CN106011627B - A kind of ultralow temperature pressure vessel quenched high strength alloy steel 06Ni9DR steel plates and preparation method thereof - Google Patents

A kind of ultralow temperature pressure vessel quenched high strength alloy steel 06Ni9DR steel plates and preparation method thereof Download PDF

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CN106011627B
CN106011627B CN201610519015.8A CN201610519015A CN106011627B CN 106011627 B CN106011627 B CN 106011627B CN 201610519015 A CN201610519015 A CN 201610519015A CN 106011627 B CN106011627 B CN 106011627B
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molten iron
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康文举
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Nanyang Hanye Special Steel Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/08Ferrous alloys, e.g. steel alloys containing nickel
    • 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
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0221Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
    • C21D8/0226Hot rolling
    • 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
    • C21D8/02Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
    • C21D8/0247Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/001Ferrous alloys, e.g. steel alloys containing N
    • 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
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/12Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/16Ferrous alloys, e.g. steel alloys containing copper
    • 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

Abstract

A kind of ultralow temperature pressure vessel quenched high strength alloy steel 06Ni9DR steel plates and preparation method thereof, the steel plate includes the chemical composition (unit, wt%) of following mass percent:C:0.01‑0.06、Si:0.10‑0.20、Mn:0.50‑0.80、P:≤0.008、S:≤0.002、Ni:8.5 9.5, Cu≤0.10, Mo≤0.10, V≤0.005, Cr≤0.25, surplus are Fe and inevitable impurity.A kind of ultralow temperature pressure vessel of the present invention passes through rational Design of Chemical Composition with quenched high strength alloy steel 06Ni9DR steel plates, RH+LF+RH techniques cause the cleanliness factor of steel to cooperate with effective technique effectively to implement, the steel plate of preparation has high intensity, excellent low-temperature flexibility, good postwelding performance the features such as.

Description

A kind of ultralow temperature pressure vessel with quenched high strength alloy steel 06Ni9DR steel plates and its Preparation method
Technical field
The present invention relates to a kind of steel heavy plate for pressure vessels and preparation method thereof, more particularly, to a kind of ultralow temperature pressure vessel With quenched high strength alloy steel 06Ni9DR steel plates and preparation method thereof.
Background technology
06Ni9DR steel is commonly called as 9%Ni steel, Ni9 steel, 9Ni steel etc., be containing Ni for 8.5-9.5% extremely low temperature tank and The quenched high strength alloy steel of pressure vessel, is the important feature material of ultralow temperature equipment and container, is widely used in manufacture or builds Liquid making nitrogen and natural gas (Liquefied Natural Gas:Abbreviation LNG) storage tank.Such as the LNG ship and storage liquid of liquified natural gas The storage tank of state natural gas will use substantial amounts of cryogenic steel 06Ni9DR.It has high yield strength and tensile strength, good Low-temperature flexibility and welding performance the features such as, the steel for low-temperature pressure container that uses of the country because production difficulty is larger, it is most of according to Rely import.
Application No. CN201510407667.8 Chinese patent discloses pressure vessel under a kind of -196 DEG C of cryogenic conditions With low nickel steel plate and its production method, the component and weight percent content of the steel plate are:C≤0.04, Si≤0.05, Mn: 1.60~2.50, P≤0.005, S≤0.003, Alt:0.015~0.050, Ni:6.00~8.00, Cu:0.35~0.50, Cr: 0.55~1.00, N≤0.004;Additionally containing one kind in Mo≤0.35, Nb≤0.05, Ti≤0.025, Ca≤0.005 or More than one combination of person, surplus is Fe and is inevitably mingled with, but patent Ni contents are 6.00~8.00, therefore is prepared Steel plate there is no sufficient intensity and toughness, it is not good enough as extremely low temperature tank and steels for pressure vessel use properties.Application number A kind of Low-temperature high-nickel steel plate and its manufacture method are disclosed for 201210276343.1 Chinese patent, involved steel has following Composition and mass percent are C:0.03~0.05%, Si:0~0.35%, Mn:0.50~0.80%, Ni:11.0~ 13.0%, P≤0.005%, S≤0.005%, Al:0.01~0.05%, O≤0.0012%, N≤0.0035%, remaining is Fe With inevitable impurity.It will be evident that Ni contents are higher in the chemical composition for the steel plate that the patent is made, while not carrying out micro- conjunction Aurification.
The content of the invention
In view of this, the purpose of the present invention is that there is provided a kind of ultralow temperature pressure vessel tune in view of the shortcomings of the prior art Matter high strength alloy steel 06Ni9DR steel plates and preparation method thereof, it is larger to solve domestic 06Ni9DR Plate Productions difficulty, big portion The problem of dividing dependence on import.
