-corrosion potential difference between USTB13Cr and S13Cr is small, the self-corrosion current density of USTB13Cr is higher, and the corrosion resistance is slightly reduced.
Examples and comparative examples CO2The results of the corrosion test are shown in FIG. 4, and the experimental conditions are CO in a 3.5% NaCl solution2The partial pressure is 1MPa, the temperature is 120 ℃, and the experimental time is 720 hours.
The comparative example surface had a yellowish product film locally attached. The surface of the example is attached with a thin product film, and the good CO resistance is still maintained2The results of the threshold stress test of the examples and comparative examples in a simulated hydrogen atmosphere using a step-by-step loading test are shown in FIG. 5, the simulated solution is 0.2 mol/L NaOH +0.22 g/L thiourea, and the charging current density is 2mA/cm2。
The comparative example S13Cr has the threshold strength of 613MPa, the example USTB13Cr has the threshold strength of 860MPa, the threshold strength is increased by 40 percent, and the H resistance of the material is greatly improved2S stress corrosion (hydrogen embrittlement) ability.
Claims (5)
1. The high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel is characterized by comprising the following chemical components in percentage by mass: c < 0.05%, Si < 0.50%, Mn: 6-10%, Cr: 12-16%, Ni: 4.5-6.5%, Mo: 0.5-3%, S < 0.01%, P < 0.02%, and the balance of Fe, trace Nb, Ti, V, Al, Cu and inevitable impurity elements;
the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel is smelted and cast to obtain a high-strength high-toughness austenitic stainless steel casting blank, then the high-strength high-toughness austenitic stainless steel casting blank is forged or hot-rolled for forming, then cold rolling treatment is carried out, and finally tempering treatment is carried out to obtain high-strength high-toughness austenitic stainless steel with different strength levels, wherein the high-strength high-toughness austenitic stainless steel comprises 110ksi and 125 ksi;
after the manufacturing process is carried out on the high-manganese nitrogen-free high-strength high-toughness hydrogen-embrittlement-resistant austenitic stainless steel, typical tissues at room temperature are residual martensite and recrystallized fine-grained austenite, wherein the fine-grained austenite is mainly divided into equiaxed austenite growing in a diffusion property and lath-shaped austenite growing in a cutting deformation manner.
2. The high strength high toughness austenitic stainless steel of claim 1, wherein when Cr content is more than 15%, Ni content needs to be more than 5.5% to ensure that the material is free of ferrite formation in high temperature solid solution state.
3. A method for preparing the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel as claimed in claim 1, which is carried out according to the following steps:
(1) smelting and casting are adopted to obtain a high-strength high-toughness austenitic stainless steel casting blank meeting the requirements of the chemical components;
(2) forging or hot rolling at 1100-1300 deg.c;
(3) cold rolling the formed high-strength high-toughness stainless steel, wherein the total reduction is 35-55%;
(4) and tempering the cold-rolled stainless steel at 600-800 ℃ to obtain the high-strength and high-toughness austenitic stainless steel with different strength levels, including 110ksi and 125 ksi.
4. The method for preparing the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel as claimed in claim 3, wherein the austenitic stainless steel is prepared based on 13Cr-5Ni-2Mo/15Cr-6Ni-2Mo super martensitic stainless steel, and a cheap alloying element Mn is added to reduce the martensite transformation temperature (Ms) for austenitizing; austenite grains are refined through a phase transformation process, and back stress strengthening is carried out on an austenite matrix through residual martensite; the fine crystal strengthening and the back stress strengthening inhibit the movement of dislocation at the initial stage of deformation, so that the material obtains extremely high yield strength.
5. The method for preparing the high-manganese nitrogen-free high-strength high-toughness hydrogen embrittlement-resistant austenitic stainless steel as claimed in claim 4, wherein when the material enters a shaping stage, dislocations start to proliferate, the stability of an austenitic matrix is destroyed, martensite transformation starts to occur, and phase transformation enables the manufactured high-strength steel to obtain high toughness.
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| CN111659732B (en) * | 2020-06-08 | 2022-04-19 | 首钢集团有限公司 | Method for solving corrosion of high-manganese hot-formed steel after pickling |
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| CN113136533B (en) * | 2021-04-15 | 2022-08-16 | 鞍钢股份有限公司 | Austenitic stainless steel for low temperature and manufacturing method thereof |
| CN113755753B (en) * | 2021-08-24 | 2022-06-17 | 北京科技大学 | Heterogeneous structure based multi-type strengthened austenitic stainless steel and manufacturing method thereof |
| CN114083090A (en) * | 2021-11-17 | 2022-02-25 | 华南理工大学 | Austenitic stainless steel hydrogen embrittlement-resistant weldment for hydrogen energy equipment and preparation method |
| CN114107630B (en) * | 2021-11-19 | 2022-08-19 | 北京科技大学 | Heat treatment method for improving hydrogen brittleness resistance of martensitic stainless steel, stainless steel and application |
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