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CN118813926B - 9Cr stainless steel quenched and tempered material for oil gas, and manufacturing method and application thereof - Google Patents

9Cr stainless steel quenched and tempered material for oil gas, and manufacturing method and application thereof

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Publication number
CN118813926B
CN118813926B CN202410821354.6A CN202410821354A CN118813926B CN 118813926 B CN118813926 B CN 118813926B CN 202410821354 A CN202410821354 A CN 202410821354A CN 118813926 B CN118813926 B CN 118813926B
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stainless steel
tempering
tempered material
oil
gas
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CN118813926A (en
Inventor
张永强
李造宇
张军
张秀丽
程志伟
孙国洋
徐朋
董晓亮
代玉磊
曾淼
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Daye Special Steel Co Ltd
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Daye Special Steel Co Ltd
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Priority to CN202410821354.6A priority Critical patent/CN118813926B/en
Publication of CN118813926A publication Critical patent/CN118813926A/en
Priority to PCT/CN2025/078332 priority patent/WO2025149093A1/en
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D8/00Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/06Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of rods or wires
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/18Hardening; Quenching with or without subsequent tempering
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/02Ferrous alloys, e.g. steel alloys containing silicon
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/04Ferrous alloys, e.g. steel alloys containing manganese
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/44Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
    • EFIXED CONSTRUCTIONS
    • E21EARTH OR ROCK DRILLING; MINING
    • E21BEARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
    • E21B17/00Drilling rods or pipes; Flexible drill strings; Kellies; Drill collars; Sucker rods; Cables; Casings; Tubings
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D2211/00Microstructure comprising significant phases
    • C21D2211/008Martensite

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Geology (AREA)
  • Mining & Mineral Resources (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Fluid Mechanics (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Heat Treatment Of Articles (AREA)

Abstract

本发明提供了一种油气用9Cr不锈钢调质材及其制造方法和应用,涉及9Cr钢在线热处理技术领域。该油气用9Cr不锈钢调质材及其制造方法主要通过控制9Cr钢材的终轧温度和快速冷却方式,以使9Cr钢材直接获得淬火马氏体,省去了传统工艺中的淬火工序,使得周期缩短1‑3天,并采用一次回火处理和去应力回火处理的两次回火步骤代替了传统工序中的退火、退火后矫直、扒皮和倒角,大大缩短了生产周期,降低了生产成本,与采用传统工艺制得的9Cr不锈钢调质材相比,采用本发明制备方法制得的9Cr不锈钢调质材具有与其相当的晶粒度以及硬度、拉伸和冲击性能。

This invention provides a 9Cr stainless steel tempered material for oil and gas applications, its manufacturing method, and its application, relating to the field of online heat treatment technology for 9Cr steel. The method for manufacturing this 9Cr stainless steel tempered material for oil and gas applications primarily achieves quenched martensite directly by controlling the final rolling temperature and rapid cooling of the 9Cr steel, eliminating the quenching step in traditional processes and shortening the cycle by 1-3 days. Furthermore, it replaces the traditional annealing, post-annealing straightening, peeling, and chamfering processes with a two-step tempering process involving one tempering treatment and stress-relief tempering treatment, significantly shortening the production cycle and reducing production costs. Compared to 9Cr stainless steel tempered materials produced using traditional processes, the 9Cr stainless steel tempered material prepared using the method of this invention exhibits comparable grain size, hardness, tensile strength, and impact resistance.

Description

9Cr stainless steel quenched and tempered material for oil gas, and manufacturing method and application thereof
Technical Field
The invention relates to the technical field of 9Cr steel on-line heat treatment, in particular to a 9Cr stainless steel quenched and tempered material for oil gas, a manufacturing method and application thereof.
Background
With the continued development and growth of the global energy market, the demand for high performance materials in the oil and gas industry is increasing. Stainless steel is widely used in oil and gas industry as a material with excellent corrosion resistance and high temperature performance. The types of the stainless steel for oil gas are not few, wherein the 9Cr stainless steel for oil gas is one of the main materials of steel for oil gas exploitation links by virtue of the performances of corrosion, high temperature resistance, high impact and the like.
At present, the existing production flow of the 9Cr stainless steel quenched and tempered materials for oil gas comprises the steps of raw material (molten iron, scrap steel, alloy and the like) preparation, electric furnace smelting, external refining, vacuum degassing (inclusion control and gas content control), continuous casting/die casting (tissue uniformity control), annealing/red feeding, heating, rolling (material grain size and compactness control), annealing, straightening (flatness preparation before quenching and tempering), skinning, chamfering (quenching and anti-cracking preparation before quenching and tempering), quenching (specifically comprising quenching, primary tempering, straightening, stress relief tempering), physical and chemical inspection, surface polishing, flaw detection, surface inspection, inspection judgment and packaging and warehousing.
