CN116904803A - Triple smelting method for deformed superalloy GH4169 large-size cast ingot - Google Patents
Triple smelting method for deformed superalloy GH4169 large-size cast ingot Download PDFInfo
- Publication number
- CN116904803A CN116904803A CN202310921855.7A CN202310921855A CN116904803A CN 116904803 A CN116904803 A CN 116904803A CN 202310921855 A CN202310921855 A CN 202310921855A CN 116904803 A CN116904803 A CN 116904803A
- Authority
- CN
- China
- Prior art keywords
- stage
- smelting
- slag
- ingot
- vacuum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000003723 Smelting Methods 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 45
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 38
- 230000008018 melting Effects 0.000 claims abstract description 38
- 230000006698 induction Effects 0.000 claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 27
- 239000000956 alloy Substances 0.000 claims abstract description 27
- 230000001681 protective effect Effects 0.000 claims abstract description 17
- 239000010955 niobium Substances 0.000 claims abstract description 12
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 10
- 239000002893 slag Substances 0.000 claims description 41
- 239000002994 raw material Substances 0.000 claims description 23
- 238000007670 refining Methods 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 21
- 229910000831 Steel Inorganic materials 0.000 claims description 17
- 239000010959 steel Substances 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000005266 casting Methods 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 claims description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 9
- 239000010936 titanium Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000009849 vacuum degassing Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 10
- 238000005242 forging Methods 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000005204 segregation Methods 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 8
- 238000005070 sampling Methods 0.000 description 5
- 239000011573 trace mineral Substances 0.000 description 5
- 235000013619 trace mineral Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 101000912561 Bos taurus Fibrinogen gamma-B chain Proteins 0.000 description 1
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a triple smelting method for a deformed superalloy GH4169 large-specification ingot, which adopts a novel triple smelting process of Vacuum Induction Melting (VIM) +protective atmosphere electroslag melting (ESR) +vacuum consumable melting (VAR) to produce the superalloy GH4169 large-specification ingot. The smelting method provided by the invention can ensure that a large ingot-shaped forging can be obtained, can greatly reduce the S content in a finished ingot, and reduces the risk of generating segregation metallurgical defects of high-niobium wrought superalloy, so that a GH4169 alloy large-size ingot with better component uniformity and lower content of impurity elements O, S, N and the like is obtained.
Description
Technical Field
The invention relates to a sample processing method, in particular to a triple smelting method of a large-specification deformed superalloy cast ingot.
Background
GH4169 is a nickel-based superalloy precipitation strengthened with the body-centered tetragonal gamma 'and face-centered cubic gamma' phases. The alloy has good comprehensive performance in the temperature range of minus 253-650 ℃, the yield strength below 650 ℃ is the first place of the deformation superalloy, and has good anti-fatigue, anti-radiation, anti-oxidation and corrosion resistance, good processability and good welding performance. Can be used for manufacturing various parts with complex shapes, and has wide application in aerospace, nuclear energy, petroleum industry and extrusion dies in the temperature range.
In order to obtain a large forging with more uniform performance, higher requirements are put on the component uniformity and inclusion content of GH4169 forging produced by a metallurgical plant, at present, a general-purpose GH4169 alloy is smelted by adopting a VIM+PESR (protective atmosphere electroslag remelting) or VIM+VAR process, however, the VIM+PESR method has good S removal effect, but because slag skin blocks heat radiation, a molten pool is deeper, and when the ingot shape is larger than phi 430mm, macrosegregation is easy to occur in the core part; the ingot is smelted by adopting a VIM+VAR process, but the number of inclusions and shrinkage cavities in an electrode cast by vacuum induction smelting is large, the density of the electrode is poor, the stability is poor during vacuum consumable remelting, the risk of metallurgical defects generated by a finished ingot is high, the ingot produced by the process is not subjected to an S removing process, the content of S element in the finished ingot is high, the effect of removing O and inclusions is not as good as the former, and the high-temperature performance of the alloy is seriously affected.
Therefore, the research on a triple smelting method capable of large-size deformation high-temperature alloy ingots is needed in the field, the S content in finished ingots can be greatly reduced while large ingot forgings are ensured to be obtained, meanwhile, the risk that high-niobium deformation high-temperature alloy generates segregation metallurgical defects is reduced, and GH4169 alloy large-size ingots with better component uniformity and lower impurity element O, N, S content can be obtained by adopting the method.