To reach above-mentioned purpose, the present invention uses following technical scheme:
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.01-0.06、Si:0.10-0.20、Mn:0.50-0.80、P:≤0.008、S:≤ 0.002、Ni:8.5-9.5, Cu≤0.10, Mo≤0.10, V≤0.005, Cr≤0.25, Als≤0.025%, N≤0.012%, Surplus is Fe and inevitable impurity.
Further, the steel plate includes the chemical composition (unit, wt%) of following mass percent:C:0.02-0.04、 Si:0.13-0.16、Mn:0.65-0.75、P:≤0.006、S:≤0.002、Ni:8.6-9.4、Cu≤0.08、Mo≤0.60、V ≤ 0.003, Cr≤0.18, Als≤0.015%, N≤0.009%, surplus are Fe and inevitable impurity.
Further, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the steel plate≤ 0.50%.
Further, the thickness of the steel plate is 12mm-50mm.
Its preparation method, comprises the following steps:
(1) KR molten iron is pre-processed:Molten iron is taken up with ladle, the molten iron that arrives at a station takes off P, S content, molten iron in preceding slag, control molten iron Molten iron P≤0.1%, S≤0.004% after KR stirring desulphurizations, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates Slag after taking off to the greatest extent, liquid level thickness of slag layer≤20mm;
(2) converter smelting:Carried out in 150 tons of converters, smelt dispensing according to steel scrap 4.5-4.8t, Ni plate 13-14t, iron Water 149-151t, total dispensing 165-170t are controlled, S≤0.0030% in the molten iron, P≤0.080%, Si≤0.45, C≤ 0.04%th, Mn≤0.7, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap uses leftover pieces;Go out Slag is tapped before being kept off before steel with floating plug, and tapping is used in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process before terminating Whole Argon;
(3) RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 20-30min, works as steel Go out station when hydrogen content is less than 2.0ppm in water, ladle uses carbon-free covering agent in RH vacuum metlings, at the end of RH vacuum metlings Liquid steel temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4) LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.05-0.06%, refining In 0.03-0.04%;S refines terminal point control in below 8ppm;1635-1645 DEG C of liquid steel temperature, soft blow are controlled at the end of refining Time >=2min;
(5) RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 18-22min, when hydrogen in molten steel Content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent in RH vacuum metlings, molten steel temperature at the end of RH vacuum metlings Spend for 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6) ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7) continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:0.7-1.0m/ Molten steel face not show is kept in min, continuous-casting steel pouring whole process blowing argon casting, middle bag casting process;Plug is controlled in steel pouring process Rod Argon amount, liquid level fluctuation of crystallizer is slight;
(8) cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is to thickness 140mm or so, to table Face is cleared up, and clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤ 1200℃;1150-1160 DEG C of soaking temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9) rear retarded cooling process is rolled:According to the difference of steel plate thickness, different section coolings is used after rolling, it is cold by adjusting But collector group number, controls red temperature a:Thickness 12-35mm red temperature is between 650-750 DEG C, b:Thickness 35-50mm's Red temperature is between 650-690 DEG C;
(10) ultrasonic examination:Steel plate is detected using supersonic detector;
(11) Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate Thickness≤12mm, using double normalizing+tempering process;Steel plate thickness>12mm, using quenching+tempering technique twice.
Further, ladle described in step (1) is the early stage bag at 3-l5 times using bag age.
Further, the temperature of tempering process described in step (11) Technology for Heating Processing is controlled at 560-580 DEG C.
The beneficial effects of the invention are as follows:
A kind of ultralow temperature pressure vessel of the present invention passes through rational chemistry with quenched high strength alloy steel 06Ni9DR steel plates Composition design, the cleanliness factor that RH+LF+RH techniques carry out steel cooperates with effective technique effectively to implement, and successfully have developed less In the thick low-temperature pressure container 06Ni9DR steel plates of 50mm, the steel plate of preparation can not only meet the requirement of national standard, and compared with national standard There is very big surplus, the features such as with high intensity, excellent low-temperature flexibility, good postwelding performance, steel plate residual induction is small In l0Cs, site operation can be met, avoid producing the requirement of welding arc blow, plate quality reaches, has been even more than both at home and abroad The advanced level in kind of like product, specifically have it is following some:
(1) a kind of ultralow temperature pressure vessel of the invention is with quenched high strength alloy steel 06Ni9DR steel plates, in its chemical composition Ni mass percent is 8.5-9.5%, and the chemical composition of analysis low-temperature pressure steel plate is understood, Ni is while improving armor plate strength With the element of toughness, grope by many experiments of the applicant in laboratory and put into practice production checking, find to work as low temperature pressure When Ni contents do not reach 8.5% in power steel plate, its intensity of the steel plate of preparation and toughness are not abundant enough, as Ni in low-temperature pressure steel plate After content is more than 9.5%, the very slow thermal hysteresis simultaneously of atoms permeatings of the Ni in steel plate are serious, influence low-temperature pressure steel plate Intensity and toughness, while as excessive Ni addition, adds the production cost of low-temperature pressure steel plate.Therefore, originally Invention prepares the steel plate that Ni mass percents are 8.5-9.5%, both with excellent intensity and tough after long-felt Degree, while reducing the production cost of steel plate again.