The process has long production flow, the delivery period generally needs two to three months, the user needs are difficult to meet, the production cost is high, the selling price is high, and the market competitiveness is lacking, so that improvement of the production flow is needed to reduce the cost and increase the efficiency.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a 9Cr stainless steel quenched and tempered material suitable for the oil and gas field and a manufacturing method thereof, and the manufacturing method of the 9Cr stainless steel quenched and tempered material breaks through the traditional production flow, shortens the production period and simultaneously reduces the production cost, and the performance and the grain size of the 9Cr stainless steel quenched and tempered material manufactured by the manufacturing method are basically equivalent to those of the 9Cr stainless steel quenched and tempered material manufactured by the traditional process.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The first object of the invention is to provide a manufacturing method of a 9Cr stainless steel quenched and tempered material for oil and gas, comprising the following steps:
S1, sequentially performing primary refining, vacuum degassing, continuous casting or die casting, annealing or red feeding, heating and rolling on raw materials according to chemical components of a 9Cr stainless steel quenched and tempered material for oil gas to obtain 9Cr steel, wherein the rolling finishing temperature is more than or equal to 850 ℃;
S2, rapidly cooling the 9Cr steel to enable the structure of the 9Cr steel to be converted into quenched martensite, and then directly performing primary tempering treatment;
s3, straightening the steel subjected to primary tempering treatment, and then carrying out stress relief tempering treatment to obtain the 9Cr stainless steel quenched and tempered material for oil gas.
Furthermore, on the basis of the technical scheme of the invention, in the step S1, the final rolling temperature of rolling is more than or equal to 900 ℃.
Furthermore, on the basis of the technical scheme, in the step S2, the cooling speed of the 9Cr steel is more than or equal to 300 ℃ per hour when the 9Cr steel is rapidly cooled;
and/or in the step S2, the 9Cr steel is rapidly cooled to be below 150 ℃.
Furthermore, on the basis of the technical scheme, in the step S2, the 9Cr steel is rapidly cooled to be below 150 ℃ at the cooling speed of more than or equal to 300 ℃ per hour, and tempering treatment is carried out for 48 hours;
And/or, in step S2, the rapid cooling mode includes air cooling, air cooling or water cooling.
Further, on the basis of the above technical scheme of the present invention, in step S2, the tempering temperature of the primary tempering treatment is 550-750 ℃, and the primary tempering heat preservation time is (4H/100 mm x D) - (4H/100 mm x d+6h), wherein H represents hours, D represents the diameter of the 9Cr steel, and mm;
And/or, in the step S2, the temperature rising rate of rising to the tempering temperature in the primary tempering treatment is less than or equal to 80 ℃ per hour;
and/or, in the step S2, the cooling mode of the primary tempering treatment is tapping air cooling.
Furthermore, on the basis of the technical scheme, in the step S2, for the 80KSI 9Cr stainless steel quenched and tempered material, the tempering temperature of the primary tempering treatment is 650-750 ℃;
And/or, in the step S2, for the 9Cr stainless steel quenched and tempered material with 100KSI, the tempering temperature of the primary tempering treatment is 565-650 ℃;
And/or, in the step S2, for the 9Cr stainless steel quenched and tempered material of 110KSI, the tempering temperature of the primary tempering treatment is 565-620 ℃.
Further, on the basis of the above technical scheme of the present invention, in step S3, the tempering temperature of the stress-relief tempering treatment is 20-60 ℃ lower than the tempering temperature of the primary tempering treatment, and the stress-relief tempering heat preservation time is (4H/100 mm×d) to (4H/100 mm×d+5h), wherein H represents hours, D represents the diameter of steel, and mm;
And/or, in the step S3, the temperature rising rate of rising to the tempering temperature is less than or equal to 80 ℃ per hour during the stress-relief tempering treatment;
and/or in the step S3, the cooling mode of the destressing tempering treatment is tapping air cooling.
The second object of the invention is to provide a 9Cr stainless steel quenched and tempered material for oil gas, which is manufactured by the manufacturing method of the 9Cr stainless steel quenched and tempered material for oil gas;
The 9Cr stainless steel quenched and tempered material for oil gas comprises the following chemical components, by mass, less than or equal to 0.15% of C, less than or equal to 1.00% of Si, 0.30-0.60% of Mn, less than or equal to 0.020% of P, less than or equal to 0.010% of S, 8.00-10.00% of Cr, less than or equal to 0.50% of Ni, 0.90-1.10% of Mo, and the balance of Fe and unavoidable impurities.
Furthermore, on the basis of the technical scheme, the 9Cr stainless steel quenched and tempered material for oil gas comprises the following chemical components, by mass, 0.09-0.15% of C, less than or equal to 1.00% of Si, 0.30-0.60% of Mn, less than or equal to 0.015% of P, less than or equal to 0.004% of S, 8.50-9.50% of Cr, less than or equal to 0.45% of Ni, 0.90-1.05% of Mo, and the balance of Fe and unavoidable impurities.
