CN113088761B - Ultrahigh-strength corrosion-resistant alloy and manufacturing method thereof - Google Patents
Ultrahigh-strength corrosion-resistant alloy and manufacturing method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 60
- 239000000956 alloy Substances 0.000 title claims abstract description 60
- 230000007797 corrosion Effects 0.000 title claims abstract description 43
- 238000005260 corrosion Methods 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- 239000010936 titanium Substances 0.000 claims abstract description 22
- 239000010955 niobium Substances 0.000 claims abstract description 20
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- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 17
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
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- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 239000010703 silicon Substances 0.000 claims abstract 2
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- 239000011593 sulfur Substances 0.000 claims abstract 2
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- 238000010079 rubber tapping Methods 0.000 claims description 14
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- 235000011941 Tilia x europaea Nutrition 0.000 claims description 7
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 7
- 239000010436 fluorite Substances 0.000 claims description 7
- 239000004571 lime Substances 0.000 claims description 7
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 6
- 239000000378 calcium silicate Substances 0.000 claims description 6
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
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- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- HBELESVMOSDEOV-UHFFFAOYSA-N [Fe].[Mo] Chemical group [Fe].[Mo] HBELESVMOSDEOV-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 239000011572 manganese Substances 0.000 claims 1
- GFUGMBIZUXZOAF-UHFFFAOYSA-N niobium zirconium Chemical compound [Zr].[Nb] GFUGMBIZUXZOAF-UHFFFAOYSA-N 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000005553 drilling Methods 0.000 abstract description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract 1
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
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- 238000007872 degassing Methods 0.000 description 4
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 229910001026 inconel Inorganic materials 0.000 description 2
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- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 2
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- 229910052698 phosphorus Inorganic materials 0.000 description 2
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- 238000005086 pumping Methods 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
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- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/055—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 20% but less than 30%
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/18—Electroslag remelting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- Organic Chemistry (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of alloy manufacturing, particularly relates to an ultrahigh-strength corrosion-resistant alloy and a manufacturing method thereof, and particularly relates to a Cr-Ni-Mo-Nb corrosion-resistant alloy with ultrahigh strength and excellent stress corrosion resistance and a production technology thereof. The alloy of the invention comprises the elements nickel, carbon, silicon, manganese, sulfur, chromium, molybdenum, iron, aluminum, titanium, niobium, zirconium, yttrium. The alloy prepared by the invention is subjected to high pressure H 2 S, high pressure CO 2 And under the chloride ion environment, the composite material has very high strength and excellent stress corrosion resistance, can be used for manufacturing key parts of oil field drilling equipment, and has long service life.
Description
Technical Field
The invention belongs to the technical field of alloy manufacturing, and particularly relates to a Cr-Ni-Mo-Nb corrosion-resistant alloy with ultrahigh strength and excellent stress corrosion performance and a production technology of the alloy.
Background
The application of steel in the fields of sea oil engineering, marine ships, offshore engineering, sea water desalination, salt industry equipment, acid-resistant equipment, oil drilling and the like faces to the water-containing H 2 S, chloride ion, high pressure CO 2 Environmental influences such as oxygen-rich environment, residual stress in machining, external stress and the like, and a tendency or a result of stress corrosion cracking. Developed some mature varieties such as GH4169, Inconel 625 and the like at home and abroad.
There are still some problems, such as GH4169 due to high pressure H 2 S, high pressure CO 2 The corrosion environment containing chloride ions is not enough to bear stress corrosion in the environment, the service life is short, and the use cost is high. Such as hydraulic springs, hydraulic valves, fasteners, pipe fittings, etc., made of Inconel 625, at high pressure H 2 S, high pressure CO 2 And under the corrosive environment containing chloride ions, the corrosion resistance to stress corrosion is excellent, but the tensile strength is low, the service life is still short, and the use cost is high.
Aging strengthening means that after alloying elements are dissolved in metal in a solid solution, the alloying elements dissolved in the metal at a high temperature are precipitated in a certain form, such as intermetallic compounds, form dispersed hard particles, cause resistance to miscut, increase the strength and reduce the toughness.
SCC refers to stress corrosion cracking in the presence of water and H 2 In the presence of S, a metal crack associated with anodic processes and tensile stresses of localized corrosion.