(2) a kind of ultralow temperature pressure vessel of the invention is with quenched high strength alloy steel 06Ni9DR steel plates, take low-carbon and Microalloy treatment, making the low-temperature pressure steel plate of preparation has good cryogenic property.C weight/mass percentage composition is in steel plate C≤0.03%, the low temperature that not only steel plate of the present invention had had enough intensity and will not excessively destroy steel plate because of C content again is tough Property and welding performance.On the other hand, steel plate of the invention uses microalloy treatment technology, adds tri- kinds appropriate of Cu, V, Cr Metallic element, and appropriate Als content is controlled, with low-temperature flexibility;The Ni in steel plate is cooperateed with, the strong of steel plate is further increased Degree, improves the welding performance of steel plate.
(3) RH+LF+RH techniques of the present invention carry out the cleanliness factor of steel, twice RH technical process, collaboration the present invention in cogging, Rolling, quenching (normalizing), quenching (normalizing), effective implementation of the technique such as tempering process, the P and S of the steel plate of the invention prepared Content difference as little as P≤0.008%, S≤0.002%, compared with prior art, steel plate P, S content prepared by the present invention is very It is low, therefore effectively prevent the defects such as surface of steel plate pattern cracking, subcrack and center porosity, the low-temperature pressure steel of preparation Plate lumber recovery is high, the low-temperature flexibility superior performance of steel plate.
(4) a kind of ultralow temperature pressure vessel of the invention with quenched high strength alloy steel 06Ni9DR steel plates in preparation process In, it is strict to wrap age in the early stage bag of 3-l5 times as ladle using use, realize and kept away when molten iron, molten steel are shifted between each station Exempt from impurity element to enter in molten iron or molten steel, effectively reduce the content of inevitable impurity in the steel plate prepared.
Embodiment
Embodiment 1
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.01、Si:0.20、Mn:0.50、P:0.006、S:0.002、Ni:8.5、Cu:0.10、Mo: 0.01、V:0.005、Cr:0.10、Als:0.015、N:0.012, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.10%, steel plate thickness is 12mm.
Its preparation method, comprises the following steps:
(1) KR molten iron is pre-processed:Molten iron is taken up with ladle, the molten iron that arrives at a station takes off P, S content, molten iron in preceding slag, control molten iron Molten iron P≤0.1%, S≤0.004% after KR stirring desulphurizations, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates Slag after taking off to the greatest extent, liquid level thickness of slag layer≤20mm;
(2) converter smelting:In 150 tons of converters carry out, smelt dispensing according to steel scrap 4.5t, Ni plate 14t, molten iron 149t, Total dispensing 167.5t is controlled, it is desirable to S≤0.0030%, P≤0.080%, Si≤0.45, C≤0.04%, Mn in the molten iron ≤ 0.7, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap strictly uses high-quality leftover pieces;Tapping Preceding to keep off preceding slag tapping with floating plug, tapping is used in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process before terminating and wanted Journey of demanding perfection Argon;
(3) RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 20min, when in molten steel Hydrogen content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent, molten steel at the end of RH vacuum metlings in RH vacuum metlings Temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4) LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.05%, refining 0.04%;S refines terminal point control in below 8ppm, and S content is detected using carbon and sulfur analytical instrument;Molten steel temperature is controlled at the end of refining 1635-1645 DEG C of degree, soft blow time 5min;
(5) RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 22min, when hydrogen content in molten steel Go out station during less than 2.0ppm, ladle uses carbon-free covering agent in RH vacuum metlings, and liquid steel temperature is at the end of RH vacuum metlings 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6) ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7) continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:0.7m/min, Continuous-casting steel pouring requires to keep molten steel face not show in whole blowing argon casting, middle bag casting process;Rationally controlled in steel pouring process Stopper Argon amount processed, liquid level fluctuation of crystallizer is slight;
(8) cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is entered to thickness 140mm to surface Row cleaning, clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤1200 ℃;1150-1160 DEG C of soaking temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9) rear retarded cooling process is rolled:According to the difference of steel plate thickness, different section coolings is used after rolling, it is cold by adjusting But collector group number, controls red temperature, and thickness 12mm red temperature is controlled between 650~750 DEG C;
(10) ultrasonic examination:Steel plate is detected using supersonic detector;
(11) Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate Thickness 12mm, using double normalizing+tempering process, temperature is controlled at 560-580 DEG C.