The third object of the present invention is to provide a pipe fitting for oil and gas well, wherein the oil and gas 9Cr stainless steel quenched and tempered material or the oil and gas 9Cr stainless steel quenched and tempered material is manufactured by the manufacturing method.
Compared with the prior art, the technical scheme of the invention has at least the following technical effects:
(1) The manufacturing method of the 9Cr stainless steel quenched and tempered material for oil gas breaks the traditional flow, shortens the production period by adjusting or omitting part of working procedures, reduces the production cost (including the cost of annealing, quenching and the like), and effectively ensures the product quality without obvious change of the grain size, the tensile property, the impact property, the hardness and the like of the 9Cr stainless steel quenched and tempered material manufactured by adopting the manufacturing method compared with the traditional process.
(2) The invention provides a 9Cr stainless steel quenched and tempered material for oil gas, which is prepared by adopting the manufacturing method of the 9Cr stainless steel quenched and tempered material for oil gas, and has basically the same grain size as the 9Cr stainless steel quenched and tempered material prepared by the traditional process, and excellent performances such as stretching, impact and hardness.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. Wherein:
FIG. 1 is a golden phase diagram of an 80KSI grade 9Cr stainless steel temper made in example 1;
FIG. 2 is a golden phase diagram of a grade 110KSI stainless steel quenched and tempered steel material made in accordance with example 2;
FIG. 3 is a golden phase diagram of an 80KSI grade 9Cr stainless steel temper made in comparative example 1;
FIG. 4 is a golden phase diagram of a modified 9Cr stainless steel grade of 110KSI steel prepared in comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The process parameters for the specific conditions not noted in the examples below are generally as usual.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present invention.
The existing production process of the 9Cr stainless steel quenched and tempered material for oil gas comprises the steps of sequentially carrying out primary refining, vacuum degassing, continuous casting or die casting, annealing or red feeding, heating and rolling on raw materials, carrying out annealing, straightening, peeling and chamfering treatment, and then carrying out quenching and tempering, wherein the quenching and tempering sequentially comprises quenching, primary tempering, straightening and stress-relief tempering, so as to obtain the 9Cr stainless steel quenched and tempered material. By adopting the production method, the production period of the 9Cr stainless steel quenched and tempered material for oil gas is two to three months, the production period is long, the production efficiency is low, and the production cost is high. And for the downstream customer who needs the steel product urgently, the demand of the downstream customer can not be met in a short time, so the invention is specially proposed.
According to a first aspect of the present invention, there is provided a method for manufacturing a 9Cr stainless steel quenched and tempered material for oil and gas, comprising the steps of:
S1, sequentially performing primary refining, continuous casting or die casting, annealing or red feeding, heating and rolling on raw materials according to chemical components of a 9Cr stainless steel quenched and tempered material for oil gas to obtain 9Cr steel, wherein the final rolling temperature of rolling is more than or equal to 850 ℃;
S2, rapidly cooling the 9Cr steel to enable the structure of the 9Cr steel to be converted into quenched martensite, and then directly performing primary tempering treatment;
s3, straightening the steel subjected to primary tempering treatment, and then carrying out stress relief tempering treatment to obtain the 9Cr stainless steel quenched and tempered material for oil gas.
Specifically, in the step S1, the process of preparing the 9Cr steel from the raw materials is basically the same as that of the existing production method, and the finishing temperature of rolling is mainly controlled to be more than or equal to 850 ℃ in the step S1.
The step S2 and the step S3 are different from the traditional working procedures, mainly control the finishing temperature and the rapid cooling mode of the 9Cr steel to directly obtain quenched martensite, save the quenching working procedure (cycle is shortened by 1-3 days) in the original technology, adopt two tempering steps (primary tempering treatment and stress-relief tempering treatment) to replace the annealing (cycle is shortened by 4-7 days) and straightening (cycle is shortened by 1-3 days) and peeling and chamfering (cycle is shortened by 1-3 days) in the traditional working procedures, greatly shorten the production cycle and reduce the production cost.
If the finishing temperature of rolling is lower than 850 ℃, the grain size of the material decreases and the impact properties decrease. If the 9Cr steel cannot be cooled rapidly, the transformation of the steel structure is not complete, and a brittle phase is likely to be precipitated.
Meanwhile, the tensile property, impact property and hardness of the 9Cr stainless steel quenched and tempered material for oil gas prepared by the preparation method are not affected basically, and the performance of the 9Cr stainless steel quenched and tempered material for oil gas is equivalent to that of the 9Cr stainless steel quenched and tempered material for oil gas produced by the traditional process.
As an alternative embodiment of the present invention, in step S1, the kind of raw material may be a conventional raw material such as molten iron, scrap steel, alloy, etc.