Vacuum deoxidation technology
The vacuum deoxidation and degassing technology is a technology for reducing the oxygen level in molten steel by reducing the gas pressure of a reaction crucible through a vacuum pump under very low CO (g) partial pressure. The expression for the carbon-oxygen reaction is as follows:
[C]+[O]＝CO(g)
thermodynamic equilibrium equation: [% C]·[％O]＝1/KP CO
K-equilibrium constant;
P CO -pressure value of CO.
Basic principle of vacuum deoxidation: the higher the vacuum degree of the smelting space (i.e. P) under the action of vacuum CO The lower the value), the lower the oxygen content in the molten steel. The vacuum promotes the development of carbon-oxygen reaction and improves the deoxidation capability of carbon.
Vacuum dehydrogenation technique
Chemical reaction formula of vacuum dehydrogenation: [ H ]]＝1/2H 2 (g)，
Thermodynamic equilibrium equation: [ H ]]＝1/K(P H2 ) 1/2 。
Basic principle of vacuum dehydrogenation: the higher the vacuum degree of the smelting space (i.e. P) under the action of vacuum H2 The lower the value), [ H ]]The smaller the value, the lower the hydrogen content in the molten steel. The vacuum promotes the development of dehydrogenation reaction and reduces the hydrogen content of molten steel.
Vacuum denitrification technique
Chemical reaction formula of vacuum denitrification, [ N ]]＝1/2N 2 (g)，
Thermodynamic equilibrium equation: [ N ]]＝1/K(P N2 ) 1/2
Basic principle of vacuum denitrification: the higher the vacuum degree of the smelting space (i.e. P) under the action of vacuum N2 Lower value), [ N ]]The smaller the value, the lower the nitrogen content in the molten steel. The vacuum promotes the development of denitrification reaction and reduces the nitrogen content of the molten steel.
Vacuum deoxidation, dehydrogenation and denitrification are essentially single methods of diffusion deoxidation, diffusion dehydrogenation and diffusion denitrification, have good effects on reducing the oxygen content, the hydrogen content and the nitrogen content of molten steel in steel smelting, and still cannot meet the requirements of high-end corrosion-resistant alloy on the oxygen content, the hydrogen content and the nitrogen content of the molten steel. Generally, under the vacuum degree of 66.7Pa (0.5mmHg), the deoxidation limit degree can only reach 35-45ppm, the dehydrogenation limit degree can only reach 5-6ppm, and the denitrification limit degree can only reach 25-35 ppm.
Vacuum smelting desulfurization technology
The traditional vacuum smelting desulfurization technology is to remove [ S ] in molten steel by applying deoxidizers Si-Fe, Si-Ca, Al powder (block) and C powder through the following chemical reactions.
[S]+[C]+(CaO)＝(CaS)+{CO}。
Disclosure of Invention
Aiming at the defects of the prior art, the corrosion resistant alloy is effectively improved at high pressure H 2 S, high pressure CO 2 And corrosion resistance in a chloride ion environment, particularly stress corrosion cracking resistance, and the invention provides an ultrahigh-strength corrosion-resistant alloy and a manufacturing method thereof.
In order to achieve the purpose, the invention aims to provide the ultrahigh-strength corrosion-resistant alloy with the service life obviously prolonged in the use environment from important links such as component design, smelting, heat treatment and the like, so that the problem of material pain points with short service life caused by insufficient stress corrosion resistance or insufficient strength index of GH4169 and Inconel 625 is fundamentally solved.
1. Optimized design of chemical compositions
The alloy provided by the invention is represented as HQ9725 alloy, and the components of the alloy are shown in Table 1.
TABLE 1 composition of HQ9725 alloy (percent)
The alloy elements of chromium, molybdenum, tungsten, niobium and cobalt form single-phase solid solution, so that the stacking fault energy is reduced, the extended dislocation is easy to form, the binding force of solute atoms is strong, the diffusion activation energy is increased, and the strength and the corrosion resistance are obviously improved. The melting points of the elements are high, namely the melting point of chromium is 1857 ℃, the melting point of molybdenum is 2620 ℃, the melting point of tungsten is 3410 ℃, the melting point of niobium is 2467 ℃ and the melting point of zirconium is 1852 ℃, and particularly the corrosion resistance of the alloy under the high-temperature condition can be improved.