Ladle is the early stage bag at l5 times using bag age wherein described in step (1).
Embodiment 2
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.03、Si:0.14、Mn:0.69、P:0.005、S:0.001、Ni:9.4、Cu:0.01、Mo: 0.01、V:0.003、Cr:0.25、Als:0.020、N:0.00189, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.50%, steel plate thickness is 40mm.
Its preparation method, comprises the following steps:
(1) KR molten iron is pre-processed:Molten iron is taken up with ladle, the molten iron that arrives at a station takes off P, S content, molten iron in preceding slag, control molten iron Molten iron P≤0.1%, S≤0.004% after KR stirring desulphurizations, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates Slag after taking off to the greatest extent, liquid level thickness of slag layer≤20mm;
(2) converter smelting:In 150 tons of converters carry out, smelt dispensing according to steel scrap 4.8t, Ni plate 13t, molten iron 151t, Total dispensing 168.8t is controlled, S≤0.0030% in the molten iron, P≤0.080%, Si≤0.45, C≤0.04%, Mn≤ 0.7, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap uses leftover pieces;Floating plug is used before tapping Slag tapping before gear, tapping uses whole Argon in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process before terminating;
(3) RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 30min, when in molten steel Hydrogen content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent, molten steel at the end of RH vacuum metlings in RH vacuum metlings Temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4) LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.06%, refining 0.03%;S refines terminal point control in below 8ppm;1635-1645 DEG C of liquid steel temperature, soft blow time are controlled at the end of refining 2min;
(5) RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 18min, when hydrogen content in molten steel Go out station during less than 2.0ppm, ladle uses carbon-free covering agent in RH vacuum metlings, and liquid steel temperature is at the end of RH vacuum metlings 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6) ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7) continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:1.0m/min, Molten steel face not show is kept in continuous-casting steel pouring whole process blowing argon casting, middle bag casting process;Stopper is controlled to blow in steel pouring process Argon amount, liquid level fluctuation of crystallizer is slight;
(8) cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is entered to thickness 140mm to surface Row cleaning, clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤1200 ℃;1150-1160 DEG C of soaking temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9) rear retarded cooling process is rolled:According to the difference of steel plate thickness, steel plate thickness is 40mm, and different laminar flows is used after rolling Cooling, by adjusting cooling manifold group number, red temperature is controlled between 650-690 DEG C;
(10) ultrasonic examination:Steel plate is detected using supersonic detector;
(11) Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate Thickness is 40mm, and using quenching+tempering technique twice, temperature is controlled at 560-580 DEG C.
Ladle is the early stage bag at 3 times using bag age wherein described in step (1).
Embodiment 3
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.03、Si:0.14、Mn:0.68、P:0.005、S:0.001、Ni:9.4、Cu:0.09、Mo: 0.01、V:0.003、Cr:0.20、Als:0.020、N:0.00195, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.15%, steel plate thickness is 50mm.