In step S1, as an alternative embodiment of the present invention, the primary refining is performed by electric furnace, the refining is performed by LF refining, and then vacuum degassing is performed. The inclusion content and the gas content are controlled by primary refining, LF refining and vacuum degassing treatment.
As an alternative embodiment of the present invention, in step S1, continuous casting or die casting is used to achieve control of tissue uniformity.
The rolling can realize the control of the grain size and compactness of the material. As an alternative embodiment of the invention, in step S1, the final rolling temperature of the rolling is greater than or equal to 900 ℃, preferably 900-980 ℃, typically but not limited to 900 ℃, 920 ℃, 940 ℃, 950 ℃, 960 ℃, 980 ℃ or the like.
As an alternative embodiment of the present invention, the cooling rate of the 9Cr steel in step S2 is 300 ℃ or more, preferably 400 ℃ or more, and the typical but non-limiting cooling rate is 300 ℃, 400 ℃, 500 ℃, 600 ℃, 800 ℃, 1000 ℃, 1200 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1700 ℃ or 1800 ℃ or the like.
As an alternative embodiment of the present invention, the rapid cooling is below 150 ℃, such as 145 ℃, 140 ℃, 130 ℃, 120 ℃, 110 ℃, 100 ℃, 90 ℃, 80 ℃, or the like.
As an alternative embodiment of the invention, in the step S2, the 9Cr steel is rapidly cooled to less than 150 ℃ at a cooling speed of more than or equal to 300 ℃ per hour, and is subjected to primary tempering treatment within 48 hours.
By defining specific process parameters of the rapid cooling process and the interval between rapid cooling and primary tempering, the tissue can be ensured to be fully transformed into quenched martensite.
As an alternative embodiment of the invention, the rapid cooling mode comprises any one of air cooling, air cooling or water cooling.
In step S2, the tempering temperature of the primary tempering treatment is 550-750 ℃, such as 550 ℃, 565 ℃, 580 ℃, 600 ℃, 620 ℃, 640 ℃, 650 ℃, 660 ℃, 680 ℃, 700 ℃, 720 ℃, 740 ℃, 750 ℃, or the like.
Different tempering temperatures are selected for the steel materials with different grades. As an alternative embodiment of the invention, in the step S2, for the 9Cr stainless steel quenched and tempered material of 80KSI, the tempering temperature of one tempering treatment is 650-750 ℃;
For the 9Cr stainless steel quenched and tempered material with 100KSI, the tempering temperature of one tempering treatment is 565-650 ℃;
For the tempering material of the 9Cr stainless steel with 110KSI, the tempering temperature of one tempering treatment is 565-620 ℃.
As an alternative embodiment of the invention, in step S2, the temperature rising rate of rising the temperature to the tempering temperature in the primary tempering treatment is less than or equal to 80 ℃ per hour.
The surface to core temperature of the steel is mainly heated by heat conduction, and the surface to temperature is too fast, but the core temperature also needs a long time to reach the temperature, and the phenomenon is more obvious when the specification is larger. The temperature rise rate is limited to not higher than 80 ℃ per hour according to production practice experience, but the temperature rise rate cannot be infinitely low in general, otherwise the production time and cost are affected. Generally, the temperature rise rate is 50-80 ℃ per hour.
As an alternative embodiment of the invention, the tempering heat preservation time of one tempering treatment is (4H/100 mm x D) to (4H/100 mm x D+6H), wherein H represents hours, and D represents the diameter (outer diameter) of the 9Cr steel material and mm. For example, when the diameter of the 9Cr steel is 100mm, the tempering heat preservation time is 4-10 hours according to the above formula, when the diameter of the 9Cr steel is 200mm, the tempering heat preservation time is 8-14 hours, and so on.
In step S2, the primary tempering is performed by discharging air cooling.
Too high a tempering temperature of the stress relief tempering treatment may change the properties of the material, and too low a tempering temperature of the stress relief tempering treatment may not achieve the stress relief effect. As an alternative embodiment of the present invention, in step S3, the tempering temperature of the stress relief tempering treatment is 20-60 ℃ lower than the tempering temperature of the primary tempering treatment.
As an alternative embodiment of the invention, in the step S3, the temperature rising rate of rising to the tempering temperature is less than or equal to 80 ℃ per hour during the stress relief tempering treatment.
As an alternative embodiment of the invention, in the step S3, the stress-relief tempering heat preservation time is (4H/100 mm D) - (4H/100 mm D+5H), wherein H represents hours, and D represents the diameter (outer diameter) of the steel material, and mm. For example, when the diameter of the 9Cr steel is 100mm, the tempering heat preservation time is 4 to 9 hours according to the above formula, when the diameter of the 9Cr steel is 200mm, the tempering heat preservation time is 8 to 13 hours, and so on.