The addition of Al, Ti, Mo and Zr enriches the precipitation of dispersed phases (second phase precipitation), and the precipitated phases can strongly obstruct the slippage of dislocation, thereby being another effective method for improving the strength.
Rare earth elements such as Zr and Y are added to the alloy, which significantly improves the activation energy of grain boundary diffusion, hinders grain boundary sliding, and increases the surface energy of grain boundary cracks, and thus is very effective in improving strength.
Ni is the main forming element of the aging strengthening phase, nickel and iron can be infinitely dissolved in solid solution, and nickel expands the austenite area of iron and is the main alloying element for forming and stabilizing austenite. Ni and C do not form carbide, improve corrosion resistance and plasticity, and Ni, Al and Ti form a second phase Ni 3 AlTi is separated out, and the strength is greatly improved.
Al and Ti can obviously refine the crystal grains of the steel according to the Hall-Peltier formula sigma s-sigma 0+ kd (-1/2) Where σ s is tensile strength and d is grain diameter, the finer the grain, the higher the strength. TiFe 2 The precipitation of (2) improves the strength of the steel. Al and Ti can also obviously improve the oxidation resistance of the steel. Al and Ti have strong affinity with oxygen and are ideal steel-making deoxidizers, so that the purity and the corrosion resistance of steel are obviously improved.
Mo has a remarkably solid-solution strengthening effect as an alloying element in steel because of its atomic electronic characteristics very similar to those of Fe. At aging temperature, Mo combines with Cr, Fe, V and other elements and carbide to form (Cr, Fe, V, Mo) 23 C 6 Composite carbide, Mo and Ni combined to form second phase Ni 3 Mo, Mo combines with Fe, Ni, Co, etc. to form a second phase (Fe, Ni, Co) 2 Mo, all play an obvious role in aging strengthening.
Nb can obviously inhibit the growth of crystal grains, so the crystal grain refining effect is obvious, the tensile strength is greatly improved, Nb is very easy to combine with C and N to form Nb (CN) in the molten steel solidification process, on one hand, the corrosion resistance, especially the intergranular corrosion resistance, is improved, on the other hand, the second phase Nb (CN) is very fine in size, plays a role in pinning dislocation movement, and obviously improves the tensile strength of the steel.
2. Production process route
The production process route of the HQ9725 alloy provided by the invention is as follows.
Raw material preparation → vacuum induction → pouring electrode → electrode finishing → electroslag remelting → electroslag ingot finishing → heating → forging → ultrasonic flaw detection → heat treatment → sampling → peeling → inspection → packaging → warehousing.
2.1 preparation of the starting Material
The raw materials comprise: pure iron, Jinchuan nickel, low-carbon ferrochrome, metal chromium, molybdenum bars, niobium bars, pure titanium, pure aluminum, calcium silicate powder, aluminum powder, lime, fluorite, zirconium alloy, metal yttrium and Ni-Mg.
The raw material requirements are as follows: the raw material is selected from low-phosphorus low-carbon grade, and has no oil stain and water. The deoxidizer (calcium silicate powder, aluminum powder, lime, fluorite, Ni-Mg, metal yttrium) is baked and dried in a baking oven at the temperature of 450-550 ℃.
2.2 vacuum smelting
The process mainly comprises the working procedures of charging, melting, refining, pouring and the like.
(1) Charging:
the charging principle is as follows: the upper part is loose and the lower part is tight, so that the bridging is prevented.
Before loading large materials, a layer of fine light materials is paved at the bottom of the furnace.
The furnace charge with high melting point and difficult oxidation, such as molybdenum strip, niobium strip, aurora nickel and micro-carbon ferrochrome, should be arranged in the middle and lower high temperature regions of the crucible.
Easily oxidized furnace materials such as Ti and Al iron are added 2-5 minutes before tapping under the condition of good deoxidation of molten metal. The zirconium alloy and the yttrium metal are added during tapping 1/3.
(2) Melting period:
after the charging, the vacuum-pumping should be started. When the vacuum chamber pressure reaches 0.03mbar, electricity is transmitted for heating.
During the initial stage of melting, a higher vacuum degree and a slower melting speed are maintained.