Its preparation method, comprises the following steps:
(1) KR molten iron is pre-processed:Molten iron is taken up with ladle, the molten iron that arrives at a station takes off P, S content, molten iron in preceding slag, control molten iron Molten iron P≤0.1%, S≤0.004% after KR stirring desulphurizations, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates Slag after taking off to the greatest extent, liquid level thickness of slag layer≤20mm;
(2) converter smelting:In 150 tons of converters carry out, smelt dispensing according to steel scrap 4.6t, Ni plate 14t, molten iron 150t, Total dispensing 168.6t is controlled, S≤0.0030% in the molten iron, P≤0.080%, Si≤0.45, C≤0.04%, Mn≤ 0.7, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap uses leftover pieces;Floating plug is used before tapping Slag tapping before gear, tapping uses whole Argon in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process before terminating;
(3) RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 25min, when in molten steel Hydrogen content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent, molten steel at the end of RH vacuum metlings in RH vacuum metlings Temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4) LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.06%, refining 0.03%;S refines terminal point control in below 8ppm, and S content is detected using carbon and sulfur analytical instrument;Molten steel temperature is controlled at the end of refining 1635-1645 DEG C of degree, soft blow time 6min;
(5) RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 17min, when hydrogen content in molten steel Go out station during less than 2.0ppm, ladle uses carbon-free covering agent in RH vacuum metlings, and liquid steel temperature is at the end of RH vacuum metlings 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6) ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7) continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:0.8m/min, Molten steel face not show is kept in continuous-casting steel pouring whole process blowing argon casting, middle bag casting process;Stopper is controlled to blow in steel pouring process Argon amount, liquid level fluctuation of crystallizer is slight;
(8) cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is entered to thickness 140mm to surface Row cleaning, clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤1200 ℃;1150-1160 DEG C of soaking temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9) rear retarded cooling process is rolled:According to the difference of steel plate thickness, steel plate thickness is 50mm, and different laminar flows is used after rolling Cooling, by adjusting cooling manifold group number, red temperature is controlled between 650~690 DEG C;
(10) ultrasonic examination:Steel plate is detected using supersonic detector;
(11) Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate Thickness is 50mm, and using quenching+tempering technique twice, temperature is controlled at 560-580 DEG C.
Ladle is the early stage bag at 15 times using bag age wherein described in step (1).
Embodiment 4
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.05、Si:0.15、Mn:0.65、P:0.004、S:0.0015、Ni:9.0、Cu:0.06、 Mo:0.05、V:0.003、Cr:0.12、Als:0.010、N:0.00843, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.25%, steel plate thickness is 30mm.
Its preparation method, comprises the following steps:
(1) KR molten iron is pre-processed:Molten iron is taken up with ladle, the molten iron that arrives at a station takes off P, S content, molten iron in preceding slag, control molten iron Molten iron P≤0.1%, S≤0.004% after KR stirring desulphurizations, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates Slag after taking off to the greatest extent, liquid level thickness of slag layer≤20mm;
(2) converter smelting:Carried out in 150 tons of converters, smelt dispensing according to steel scrap 4.7t, Ni plate 13.5t, molten iron 150t, total dispensing 168.2t are controlled, S≤0.0030% in the molten iron, P≤0.080%, Si≤0.45, C≤0.04%, Mn≤0.7, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap uses leftover pieces;The preceding gear of tapping Slag tapping before slag plug gear, tapping uses whole process in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process to blow before terminating Argon;
(3) RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 25min, when in molten steel Hydrogen content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent, molten steel at the end of RH vacuum metlings in RH vacuum metlings Temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4) LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.06%, refining 0.03%;S refines terminal point control in below 8ppm;1635-1645 DEG C of liquid steel temperature, soft blow time are controlled at the end of refining 4min;
(5) RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 17min, when hydrogen content in molten steel Go out station during less than 2.0ppm, ladle uses carbon-free covering agent in RH vacuum metlings, and liquid steel temperature is at the end of RH vacuum metlings 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6) ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7) continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:0.9m/min, Molten steel face not show is kept in continuous-casting steel pouring whole process blowing argon casting, middle bag casting process;Stopper is controlled to blow in steel pouring process Argon amount, liquid level fluctuation of crystallizer is slight;
(8) cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is entered to thickness 140mm to surface Row cleaning, clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤1200 ℃;1150-1160 DEG C of soaking temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9) rear retarded cooling process is rolled:According to the difference of steel plate thickness, steel plate thickness is 30mm, and different laminar flows is used after rolling Cooling, by adjusting cooling manifold group number, red temperature is controlled between 650~750 DEG C;
(10) ultrasonic examination:Steel plate is detected using supersonic detector;
(11) Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate Thickness is 30mm, and using quenching+tempering technique twice, temperature is controlled at 560-580 DEG C.
Ladle is the early stage bag at 9 times using bag age wherein described in step (1).
Embodiment 5
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.04、Si:0.16、Mn:0.60、P:0.004、S:0.0017、Ni:9.2、Cu:0.06、 Mo:0.07、V:0.002、Cr:0.18、Als:0.008、N:0.00135, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.20%, steel plate thickness is 20mm.
Its preparation method is identical with the preparation method of embodiment 1.
Embodiment 6
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.05、Si:0.14、Mn:0.80、P:0.006、S:0.0009、Ni:9.4、Cu:0.02、 Mo:0.09、V:0.003、Cr:0.16、Als:0.025、N:0.00164, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.50%, steel plate thickness is 30mm.