Disclosure of Invention
In order to solve the technical problems, the invention provides a large-specification deformed superalloy cast ingot, wherein the deformed superalloy is GH4169 superalloy, and the large-specification deformed superalloy cast ingot comprises the following chemical components in percentage by mass: 0.015-0.06% of C, 17.0-21.0% of Cr, 50.0-55.0% of Ni, 0.75-1.15% of Ti, 0.30-0.70% of Al, 2.80-3.30% of Mo, 4.75-5.50% of Nb, less than or equal to 0.0020% of S, less than or equal to 0.0060% of B, less than or equal to 0.30% of Cu, less than or equal to 0.0050% of Mg, less than or equal to 0.0050% of O, less than or equal to 0.010% of N and the balance of Fe.
The invention also provides a triple smelting method of the large-specification deformed superalloy ingot, which is used for preparing the large-specification deformed superalloy ingot, and adopts a novel triple smelting process of vacuum induction smelting (VIM) +protective atmosphere Electroslag Smelting (ESR) +vacuum consumable smelting (VAR) to produce a superalloy GH4169 large-specification ingot, and comprises the following steps:
s1, vacuum induction melting: the raw materials for vacuum induction smelting and the weight thereof are as follows: 3100-3348kg of nickel plate, 1054-1116kg of vacuum degassing chromium, 46-65kg of titanium ingot, 19-37kg of aluminum ingot, 173-183kg of molybdenum strip, 295-340kg of niobium strip, 1.30-1.50kg of ferroboron intermediate alloy, 14-17kg of nickel magnesium intermediate alloy, 1100-1500kg of ultra-pure iron and 0.5-1.0kg of graphite carbon;
the mass fraction of B element of the ferroboron intermediate alloy is not less than 18.5%, preferably 18.5%, and the mass fraction of Mg element of the nickel-magnesium intermediate alloy is not less than 17%, preferably 17%;
s2, protective atmosphere electroslag smelting: the protective atmosphere electroslag smelting comprises a slag melting stage, a first steady-state stage and a first heat-seal top stage;
s3, vacuum consumable smelting: the vacuum consumable smelting comprises an arcing stage, a second steady-state stage and a second heat-seal top stage, wherein the pre-vacuum of the vacuum consumable smelting is less than 0.1Pa, and the leak rate is less than 0.13Pa/min.
Preferably, the weight of nickel plate in the raw material for vacuum induction melting is preferably 3100kg, 3150kg, 3200kg, 3250kg, 3300kg, 3348kg.
Preferably, the weight of vacuum deaerated chromium in the raw material for vacuum induction smelting is preferably 1054kg, 1064kg, 1074kg, 1084kg, 1094kg, 1104, 1116kg.
Preferably, the weight of the titanium ingot in the raw material for vacuum induction melting is 46kg, 50kg, 55kg, 60kg, 65kg.
Preferably, the weight of the aluminum ingot in the raw material for vacuum induction melting is preferably 19kg, 25kg, 30kg, 35kg, or 37kg.
Preferably, the weight of the molybdenum strip in the raw material for vacuum induction melting is 173kg, 175kg, 177kg, 179kg, 181kg, 183kg.
Preferably, in the raw material for vacuum induction melting, the weight of the niobium rod is 295kg, 300kg, 305kg, 60kg, 65kg.
Preferably, the weight of the ultra-pure iron in the raw material for vacuum induction smelting is preferably 1100kg, 1105kg, 1200kg, 1300kg, 1400kg and 1500kg.
Preferably, the weight of the graphite carbon in the raw material for vacuum induction melting is preferably 0.5kg, 0.6kg, 0.7kg, 0.8kg, 0.9kg, 1.0kg.
Preferably, the weight of the ferroboron master alloy in the raw material for vacuum induction melting is preferably 1.30kg, 1.35kg, 1.40kg, 1.45kg and 1.5kg.
Preferably, the weight of the nickel-magnesium intermediate alloy in the raw material for vacuum induction smelting is preferably 14kg, 15kg, 16kg and 17kg.