The melting time is greater than 120 minutes. And sampling and fully analyzing after melting down.
(3) And (3) refining period:
the main tasks of the refining phase are: deoxidizing, degassing, removing volatile impurities, adjusting temperature and adjusting components.
The refining temperature is 1530 and 1560 ℃, the vacuum degree is further increased to 0.013mbar, and the refining time is more than 35 minutes.
The slagging frequency in the refining period is 5-7 times. Sampling and analyzing completely.
Adjusting the alloy components to meet the process requirements, adding easily-oxidizable alloys such as Si, Mn, Al and Ti, and stirring for 5-7min at high power.
Adding Ni-Mg 2-3min before tapping to further deoxidize and desulfurize, wherein the adding amount of Ni-Mg is controlled to be 0.02-0.04% of the molten steel amount. The adding amount of the zirconium alloy is controlled to be 0.01-0.08 percent of the molten steel, the adding amount of the metal yttrium is controlled to be 0.01-0.08 percent of the molten steel, and the zirconium alloy and the metal yttrium are added when the tapping amount is 1/3.
(4) Pouring:
stirring for 2-4 minutes with high power before tapping.
The tapping temperature is controlled at 1550-.
And casting an ingot mold phi 220.
2.3 electroslag remelting
Electrode size: phi 220
Finishing electrodes: and (4) cutting shrinkage cavities at the head of the induction electrode, and completely grinding the defects of cold steel, cracks, slag inclusion, impurities and the like on the surface of the electrode.
Electroslag system: adopting quaternary slag with low melting point and good fluidity
CaF 2 :Al 2 O 3 :MgO:CaO＝70:20:5:5。
Voltage and current system: the voltage is 60-65V, and the current is 8000- & 8500A.
Electroslag ingot finishing: and cutting off shrinkage cavities at the head of the electroslag ingot, and cleaning the defects of oxidized heavy skin, slag inclusion, inclusion and the like on the surface of the electroslag ingot.
2.4 forging
The forging equipment adopts a hydraulic air hammer or a quick forging hydraulic machine.
The forging ratio requirement is as follows: 8-10.
As shown in fig. 1, soaking temperature: 1050-: the forging temperature is not less than 1030 and not less than 1150 ℃ and the finish forging temperature is not less than 900 ℃ for 4-6 hours, and the upsetting frequency is not less than 2-3 times for ensuring the forging ratio.
2.5 ultrasonic inspection
Flaw detection is carried out by adopting GB/T4162-2008 'forged and rolled steel bar ultrasonic detection method', the diameter of a flat bottom hole is 2.0, and the grade of acceptance grade is grade A.
2.6 Heat treatment
The heat treatment is divided into two steps, namely the first step of solution treatment and the second step of aging treatment.
In the first step, solution treatment is performed at 1060-1200 deg.C, preferably 1180 deg.C, and soaking time of 1-2 min/mm (outer diameter, thickness, wall thickness, etc.) as shown in FIG. 2.
And rapidly cooling with water after heat treatment. It is required to cool to below 100 ℃ within 15 minutes.
And secondly, aging treatment, as shown in figure 3, wherein the soaking temperature is 650-. Wherein D is wall thickness (pipe fitting)/outer diameter (round steel)/thickness (square steel or plate) in mm.
After the HQ9725 is subjected to solution heat treatment, Cr, Ni and Mo are fully dissolved in an austenite matrix, so that the lattice distortion is greatly improved, the interatomic binding force is greatly enhanced, the diffusion activation energy is greatly increased, the stacking fault energy is greatly reduced, and the solid solution strength of the alloy is finally improved.
HQ9725 is subjected to aging heat treatment, and then a large amount of dispersed fine second phase Ni is precipitated 3 Nb、Ni 3 Ti、Ni 3 AlTi、TiFe 2 、(Fe,Ni)Mo 2 Nb (cn), etc., significantly improving the material strength.
The innovation points of the invention comprise: (1) designing the Ti/Al ratio range to be 4.0-6.0, and optimally 5.0; (2) the innovation is bold, Zr is added for the first time, the control range is 0.01-0.08%, Y is added for the first time, and the control range is 0.01-0.08%.