Its preparation method is identical with the preparation method of embodiment 4.
Embodiment 7
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.02、Si:0.12、Mn:0.55、P:0.005、S:0.0013、Ni:9.0、Cu:0.05、 Mo:0.06、V:0.001、Cr:0.14、Als:0.009、N:0.00531, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.30%, steel plate thickness is 24mm.
Its preparation method is identical with the preparation method of embodiment 1.
Embodiment 8
A kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, including following mass percent Chemical composition (unit, wt%):C:0.04、Si:0.13、Mn:0.75、P:0.003、S:0.0018、Ni:8.6、Cu:0.03、 Mo:0.10、V:0.002、Cr:0.17、Als:0.007、N:0.00473, surplus is Fe and inevitable impurity.
Wherein, the carbon equivalent [Ceq=C+Mn/6+ (Cr+V+Mo)/5+ (Cu+Ni)/15] of the alloy-steel plate= 0.30%, steel plate thickness is 36mm.
Its preparation method is identical with the preparation method of embodiment 3.
Interpretation of result
Yield strength and tensile strength are carried out using the GB/T228 standard detection embodiment of the present invention 1-8 steel plates prepared It can detect, testing result is shown in Table 1.
Steel plate yield strength and tensile strength performance testing result prepared by the embodiment 1-8 of table 1
Project Steel plate thickness/mm Yield strength/MPa Tensile strength/MPa
Embodiment 1 12 650 720
Embodiment 2 40 710 740
Embodiment 3 50 710 740
Embodiment 4 30 700 710
Embodiment 5 20 660 720
Embodiment 6 30 680 730
Embodiment 7 24 710 720
Embodiment 8 36 715 730
As a result find, the 06Ni9DR steel plate yield strengths of the normalizing that thickness is 12mm+tempering state are 650Mpa, and tension is strong Spend for 720MPa, performance meets standard requirement, yield strength has larger surplus capacity.The 06Ni9DR steel of 20-50mm quenched and tempered state Plate yield strength is in 660-710MPa scope, and tensile strength is in 710-740MPa scope, and performance all meets all kinds of The requirement of standard, and yield strength has nearly l00Mpa surplus capacity.And the steel plate yield strength 710MPa of the preparation of embodiment 2, Tensile strength 740MPa, steel plate yield strength 710MPa, tensile strength 740MPa prepared by embodiment 3, performance is optimal.
Ultralow temperature pressure vessel prepared by embodiment 2, embodiment 3 is chosen with quenched high strength alloy steel 06Ni9DR steel plates Every test is carried out, test result is as follows.
Strand acidleach macroscopic examination:The steel plate low power result of the present invention shows C0.5 grades of the center segregation of casting blank, loose to be 0.5-1.0 grades, illustrating the steel plate of the present invention has good internal soundness.
Constituent analysis:Steel plate prepared by Example 2, embodiment 3, is analyzed its different parts chemical composition, is tied Fruit is as shown in table 2, steel plate constituent analysis wt%:
Table 2:Steel plate composition analysis result prepared by embodiment 2, embodiment 3
Gas content is analyzed:Gas content analysis is carried out to steel plate prepared by embodiment 2, embodiment 3, as a result such as table 3 It is shown, as a result show that gas content is relatively low in steel plate, steel plate gas content analysis (wt%).
Table 3:Steel plate gas content analysis result prepared by embodiment 2, embodiment 3
Project Specification N% O%
Embodiment 2 40mm 0.00189 0.00103
Embodiment 3 50mm 0.00195 0.00113
The remanent magnetism of steel plate:The remanent magnetism of the steel plate prepared using JCZ-30 remanent magnetometers to embodiment 2, embodiment 3 is tested, As a result it is as shown in table 4:
Table 4:Steel plate remanent magnetism assay prepared by embodiment 2, embodiment 3
Project Thickness mm The condition of delivery Residual induction Gs
Embodiment 2 40 It is quenched 6
Embodiment 3 50 It is quenched 6
Metallographic structure:The fine microstructures of steel plate are uniform, grain size about at 9-10 grade or so, the fiery steel plate of normalizing add-back Martensite+reversed austenite is organized as, quench the fiery steel plate of add-back is organized as martensite+reversed austenite.
The mechanical property of the steel plate condition of delivery:
Testing result shows, steel plate head, afterbody and intensity longitudinally, laterally and elongation percentage quite, 50mm steel plates Less, difference shows that each position of steel plate has more uniform mechanical property to the intensity difference of thickness 1/4 and 1/2 only within 20MPa Can, anisotropy is smaller.