Specifically, in S1, the vacuum induction melting includes the following stages:
1) Cold charge baking stage: firstly, carrying out open furnace cold charging on nickel plates, graphite carbon, metallic chromium, molybdenum strips and ultrapure iron in the raw materials, sequentially spreading the materials at the bottom of a crucible from bottom to top, sealing the furnace for evacuation after charging, and baking with power of 100-300kW, preferably 100kW, 150kW, 200kW and 250kW after the vacuum degree is lower than 5Pa, and slowly increasing the power to 800-1200kW, preferably 800kW, 900kW, 1000kW, 1100kW and 1200kW until the materials are completely melted;
2) A first refining stage: controlling the temperature within 1520-1560 ℃ and the vacuum degree to be less than or equal to 1Pa, simultaneously carrying out electromagnetic stirring, adding niobium strips, stirring for 0.5h, then reducing the power to 50-150kW, adding aluminum ingots and titanium ingots after the film forming on the surface of molten steel, and heating with 500-800kW until the materials are completely melted;
3) And a second refining stage: controlling the temperature within 1440-1500 ℃ and the vacuum degree less than or equal to 1Pa, simultaneously carrying out electromagnetic stirring, and then reducing the power to 300-500kW for heat preservation;
4) Adding volatile and easily burnt raw materials: filling Ar gas with the pressure of 15000-30000Pa, adding the nickel-magnesium intermediate alloy and the ferroboron intermediate alloy, and measuring the temperature after 10-15 min;
5) Casting steel: and (5) regulating the temperature to 1460-1480 ℃ and casting steel.
Specifically, in the cold charge baking stage, the baking time is 0.5-2h, preferably 0.5h, 1h, 1.5h, 2h.
Specifically, in the first refining stage, the refining time is 0.8-1.5h, preferably 0.8h, 1h, 1.2h, 1.5h.
In particular, in the second refining stage, the refining time is 1-2h, preferably 1h, 1.2h, 1.4h, 1.6h, 1.8h, 2h.
Specifically, in S2, the slag system of the protective atmosphere electroslag smelting is: caF (CaF) 2 :MgO:Al 2 O 3 CaO=50%: 5%:25%:20%, the slag amount of the protective atmosphere electroslag smelting is 90-120kg, the specification of the copper crystallizer is phi 550mm, and the protective atmosphere electroslag smelting comprises the following stages:
1) Slag melting stage: charging the slag into a slag charging bin, wherein the initial slag charging amount is 20-50%, charging and charging are started after power transmission is carried out for 2-5min, and charging time is 15-20min;
2) First steady-state phase: the melting speed and slag pendulum control are adopted, the melting speed is 300-420kg/h, and the slag pendulum is 0.5-0.7mohm;
3) A first heat-seal top stage: the current and slag resistance control is adopted, the current is reduced to 30-45% of the first steady-state stage, and the slag resistance is increased to 160-180% of the first steady-state stage.
Specifically, the slag melting stage adopts current and slag resistance control, the slag melting current is 3000-11000A, the slag resistance is 3-6mohm, and the slag melting time is 50-80min.
Specifically, in the first steady-state stage, ar gas with the pressure of 2000Pa is introduced for protection.
Specifically, in S3, the specification of the copper crystallizer for vacuum consumable smelting is Φ508mm, and the vacuum consumable smelting includes the following steps:
1) Arc starting stage: the current and the molten drop are adopted for control, the current is 3.0-8.0kA, the voltage is 23.0-24.0V, and the time of the arcing stage is 50-80min;
2) Second steady-state phase: adopting melting speed and droplet control, wherein the melting speed is 3.5-3.9kg/min, the droplet is 4-6 droplets per second, he gas is introduced, and the air pressure is controlled to be 400-800Pa;
3) The second heat-seal top stage: with current + droplet control, the current is reduced to 1.4-2.0kA and the droplet is increased from the second steady state phase to 10-16 droplets per second.
The sample pretreatment method has the following beneficial effects:
1. by adopting the triple smelting method of the large-size cast ingot, main element components such as Ni, al, ti, mo, nb, C, B in the produced large-size GH4169 alloy cast ingot are extremely poor and have good component uniformity.
2. By adopting the triple smelting method of the large-size cast ingot, the impurity element content of O, N, S and the like in the produced GH4169 high-temperature alloy is lower, and the purity of the cast ingot is improved.
3. By adopting the method, the smelting process of the finished product is more stable when large-specification cast ingots are produced by three times of smelting, and the stability of metallurgical quality is improved.
4. According to the triple smelting method for the large-size cast ingot, provided by the invention, the temperature range 1520-1560 ℃ in the first refining stage is controlled, the refining time is 0.8-1.5h, the vacuum degree is less than or equal to 1Pa, electromagnetic stirring is performed, the melting speed of materials is enhanced, and meanwhile, the components of molten steel are more uniform.
5. According to the triple smelting method of the large-size cast ingot, in the first refining stage, the niobium strip is added after complete melting and stirring, and after adding, stirring is carried out for 0.5h, so that niobium segregation is reduced.