The beneficial effects of the invention include: the invention first of allSystematic study of alloy elements such as Cr, Ni, Mo, Ti, Al, Nb, Zr and Y under high pressure H 2 S, high pressure CO 2 And the effect of improving the mechanical property and the corrosion resistance under the chloride ion environment. The strengthening effect of the second phase precipitation and the effect of grain refinement are fully developed. Vacuum induction and vacuum electroslag advanced equipment are adopted, vacuum degassing is fully utilized to improve the purity of molten steel, and further Ni-Mg and rare earth (Zr and Y) are adopted for refining, so that the deoxidation, desulfurization and degassing effects of the Ni-Mg and the rare earth (Zr and Y) are fully exerted. To make it [ O ]]The content is greatly reduced from 35-45ppm of the original traditional vacuum refining to 6-8ppm, and the [ S ] is obtained]The content is greatly reduced from 5-6ppm of the original traditional vacuum refining to 1-2ppm, and the [ N ] is obtained]The content is greatly reduced to a level less than 10ppm from 25-35ppm of the original traditional vacuum refining, and simultaneously, the content of the non-metallic inclusions is greatly reduced, thereby greatly reducing the alloy crystal boundary defects, enhancing the alloy intercrystalline strength and resisting the crack propagation. Finally, through reasonable solid solution and aging heat treatment, a large amount of dispersed fine second phase Ni is precipitated 3 Nb、Ni 3 Ti、Ni 3 AlTi、TiFe 2 、(Fe,Ni)Mo 2 And the strength of the steel material is greatly improved. So that the alloy is under high pressure H 2 S, high pressure CO 2 And under the chloride ion environment, the composite material not only has very high strength, but also has excellent stress corrosion resistance, can be used for manufacturing key parts of oil field drilling and production equipment, and has one to two times of service life.
Drawings
FIG. 1 is a drawing of the forging heating process for the HQ9725 alloy of the present invention.
FIG. 2 is a heat treatment process diagram of the HQ9725 alloy of the present invention.
FIG. 3 is a diagram of the aging process of the HQ9725 alloy of the present invention.
Detailed Description
The HQ9725 alloy developed by the invention comprises the optimized design of chemical components and the optimized design of a production process route.
Chemical composition design of HQ9725 alloy
Compared with the traditional GH4169 and Inconel 625 alloys, the HQ9725 alloy produced by the method has the advantages that the components are optimized, the Ti/Al ratio is designed to be 4.0-6.0, the best Ti/Al ratio is 5.0, and the strength of the alloy is further improved; the innovative design of the method is boldly that Zr is added, the control range is 0.01-0.08%, the best is 0.02%, Y is added, the control range is 0.01-0.08%, the best is 0.02%, and the detail is shown in Table 2.
Table 2 ingredient design comparison (percent,%)
The specific manufacturing process is described below by taking the preferred scheme of the HQ9725 alloy as an example, and the comprehensive performance is compared with the conventional GH4169 and Inconel 625 alloys on the basis of the specific manufacturing process.
The production process route of the HQ9725 alloy is as follows.
Raw material preparation → vacuum induction → pouring electrode → electrode finishing → electroslag remelting → electroslag ingot finishing → heating → forging → ultrasonic flaw detection → heat treatment → sampling → peeling → inspection → packaging → warehousing.
2.1 preparation of the starting Material
The raw materials comprise: pure iron, aurora nickel, low-carbon ferrochrome, metal chromium, molybdenum strips, niobium strips, pure titanium, pure aluminum, calcium silicate powder, aluminum powder, lime, fluorite, zirconium alloy, metal yttrium and Ni-Mg.
The raw material requirements are as follows: the raw material is selected from low-phosphorus low-carbon grade, and has no oil stain and water. The deoxidizer (calcium silicate powder, aluminum powder, lime, fluorite, Ni-Mg, metal yttrium) is baked and dried in a baking oven at the temperature of 450-550 ℃.
2.2 vacuum smelting
The process mainly comprises the working procedures of charging, melting, refining, pouring and the like.
(1) Charging:
the charging principle is as follows: the upper part is loose and the lower part is tight, so that the bridging is prevented.
Before loading large materials, a layer of fine light materials is paved at the bottom of the furnace.