Z-direction performance:The steel plate prepared to embodiment 2, embodiment 3, thickness direction drawing has been carried out using GB/T5313 standards Performance test is stretched, as a result as shown in table 5, either head or afterbody, thickness draw the contraction percentage of area of sample more than 70%, Highest standard requirement far above Z35, shows that steel plate has good anti-lamellar tearing performance.
Table 5:Steel plate stretching the performance test results prepared by embodiment 2, embodiment 3
Project Thickness/mm The condition of delivery Head Z/% Afterbody Z/%
Embodiment 2 40 It is quenched 78 79
Embodiment 3 50 It is quenched 75 76
Low-temperature impact toughness:The steel plate prepared according to the standards of GB/T 229 to embodiment 2, embodiment 3 has done diverse location - 196 DEG C of impact ductility tests, as a result as shown in table 6:
Table 6:- 196 DEG C of impact ductility test results of steel plate prepared by embodiment 2, embodiment 3
The 06Ni9DR steel plates of different size and the different conditions of delivery are can be seen that at -196 DEG C from above-mentioned result of the test Ballistic work is satisfied by the technical requirements to steel plate, and has a larger surplus, and average impact work(is (or close in more than 200J In 200J), side expansion is in 2mm or so.
Cold-bending property:For cold bending test, using horizontal sample, specimen width b=2a, curved core diameter d=2a.Steel plate table Flat processing.Carry out whole qualified, surface flawless after 180 DEG C of clod washes at room temperature.Illustrate that steel is pulled with good surface quality.
Hardness:The case hardness of each specification steel plate is examined according to GB/T231,7 are the results are shown in Table.All surface of steel plate are hard Degree is relatively stable between 229-240HB.
Table 7:Surface of steel plate hardness test result prepared by embodiment 2, embodiment 3
Project Thickness/mm The condition of delivery Hardness HB
Embodiment 2 40 It is quenched 235 234 232(234)
Embodiment 3 50 It is quenched 230 233 232(232)
Drop weight test determines steel plate nil-ductility temperature NDTT:Steel plate prepared by embodiment 2, embodiment 3 is carried out Drop weight test, sample takes horizontal sample.Experiment is by the built-up welding fragility welding bead on sample, under dynamic load drop impact, when fragility is split Line crack initiation is simultaneously broken corresponding temperature when traveling to an end of sample, and material resists brittle crack at a certain temperature The ability of propagation.Experimental evidence GS/T 6803-2008 are carried out, and drop weight test result is as shown in table 8:(f.Represent to break, x is represented Fracture).
Table 8:Steel plate drop weight test result prepared by embodiment 2, embodiment 3
Steel plate temper resistance can be tested:In order to grope mechanical property of the 06Ni9DR steel plates under different temperatures Situation of change and temper resistance, from the quenching state steel plate of different size thickness, are carried out with different heat treating regimes respectively Tempering, is processed into sample and carries out mechanical properties test.
Simulated post-weld heat treatment performance:By laboratory to the steel plate of delivery state steel plate sample mould manufacturer level in kind Quite, but cryogenic property is substantially dominant.
The steel plate developed carries out outer inspection, the percentage of A-class goods 100%;Detected a flaw by JB/T 47030, unification level rate is 80%, It is 100% to close three-level rate, has reached Expected Results.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, this area is common Other modifications or equivalent substitution that technical staff is made to technical scheme, without departing from technical solution of the present invention Spirit and scope, all should cover among scope of the presently claimed invention.