6. According to the triple smelting method for the large-size cast ingot, provided by the invention, the temperature of the slag pool is slowly reduced in a mode of slowly reducing the current and increasing the slag resistance, so that the effect of reducing the shrinkage cavity depth of the cast ingot is achieved.
7. According to the triple smelting method for the large-size cast ingot, provided by the invention, the smelting power is gradually reduced in a mode of reducing the current and increasing the molten drops, so that the depth of a molten pool is gradually reduced, the depth of shrinkage cavities of the cast ingot is reduced, and the yield of the cast ingot is improved.
Drawings
Fig. 1 is a process flow chart of the triple smelting method provided by the invention.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, the triple smelting is performed as follows:
step 1, vacuum induction melting VIM
The method comprises the steps of (1) carrying out furnace opening cold charging on raw materials of 3338kg of nickel plate, 0.86kg of graphite carbon, 1115kg of metallic chromium, 183kg of molybdenum bar and 1105kg of ultrapure iron, spreading the raw materials in a crucible layer by layer from bottom to top in sequence, sealing the furnace, evacuating, enabling the vacuum degree to be below 5Pa after 30min, and beginning to bake for 2h with 150kW power; after baking, gradually increasing the power in the sequence of 150kW, 250kW (10 min), 350kW (15 min), 450kW (10 min), 600kW (15 min), 800kW (25 min) and 1000kW (holding), feeding the materials into a first refining stage after all the materials are melted down, adjusting the power to 600kW, detecting the temperature of molten steel to 1520-1560 ℃, and the vacuum degree to 1Pa, starting refining for 1h, and simultaneously carrying out electromagnetic stirring; lifting the power to 1000kW, adding niobium strips after 20min, and stirring for 0.5h; reducing the power to 150kW, observing the film on the surface of molten steel in the crucible, then adding 37kg of aluminum ingot and 65kg of titanium ingot, heating with 800kW power until all molten steel enters a second refining stage, adjusting the power parameter to detect the temperature of the molten steel, keeping the temperature between 1440 and 1500 ℃ for 1h, wherein the vacuum degree requirement of the second refining stage is less than or equal to 1Pa, and simultaneously carrying out electromagnetic stirring; reducing the power to 280kW, preserving heat, charging 15000Pa Ar gas, adding 14.5kg of nickel-magnesium intermediate alloy and 1.4kg of ferroboron intermediate alloy, measuring the temperature to 1445 ℃ after 15min, detecting the temperature of molten steel to 1472 ℃ after increasing the power, meeting the casting requirement, and casting into an ingot mould with phi of 440 mm;
after the VIM electrode was demolded and cooled, component detection was performed by sampling at the tip, middle and tail of the electrode, respectively, and the results are shown in table 1.
Table 1GH4169 vacuum induction melting compositions
As can be seen, the electrode head, middle and tail main elements Ni, cr, al, ti, nb, mo, trace elements C, B and the like formed by vacuum induction smelting casting have large extremely poor component uniformity, the S content of the impurity element is about 20ppm, the O content is about 11ppm, and the N content is about 24ppm;
step 2, ESR (equivalent series resistance) smelting by electroslag in protective atmosphere
Carrying out surface treatment on the induction electrode, sawing the head and the tail, then carrying out welding, and carrying out secondary remelting on protective atmosphere electroslag; the selected component proportion is CaF 2 :MgO:Al 2 O 3 CaO=50% > 5% > 25% > 20% slag, weighing 120kg, putting into a slag adding bin, setting a slag adding process, starting to supplement slag after 2min, and supplementing slag adding time for 18min;
the smelting process parameters are set as follows:
technological parameters of the slag melting stage: current flow: 3000A-5000A-8000A-11000A-9500A; slag resistance: 3.0mohm→6.0mohm→4.5mohm→3.8mohm→3.0mohm; time: 1 min-10 min-15 min-20 min;
first steady-state stage process parameters: melting speed: 330kg/h, slag pendulum: 0.50mohm; argon pressure: 2000Pa;
first heat-seal top stage process parameters: current flow: 100% → 85% → 70% → 50% → 30%, slag resistance: 102% →110% →120% →130% →160%, time: 1min, 5min, 10min, 15min, 25min, 220kg of heat sealing jacking starting weight and 40kg of finishing weight;
after the electroslag ingot is cooled, sampling the ingot at the head, middle and tail of the ingot, and detecting the components, wherein the results are shown in Table 2.