In step S3, the cooling mode of the stress relief tempering treatment is tapping air cooling.
According to a second aspect of the invention, there is also provided a 9Cr stainless steel quenched and tempered material for oil gas, which is manufactured by the manufacturing method of the 9Cr stainless steel quenched and tempered material for oil gas;
The 9Cr stainless steel quenched and tempered material for oil gas comprises the following chemical components, by mass, less than or equal to 0.15% of C, less than or equal to 1.00% of Si, 0.30-0.60% of Mn, less than or equal to 0.020% of P, less than or equal to 0.010% of S, 8.00-10.00% of Cr, less than or equal to 0.50% of Ni, 0.90-1.10% of Mo, and the balance of Fe and unavoidable impurities.
As an alternative embodiment of the invention, the 9Cr stainless steel quenched and tempered material for oil gas comprises the following chemical components, by mass, 0.09-0.15% of C, less than or equal to 1.00% of Si, 0.30-0.60% of Mn, less than or equal to 0.015% of P, less than or equal to 0.004% of S, 8.50-9.50% of Cr, less than or equal to 0.45% of Ni, 0.90-1.05% of Mo, and the balance of Fe and unavoidable impurities.
According to a third aspect of the present invention, there is also provided a pipe for an oil and gas well, which is made of the above-mentioned 9Cr stainless steel quenched and tempered material for oil and gas or the above-mentioned 9Cr stainless steel quenched and tempered material for oil and gas.
In view of the advantages of the oil gas 9Cr stainless steel quenched and tempered material, the manufactured oil gas well pipe fitting has the same advantages.
The present invention will be described in detail below with reference to the drawings and examples of the present invention. The examples are provided by way of explanation of the invention and not limitation of the invention. Indeed, it will be apparent to those skilled in the art that modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For example, features illustrated or described as part of one embodiment can be used on another embodiment to yield still a further embodiment. Accordingly, it is intended that the present invention encompass such modifications and variations as fall within the scope of the appended claims and their equivalents.
Example 1
The embodiment provides a 9Cr stainless steel quenched and tempered material for oil and gas, which is used for producing round steel with the specification of 80KSI steel grade and phi 210mm, wherein the main chemical components of the steel grade and the content (wt%) thereof are 0.10 percent of C, 0.31 percent of Si, 0.47 percent of Mn, 0.018 percent of P, 0.003 percent of S, 8.61 percent of Cr, 0.11 percent of Ni, 0.92 percent of Mo, and the balance of Fe and unavoidable impurities.
Specifically, the manufacturing method of the stainless steel quenched and tempered material of the embodiment 9Cr comprises the following steps:
S1, preparing steel, namely sequentially carrying out electric furnace smelting, LF refining, vacuum degassing, continuous casting, red feeding, heating and rolling on raw materials to obtain 9Cr round steel, wherein the final rolling temperature is 926 ℃;
S2, rapidly cooling the 9Cr round steel product obtained in the step S1 through a water tank, cooling to 50 ℃ for 30min, carrying out water outlet rewarming on the 9Cr round steel product to 72 ℃, standing for 26h, and carrying out primary tempering treatment in a tempering furnace;
Primary tempering, namely heating 9Cr round steel to the tempering temperature of 720 ℃ at the heating rate of 75 ℃ per hour, preserving heat for 13 hours, discharging from a furnace for air cooling after the heat preservation is finished, and finishing primary tempering;
S3, straightening, namely straightening the steel billet subjected to primary tempering treatment;
and (3) stress-relief tempering treatment, namely heating the straightened 9Cr round steel to the stress-relief tempering temperature of 690 ℃ at the heating rate of 75 ℃ per hour, preserving heat for 13 hours, discharging from a furnace for air cooling after preserving heat, and obtaining the 9Cr stainless steel quenched and tempered material.
Example 2
The embodiment provides a 9Cr stainless steel quenched and tempered material for oil and gas, which is used for producing round steel with 110KSI steel grade and phi 90mm, wherein the steel comprises the main chemical components of 0.09 percent of C, 0.32 percent of Si, 0.51 percent of Mn, 0.017 percent of P, 0.002 percent of S, 9.10 percent of Cr, 0.09 percent of Ni, 0.97 percent of Mo, and the balance of Fe and unavoidable impurities.