The furnace charge with high melting point and difficult oxidation, such as molybdenum strip, niobium strip, aurora nickel and micro-carbon ferrochrome, should be arranged in the middle and lower high temperature regions of the crucible.
Easily oxidized furnace materials such as Ti and Al iron are added 3 minutes before tapping under the condition of good deoxidation of molten metal. The zirconium alloy and the yttrium metal are added during tapping 1/3.
(2) Melting period:
after the charging, the vacuum-pumping should be started. When the vacuum chamber pressure reaches 0.03mbar, electricity is transmitted for heating.
During the initial stage of melting, a higher vacuum degree and a slower melting speed are maintained.
The melting time is greater than 120 minutes. And sampling and fully analyzing after melting down.
(3) And (3) refining period:
the main tasks of the refining phase are: deoxidizing, degassing, removing volatile impurities, adjusting temperature and adjusting components.
The refining temperature is 1550 ℃, the vacuum degree is further increased to 0.013mbar, and the refining time is more than 35 minutes.
The slagging times in the refining period are 6 times. Sampling and analyzing completely.
Adjusting the alloy components to meet the process requirements, adding easily-oxidizable alloys such as Si, Mn, Al and Ti, and stirring for 6min at high power.
Adding Ni-Mg 3min before tapping to further deoxidize and desulfurize, wherein the adding amount of Ni-Mg is controlled at 0.02% of molten steel. The adding amount of the zirconium alloy is controlled to be 0.02 percent of the molten steel, the adding amount of the metal yttrium is controlled to be 0.02 percent of the molten steel, and the zirconium alloy and the metal yttrium are added when the steel tapping amount is 1/3 percent.
(4) Pouring:
stirring for 2-4 minutes with high power before tapping.
The tapping temperature is controlled at 1560 ℃.
And casting an ingot mold phi 220.
2.3 electroslag remelting
Electrode size: phi 220
Finishing electrodes: and cutting the shrinkage cavity at the head of the induction electrode, and grinding the defects of cold steel, cracks, slag inclusion and the like on the surface of the electrode.
Electroslag system: adopting quaternary slag with low melting point and good fluidity
CaF 2 :Al 2 O 3 :MgO:CaO＝70:20:5:5。
Voltage and current system: the voltage is 60-65V, and the current is 8000- & 8500A.
Electroslag ingot finishing: and cutting off the shrinkage cavity at the head of the electroslag ingot, and cleaning the defects of oxidized heavy skin, slag inclusion, inclusion and the like on the surface of the electroslag ingot.
2.4 forging
The forging equipment adopts a hydraulic air hammer or a quick forging hydraulic machine.
The forging ratio requirement is as follows: 8-10.
Soaking temperature: 1120 ℃, the heating speed is less than or equal to 120 ℃/h, and the soaking time is as follows: and 5 hours, the forging opening temperature is not less than 1030 and not less than 1150 ℃, the finish forging temperature is not less than 900 ℃, and the upsetting frequency is not less than 2-3 times for ensuring the forging ratio.
2.5 ultrasonic inspection
Flaw detection is carried out by adopting GB/T4162-2008 'forged and rolled steel bar ultrasonic detection method', the diameter of a flat bottom hole is 2.0, and the grade of acceptance grade is grade A.
2.6 Heat treatment
The heat treatment comprises two steps, namely the first step of solution treatment and the second step of aging treatment.
Firstly, carrying out solution treatment at 1180 ℃ for 1-2 min/mm (outer diameter, thickness, wall thickness and the like of a workpiece).
And rapidly cooling with water after heat treatment. It is required to cool to below 100 ℃ within 15 minutes.
And secondly, aging treatment is carried out, wherein the soaking temperature is 732 ℃, and the heat preservation time T is D/50+5, and the unit is hour. Wherein D is wall thickness (pipe fitting)/outer diameter (round steel)/thickness (square steel or plate) in mm.
Compared with the traditional GH4169 and Inconel 625 alloys, the HQ9725 alloy produced by the invention is purer and has lower content of non-metallic inclusions, and the details are shown in Table 3.
TABLE 3 comparison of the contents of inclusions
Compared with the traditional Inconel 625 alloy, the strength of the HQ9725 alloy produced by the method is improved by 150% after aging, and compared with the traditional GH4169 alloy, the strength of the HQ9725 alloy after aging is improved by 25%, and the details are shown in Table 4.