Claims (5)

1. a kind of ultralow temperature pressure vessel is with quenched high strength alloy steel 06Ni9DR steel plates, it is characterised in that:Including following quality The chemical composition (unit, wt%) of percentage:C:0.01-0.06、Si:0.10-0.20、Mn:0.50-0.80、P:≤0.008、S: ≤0.002、Ni:8.5-9.5, Cu≤0.10, Mo≤0.10, V≤0.005, Cr≤0.25, Als≤0.025, N≤0.012, it is remaining Measure as Fe and inevitable impurity;
The ultralow temperature pressure vessel preparation method of quenched high strength alloy steel 06Ni9DR steel plates, comprises the following steps:
(1)KR molten iron is pre-processed:Molten iron is contained with ladle, the molten iron that arrives at a station takes off P, S content in preceding slag, control molten iron, and molten iron is through KR Molten iron P≤0.1%, S≤0.004% after stirring desulphurization, desulfurization cycle≤25min, desulfurization temperature drop≤20 DEG C;De- S terminates to take off to the greatest extent Slag, liquid level thickness of slag layer≤20mm afterwards;
(2)Converter smelting:Carried out in 150 tons of converters, smelt dispensing according to steel scrap 4.5-4.8t, Ni plate 13-14t, molten iron 149-151t, total dispensing 165-170t are controlled, and S≤0.0030%, P≤0.080%, Si≤0.45%, C in the molten iron≤ 0.04%th, Mn≤0.7%, molten iron temperature >=1270 DEG C, molten iron charge weight is controlled by ± 1t;The steel scrap uses leftover pieces;Go out Slag is tapped before being kept off before steel with floating plug, and tapping is used in slag retaining cone pushing off the slag, thickness of slag layer≤20mm, converter tapping process before terminating Whole Argon;
(3)RH vacuum metlings are with skimming:Enter RH application of vacuum station vacuum metling, process cycle is 20-30min, when in molten steel Hydrogen content goes out station when being less than 2.0ppm, and ladle uses carbon-free covering agent, molten steel at the end of RH vacuum metlings in RH vacuum metlings Temperature is 1570-1580 DEG C, and the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(4)LF refining:Refining process whole process Argon, wherein Al beforehand controls are controlled at the end of 0.05-0.06%, refining 0.03-0.04%;S refines terminal point control in below 8ppm;1635-1645 DEG C of liquid steel temperature, soft blow time are controlled at the end of refining ≥2min;
(5)RH vacuum metlings:Enter RH application of vacuum station vacuum metling, process cycle is 18-22min, when hydrogen content in molten steel Go out station during less than 2.0ppm, ladle uses carbon-free covering agent in RH vacuum metlings, and liquid steel temperature is at the end of RH vacuum metlings 1570-1580 DEG C, the scum silica frost of molten steel surface is pulled out in RH vacuum metlings with Cinder Machine after terminating;
(6)Ladle wire feeding:Enter to feed silk station, add Al lines and Ca-Si lines;
(7)Continuous casting:Enter 15 ± 10 DEG C of the bag degree of superheat, pulling rate in continuous casting station, casting process:0.7-1.0m/min, Molten steel face not show is kept in continuous-casting steel pouring whole process blowing argon casting, middle bag casting process;Stopper is controlled to blow in steel pouring process Argon amount, liquid level fluctuation of crystallizer is slight;
(8)Cogging, cleaning, heating, rolling:Casting billet surface is polished and cleared up, and cogging is carried out clear to thickness 140mm to surface Reason, clears up temperature>250℃;Will be from cogging in continuous stove heat, total heat time >=3h, maximum heating temperature≤1200 DEG C; Hot 1150-1160 DEG C of temperature;Then the rolling of steel plate is carried out in 3800mm milling trains;
(9)Roll rear retarded cooling process:According to the difference of steel plate thickness, different section coolings is used after rolling, by adjusting cooling collection Pipe group number, control red temperature a:Thickness 12-35mm red temperature is between 650-750 DEG C, b:Returning for thickness 35-50mm is red Temperature is between 650-690 DEG C;
(10)Ultrasonic examination:Steel plate is detected using supersonic detector;
(11)Technology for Heating Processing:The qualified steel plate of detection, according to different steel plate thickness, is accordingly heat-treated, steel plate thickness ≤ 12mm, using double normalizing+tempering process;Steel plate thickness>12mm, using quenching+tempering technique twice.
2. a kind of ultralow temperature pressure vessel according to claim 1 quenched high strength alloy steel 06Ni9DR steel plates, its spy Levy and be:Chemical composition (unit, wt%) including following mass percent:C:0.02-0.04、Si:0.13-0.16、Mn: 0.65-0.75、P:≤0.006、S:≤0.002、Ni:8.6-9.4、Cu≤0.08、Mo≤0.60 、V≤0.003 、Cr≤ 0.18th, Als≤0.015, N≤0.009, surplus are Fe and inevitable impurity.
3. a kind of ultralow temperature pressure vessel according to claim 1 or 2 is with quenched high strength alloy steel 06Ni9DR steel plates, It is characterized in that:The thickness of the steel plate is 12mm-50mm.
4. a kind of ultralow temperature pressure vessel according to claim 1 quenched high strength alloy steel 06Ni9DR steel plates, its spy Levy and be, step(1)Described in ladle be using early stage bag of the bag age at 3-l5 times.
5. a kind of ultralow temperature pressure vessel according to claim 1 quenched high strength alloy steel 06Ni9DR steel plates, its spy Levy and be, step(11)The temperature of tempering process described in Technology for Heating Processing is controlled at 560-580 DEG C.
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