Specifically, the manufacturing method of the stainless steel quenched and tempered material of the embodiment 9Cr comprises the following steps:
s1, preparing steel, namely sequentially performing primary refining on raw materials in an electric furnace, secondary refining in an LF furnace, vacuum degassing, continuous casting, red feeding, heating and rolling to obtain 9Cr round steel, wherein the final rolling temperature is 934 ℃;
s2, rapidly cooling the 9Cr round steel product prepared in the step S1 to 80 ℃ at 400 ℃ per hour through air cooling, and then directly entering a tempering furnace for primary tempering treatment;
Primary tempering, namely heating 9Cr round steel to a tempering temperature of 595 ℃ at a heating rate of 80 ℃ per hour, preserving heat for 6 hours, discharging from a furnace for air cooling after the heat preservation is finished, and finishing primary tempering;
s3, straightening, namely straightening the 9Cr steel subjected to primary tempering treatment;
And (3) stress-relief tempering treatment, namely heating the straightened 9Cr round steel to the stress-relief tempering temperature of 560 ℃ at the heating rate of 80 ℃ per hour, preserving heat for 6 hours, discharging from a furnace for air cooling after preserving heat, and obtaining the 9Cr stainless steel quenched and tempered material.
Comparative example 1
This comparative example provides a 9Cr stainless steel quenched and tempered material for oil and gas, which has the same production specifications, dimensions and chemical composition as in example 1.
The manufacturing method (old process) of the comparative example 9Cr stainless steel quenched and tempered material comprises the following steps:
s1, preparing steel, namely sequentially carrying out electric furnace smelting, primary smelting, LF external refining, vacuum degassing, continuous casting, red feeding, heating and rolling on raw materials to obtain 9Cr round steel, wherein the final rolling temperature is 917 ℃;
S2, annealing, namely annealing the 9Cr round steel material prepared in the step S1 in an annealing furnace, wherein the temperature rising rate of the annealing furnace to the annealing heat preservation temperature is 80 ℃ per hour, the heat preservation temperature of the annealing treatment is 700 ℃ and the heat preservation time is 13 hours;
S3, straightening;
S4, peeling and chamfering;
s5, tempering the 9Cr round steel material transformation tempering line, wherein the quenching temperature is 926 ℃, the heat preservation time is 5 hours, water quenching is performed after discharging, and water quenching billet surface temperature is lower than 100 ℃ and water is discharged;
s6, primary tempering treatment, namely placing the water quenched steel material after water discharge in a tempering furnace, heating to a tempering temperature of 720 ℃ at a heating rate of 75 ℃ per hour, preserving heat for 13 hours, discharging from the furnace for air cooling after the heat preservation is finished, and finishing primary tempering treatment;
s7, straightening, namely straightening the steel subjected to primary tempering treatment;
and (3) stress-relief tempering treatment, namely heating the straightened 9Cr round steel to the stress-relief tempering temperature of 690 ℃ at the heating rate of 75 ℃ per hour, preserving heat for 13 hours, discharging from a furnace for air cooling after preserving heat, and obtaining the 9Cr stainless steel quenched and tempered material.
Comparative example 2
This comparative example provides a 9Cr stainless steel quenched and tempered material for oil and gas, which has the same production specifications, dimensions and chemical composition as in example 2.
The manufacturing method (old process) of the comparative example 9Cr stainless steel quenched and tempered material comprises the following steps:
S1, preparing steel, namely sequentially carrying out electric furnace smelting, primary smelting, LF external refining, vacuum degassing, continuous casting, red feeding, heating and rolling on raw materials to prepare a 9Cr round steel billet, wherein the final rolling temperature is 921 ℃;
S2, annealing, namely annealing the 9Cr round steel material prepared in the step S1 in an annealing furnace, wherein the heating rate of the annealing furnace to the annealing heat preservation temperature is 80 ℃ per hour, the heat preservation temperature of the annealing treatment is 710 ℃ and the heat preservation time is 6 hours;
S3, straightening;
S4, peeling and chamfering;
s5, tempering a 9Cr round steel billet transformation tempering line, wherein the quenching temperature is 934 ℃, the heat preservation time is 5 hours, water quenching is performed after discharging, and water is discharged when the surface temperature of the water quenched billet is lower than 100 ℃;
s6, primary tempering treatment, namely placing the water quenched steel billet after water discharge in a tempering furnace, heating to a tempering temperature of 595 ℃ at a heating rate of 80 ℃ per hour, preserving heat for 6 hours, discharging from the furnace for air cooling after the heat preservation is finished, and finishing primary tempering treatment;
S7, straightening, namely straightening the steel billet subjected to primary tempering treatment;
And (3) stress-relief tempering treatment, namely heating the straightened 9Cr round steel billet to the stress-relief tempering temperature of 560 ℃ at the heating rate of 80 ℃ per hour, preserving heat for 6 hours, discharging from a furnace for air cooling after preserving heat, and obtaining the 9Cr stainless steel quenched and tempered material.
Comparative example 3
This comparative example provides a 9Cr stainless steel quenched and tempered material for oil gas and a method for producing the same, except that the finishing temperature in step S1 was adjusted to 825 ℃.
Comparative example 4
This comparative example provides a 9Cr stainless steel quenched and tempered material for oil gas and a method for producing the same, and the other steps are the same as in example 1 except that the rapid cooling rate in step S2 is adjusted to 30 ℃ per hour with furnace cooling.