TABLE 4 comparison of age Strength indices
Compared with the traditional GH4169 and Inconel 625 alloys, the HQ9725 alloy produced by the invention has the advantages of 2 percent of NaCl and H 2 S pressure 13.8Bar (1.38MPa), CO 2 The pressure is 13.8Bar (1.38MPa), and the cracking is avoided within 30 days under the temperature of 177 ℃. Under the same test conditions, GH 416910 and Inconel 15 do not crack. The stress corrosion resistance of HQ9725 is respectively improved by 200% compared with GH4169 and 100% compared with Inconel. See table 5 for details.
TABLE 5 comparison of stress corrosion resistance indexes
| Number plate | Results | Comparison of resistance to stress corrosion |
| HQ9725 | No cracking after 30 days | -- |
| GH4169 | No crack after 10 days | HQ9725 is 200% higher than GH4169 |
| Inconel 625 | No crack after 15 days | HQ9725 is 100 percent higher than Inconel 625 |
Optimization of HQ9725 ingredient design
For the chemical composition, 9 sets of solutions as shown in table 6 were designed, and the preferred solution was derived from the dimensions of stress corrosion resistance.
TABLE 6 optimization of chemical composition design of HQ9725
For the amounts of added Zr and Y, 9 sets of recipes as shown in table 7 were designed, and the preferable recipe was derived from the dimension of stress corrosion resistance.
TABLE 7 optimization of HQ9725 Zr and Y addition
For the ageing temperature, 6 sets of solutions as shown in table 8 were designed, and the preferred solution was derived from the ageing strength dimension.
TABLE 8 optimization scheme of HQ9725 ageing temperature
| Name of the scheme | Aging temperature of | Rm，MPa | Rp0.2，MPa | Remarks for note |
| Scheme 1 | 650 | 1.5 | 520 | |
| Scheme 2 | 700 | 1.5 | 520 | |
| Scheme 3 | 730 | 1750 | 1710 | Preference is given to |
| Scheme 4 | 760 | 1680 | 1620 | |
| Scheme 5 | 790 | 1590 | 1520 | |
| Scheme 6 | 820 | 1440 | 1390 |
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.
Claims (7)
1. An ultrahigh-strength corrosion-resistant alloy is characterized in that: the weight percentage of the components is as follows:
56 to 60 percent of nickel
0 to 0.03 percent of carbon
0 to 0.2 percent of silicon
0.3 to 0.5 percent of manganese
0 to 0.01 percent of sulfur
17.0 to 22.0 percent of chromium
8 to 10 percent of molybdenum
Iron residue
0.2 to 0.4 percent of aluminum
1.2 to 2.0 percent of titanium
2.8 to 3.5 percent of niobium
Zirconium 0.01-0.08%
Yttrium 0.01-0.08%
The mass percentage of the titanium to the aluminum is 4.0 to 6.0;
the manufacturing method of the ultrahigh-strength corrosion-resistant alloy comprises the following steps:
(2.1) preparation of raw Material
The raw materials comprise: pure iron, aurora nickel, low-carbon ferrochrome, metal chromium, molybdenum strips, niobium strips, pure titanium, pure aluminum, calcium silicate powder, aluminum powder, lime, fluorite, zirconium alloy, metal yttrium and Ni-Mg;
(2.2) vacuum melting
1) Charging
2) Melting of
Vacuumizing after the charging is finished, and when the pressure of a vacuum chamber reaches 0.03mbar, transmitting electricity for heating;
3) refining
The refining temperature is 1530 and 1560 ℃, the vacuum degree is further increased to 0.013mbar, and the refining time is more than 35 minutes; in the refining process, adjusting alloy components to meet the process requirements;
4) pouring
(2.3) electroslag remelting
(2.4) forging
The forging ratio requirement is as follows: 8-10;
soaking temperature: 1050-: 4-6 hours, open forging temperature: 1030 ℃ and 1150 ℃, the finish forging temperature is not less than 900 ℃, and the upsetting times are not less than 2;
(2.5) flaw detection
(2.6) Heat treatment
The heat treatment is divided into two steps, namely, the first step of solution treatment and the second step of aging treatment;
solution treatment, wherein the soaking temperature is 1060-1200 ℃, and the soaking time is 1-2 min/mm; rapidly cooling to below 100 ℃ within 15 minutes; and (3) aging treatment, wherein the soaking temperature is 650-780 ℃, the heat preservation time T = D/50+5, the unit is hour, and the unit is wall thickness and mm.
2. The ultra-high strength, corrosion resistant alloy of claim 1, wherein: the mass percentage of zirconium is preferably 0.02%, and the mass percentage of yttrium is preferably 0.02%.
3. The method of manufacturing an ultra-high strength, corrosion resistant alloy according to claim 1 or 2, wherein: the method comprises the following steps:
(2.1) preparation of raw Material
The raw materials comprise: pure iron, aurora nickel, low-carbon ferrochrome, metal chromium, molybdenum strips, niobium strips, pure titanium, pure aluminum, calcium silicate powder, aluminum powder, lime, fluorite, zirconium alloy, metal yttrium and Ni-Mg;
(2.2) vacuum melting
1) Charging
2) Melting
Vacuumizing after the charging is finished, and when the pressure of a vacuum chamber reaches 0.03mbar, transmitting electricity for heating;
3) refining
The refining temperature is 1530 and 1560 ℃, the vacuum degree is further increased to 0.013mbar, and the refining time is more than 35 minutes; in the refining process, adjusting alloy components to meet the process requirements;
4) pouring
(2.3) electroslag remelting
(2.4) forging
The forging ratio requirement is as follows: 8-10;
soaking temperature: 1050-: 4-6 hours, open forging temperature: 1030 ℃ and 1150 ℃, the finish forging temperature is not less than 900 ℃, and the upsetting times are not less than 2;
(2.5) flaw detection
(2.6) Heat treatment
The heat treatment is divided into two steps, namely, the first step of solution treatment and the second step of aging treatment;
solution treatment, wherein the soaking temperature is 1060-1200 ℃, and the soaking time is 1-2 min/mm; rapidly cooling to below 100 ℃ within 15 minutes; and (3) aging treatment, wherein the soaking temperature is 650-780 ℃, the heat preservation time T = D/50+5, the unit is hour, and the unit is wall thickness and mm.
4. The method of manufacturing an ultra-high strength corrosion resistant alloy of claim 3, wherein: adding Ni-Mg 2-3min before tapping, wherein the adding amount of the Ni-Mg is controlled to be 0.02-0.04% of that of the molten steel; the zirconium alloy and the metal yttrium are added when the steel tapping amount is 1/3, the adding amount of the zirconium alloy is controlled to be 0.01-0.08 percent of the molten steel, and the adding amount of the metal yttrium is controlled to be 0.01-0.08 percent of the molten steel.
5. The method of manufacturing an ultra-high strength corrosion resistant alloy of claim 3, wherein: the electroslag remelting step comprises the following steps:
electrode size: phi 220;
finishing electrodes: cutting off shrinkage holes at the head of the induction electrode, and grinding the surface of the electrode to remove cold steel, cracks, slag and inclusion defects;
electroslag system: using four-element slag CaF 2 :Al 2 O 3 :MgO:CaO=70:20:5:5；
Voltage and current system: the voltage is 60-65V, and the current is 8000- & gt 8500A;
electroslag ingot finishing: and cutting off the shrinkage cavity at the head of the electroslag ingot, and cleaning the defects of oxidized heavy skin, slag inclusion and inclusion on the surface of the electroslag ingot.
6. The method of manufacturing an ultra-high strength corrosion resistant alloy of claim 3, wherein: the charging principle is as follows: the upper part is loose and the lower part is tight, so that the bridging is prevented; before loading large materials, a layer of fine light materials is paved at the bottom of the furnace; the molybdenum strips, the niobium strips, the Jinchuan nickel and the low-carbon ferrochromium are arranged in the middle and lower high-temperature regions of the crucible.
7. The method of manufacturing an ultra-high strength corrosion resistant alloy of claim 3, wherein: in the raw materials, the silico-calcium powder, the aluminum powder, the lime, the fluorite, the Ni-Mg and the metal yttrium are baked and dried in a baking oven at the temperature of 550 ℃ of 450-.
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