In order to compare technical effects of the above-described embodiments and comparative examples, the following experimental examples were specially set.
Experimental example 1
The metallographic structures of the 9Cr stainless steel quenched and tempered materials for oil gas, which are provided in each example and comparative example, are analyzed, and specific reference is made to fig. 1-4. As can be seen from fig. 1 and 3, the oil and gas 9Cr stainless steel tempers of example 1 and comparative example 1 obtained substantially the same grain size. As can be seen from fig. 2 and 4, the grain sizes of the 9Cr stainless steel quenched and tempered materials for oil gas of example 2 and comparative example 2 are also substantially equivalent.
Experimental example 2
Samples were taken at 1/2R of the 9Cr steels (80 KSI) prepared in example 1 and comparative example 1, comparative example 3 and comparative example 4, and room temperature tensile properties and low temperature impact properties were tested according to ASTM A370 and ASTM E23, and the actual data pair are shown in Table 1:
TABLE 1
Meanwhile, samples were taken at 1/2R of the 9Cr steels (110 KSI) prepared in example 2 and comparative example 2, and room temperature tensile properties and low temperature impact properties were tested according to ASTM A370 and ASTM E23, and the actual data pair are shown in Table 2:
TABLE 2
As can be seen from the data in Table 1, the 9Cr stainless steel quenched and tempered materials for oil gas prepared in the embodiment 1 and the comparative example 1 have excellent tensile and impact properties, but the production period of the embodiment 1 is shortened by about 4 days, the production efficiency is remarkably improved, and the method has obvious cost advantages.
Comparing comparative examples 3 and 4 with example 1, it is known that when the finishing temperature is too low (below 850 ℃), the impact properties of the 9Cr stainless steel quenched and tempered material are significantly reduced, mainly due to the reduction in the grain size of the material. When the 9Cr steel cannot be cooled rapidly (the cooling rate is too low), since the transformation of the steel structure is incomplete and a brittle phase is precipitated, impact properties and hardness are also significantly reduced.
As can be seen from the data in Table 2, the 9Cr stainless steel for oil gas prepared in example 2 and comparative example 2 according to the present invention has comparable tensile properties and hardness, except that the impact properties of example 2 are slightly lower than those of comparative example 2, but are far higher than the standard requirements. And because a plurality of working procedures are regulated or omitted, the production period of the embodiment 2 of the invention is obviously shortened compared with that of the comparative example 2, the production cost is obviously reduced, and the aims of reducing the cost and enhancing the efficiency are achieved.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1.一种油气用9Cr不锈钢调质材的制造方法,其特征在于,包括以下步骤:1. A method for manufacturing a 9Cr stainless steel tempered material for oil and gas applications, characterized by comprising the following steps: S1. 按油气用9Cr不锈钢调质材的化学成分将原料依次进行初炼、精炼、真空脱气、连铸或模铸、退火或红送、加热和轧制,得到9Cr钢材;S1. According to the chemical composition of 9Cr stainless steel tempered material for oil and gas, the raw materials are subjected to primary refining, refining, vacuum degassing, continuous casting or ingot casting, annealing or hot-pressing, heating and rolling in sequence to obtain 9Cr steel. S2. 将所述9Cr钢材快速冷却以使其组织转变为淬火马氏体,然后直接进行一次回火处理;S2. The 9Cr steel is rapidly cooled to transform its microstructure into quenched martensite, and then directly subjected to a tempering treatment. S3. 将一次回火处理后的钢材进行矫直,然后进行去应力回火处理,得到油气用9Cr不锈钢调质材;S3. Straighten the steel after the first tempering treatment, and then perform stress-relief tempering treatment to obtain 9Cr stainless steel tempered material for oil and gas. 步骤S1中,轧制的终轧温度≥920℃;In step S1, the final rolling temperature is ≥920℃; 步骤S2中,将所述9Cr钢材以≥300℃/h的冷却速度快速冷却至150℃以下,并于48h内进行一次回火处理;In step S2, the 9Cr steel is rapidly cooled to below 150°C at a cooling rate of ≥300°C/h, and then tempered once within 48 hours. 步骤S2中,所述一次回火处理的回火温度为550~750℃,一次回火保温时间为(4H/100mm*D)~(4H/100mm*D+6H),其中H代表小时,D代表9Cr钢材的直径,mm;In step S2, the tempering temperature of the first tempering treatment is 550~750℃, and the first tempering holding time is (4H/100mm*D)~(4H/100mm*D+6H), where H represents hours and D represents the diameter of 9Cr steel in mm. 步骤S3中,所述去应力回火处理的回火温度低于一次回火处理的回火温度20-60℃,去应力回火保温时间为(4H/100mm*D)~(4H/100mm*D+5H),其中H代表小时,D代表钢材的直径,mm;In step S3, the tempering temperature of the stress-relief tempering treatment is 20-60℃ lower than the tempering temperature of the primary tempering treatment, and the stress-relief tempering holding time is (4H/100mm*D)~(4H/100mm*D+5H), where H represents hours and D represents the diameter of the steel in mm. 所述油气用9Cr不锈钢调质材,包括如下质量分数的化学成分:C:≤0.15%、Si:≤1.00%、Mn:0.30~0.60%、P:≤0.020%、S:≤0.010%、Cr:8.00~10.00%、Ni:≤0.50%、Mo:0.90~1.10%,其余为Fe及不可避免的杂质。The 9Cr stainless steel tempered material for oil and gas applications comprises the following chemical composition by mass fraction: C: ≤0.15%, Si: ≤1.00%, Mn: 0.30~0.60%, P: ≤0.020%, S: ≤0.010%, Cr: 8.00~10.00%, Ni: ≤0.50%, Mo: 0.90~1.10%, with the remainder being Fe and unavoidable impurities. 2.根据权利要求1所述的油气用9Cr不锈钢调质材的制造方法,其特征在于,2. The method for manufacturing 9Cr stainless steel tempered material for oil and gas applications according to claim 1, characterized in that, 步骤S2中,快速冷却的方式包括空冷、风冷或水冷。In step S2, rapid cooling methods include air cooling, air cooling, or water cooling. 3.根据权利要求1所述的油气用9Cr不锈钢调质材的制造方法,其特征在于,3. The method for manufacturing 9Cr stainless steel tempered material for oil and gas applications according to claim 1, characterized in that, 步骤S2中,所述一次回火处理时升温至回火温度的升温速率≤80℃/h;In step S2, the heating rate to the tempering temperature during the first tempering process is ≤80℃/h; 和/或,步骤S2中,所述一次回火处理的冷却方式为出炉空冷。And/or, in step S2, the cooling method for the primary tempering process is air cooling after exiting the furnace. 4.根据权利要求1所述的油气用9Cr不锈钢调质材的制造方法,其特征在于,步骤S2中,对于80KSI的9Cr不锈钢调质材,所述一次回火处理的回火温度为650-750℃;4. The manufacturing method of 9Cr stainless steel tempered material for oil and gas according to claim 1, characterized in that, in step S2, for 80KSI 9Cr stainless steel tempered material, the tempering temperature of the first tempering treatment is 650-750℃. 和/或,步骤S2中,对于100KSI的9Cr不锈钢调质材,所述一次回火处理的回火温度为565-650℃;And/or, in step S2, for 9Cr stainless steel quenched and tempered material of 100KSI, the tempering temperature of the first tempering treatment is 565-650℃. 和/或,步骤S2中,对于110KSI的9Cr不锈钢调质材,所述一次回火处理的回火温度为565-620℃。And/or, in step S2, for 9Cr stainless steel quenched and tempered material of 110KSI, the tempering temperature of the first tempering treatment is 565-620℃. 5.根据权利要求1所述的油气用9Cr不锈钢调质材的制造方法,其特征在于,步骤S3中,所述去应力回火处理时升温至回火温度的升温速率≤80℃/h;5. The method for manufacturing 9Cr stainless steel tempered material for oil and gas according to claim 1, characterized in that, in step S3, the heating rate to the tempering temperature during the stress-relief tempering treatment is ≤80℃/h. 和/或,步骤S3中,所述去应力回火处理的冷却方式为出炉空冷。And/or, in step S3, the cooling method for the stress-relief tempering treatment is air cooling after exiting the furnace. 6.根据权利要求1所述的油气用9Cr不锈钢调质材的制造方法,其特征在于,所述油气用9Cr不锈钢调质材,包括如下质量分数的化学成分:C:0.09-0.15%、Si:≤1.00%、Mn:0.30~0.60%、P:≤0.015%、S:≤0.004%、Cr:8.50~9.50%、Ni:≤0.45%、Mo:0.90~1.05%,其余为Fe及不可避免的杂质。6. The manufacturing method of the 9Cr stainless steel tempered material for oil and gas according to claim 1, characterized in that the 9Cr stainless steel tempered material for oil and gas comprises the following chemical composition by mass fraction: C: 0.09-0.15%, Si: ≤1.00%, Mn: 0.30~0.60%, P: ≤0.015%, S: ≤0.004%, Cr: 8.50~9.50%, Ni: ≤0.45%, Mo: 0.90~1.05%, with the remainder being Fe and unavoidable impurities. 7.一种油气井用管件,其特征在于,采用权利要求1-6任一项所述的制造方法制得的油气用9Cr不锈钢调质材制成。7. A pipe fitting for oil and gas wells, characterized in that it is made of 9Cr stainless steel tempered material for oil and gas wells, obtained by the manufacturing method described in any one of claims 1-6.
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