TABLE 2GH4169 electroslag cast ingot composition
It can be seen that after electroslag remelting in protective atmosphere, the extreme differences of the head, the middle and the tail of main elements and trace elements in the cast ingot are reduced, and the uniformity of components is improved. The impurity element S in the cast ingot is reduced from 20ppm to 8ppm, the electroslag desulfurization effect is very obvious, the O content is about 9ppm, the N content is about 22ppm, and the gas element content is slightly reduced.
Step 3, vacuum consumable smelting VAR
After forging an electroslag remelting cast ingot, carrying out surface treatment, welding, then carrying out vacuum consumable three remelting, detecting that the vacuum degree is 0.05Pa, the leak rate is 0.094Pa/min after charging, and starting smelting;
the smelting parameters are set as follows:
technological parameters of the arcing stage: current flow: 3.0kA→12.0kA→10.4kA→9.2kA→8.6kA, voltage: 23.8V→24.2V→23.8V→23.6V→23.0V, time: 5min, 10min, 20min, 10min and 15min;
second steady-state stage process parameters: melting speed: 3.7kg/min, melt drop: 6.0 1/s, he gas pressure: 600Pa;
second heat-seal top stage process parameters: current flow: 6.2kA→3.6kA→3.2kA→2.4kA→1.8kA, solution drops: 7.0 1/s-7.5 1/s-8.5 1/s-12.0 1/s-14.0 1/s, time 25 min-15 min-20 min-15 min-25 min; the heat seal top starts with 300kg and ends with 60kg.
After the ingot is taken out of the furnace and cooled, sampling is carried out on the head, middle and tail of the ingot respectively, and the composition detection is carried out, and the results are shown in Table 3.
TABLE 3GH4169 vacuum consumable cast ingot composition
It can be seen that after three remelting processes of vacuum consumable consumption, the head, middle and tail of main elements and trace elements in the cast ingot are extremely small, and the uniformity of components is further improved. The S content of the impurity element in the cast ingot is about 6ppm, the O content is about 7ppm, the N content is about 21ppm, and the gas element content is reduced.
Comparative example 1
The raw materials with the same components as those in the embodiment 1 are adopted for duplex smelting, the vacuum consumable finished product smelting is controlled by the same parameters, the uniformity of the components and the content of impurity elements are detected, and meanwhile, the comparison analysis is carried out with the triple smelting cast ingot in the embodiment 1.
Step 1, vacuum induction melting
The method comprises the steps of (1) carrying out open furnace cold charging on raw materials of 3318kg of nickel plate, 0.86kg of graphite carbon, 1105kg of metallic chromium, 183kg of molybdenum bar and 1135kg of ultrapure iron, laying the raw materials in a crucible layer by layer from bottom to top in sequence, sealing the crucible, evacuating, enabling the vacuum degree to be below 5Pa after 30min, and beginning to bake for 2h with 150kW power; after baking, gradually increasing the power in the sequence of 150kW, 250kW (10 min), 350kW (15 min), 450kW (10 min), 600kW (15 min), 800kW (25 min) and 1000kW (holding), feeding the materials into a first refining stage after all the materials are melted down, adjusting the power to 600kW, detecting the temperature of molten steel to 1520-1560 ℃, and the vacuum degree to 1Pa, starting refining for 1h, and simultaneously carrying out electromagnetic stirring; lifting the power to 1000kW, adding niobium strips after 20min, and stirring for 0.5h; reducing the power to 150Kw, observing the film on the surface of molten steel in the crucible, then adding 37kg of aluminum ingot and 65kg of titanium ingot, heating with 800kW power until all molten steel enters a second refining stage, adjusting the power parameter to detect the temperature of the molten steel, keeping the temperature between 1440 and 1500 ℃ for 1h, wherein the vacuum degree requirement in the second refining stage is less than or equal to 1Pa, and simultaneously carrying out electromagnetic stirring; reducing the power to 280kW, preserving heat, charging 15000Pa Ar gas, adding 14.5kg of nickel-magnesium intermediate alloy and 1.4kg of ferroboron intermediate alloy, measuring the temperature to 1440 ℃ after 15min, detecting the temperature of molten steel to 1470 ℃ after increasing the power, meeting the casting requirement, and casting into an ingot mould with phi of 440 mm;
after the VIM electrode was demolded and cooled, the components were detected by sampling at the tip, middle and tail of the electrode, respectively, and the results are shown in table 4.
Table 4GH4169 vacuum induction melting compositions
It can be seen that the vacuum induction electrode head, middle and tail main elements Ni, cr, al, ti, nb, mo, trace elements C, B and the like of duplex smelting are extremely poor, the uniformity of components is poor, the S content of impurity elements is about 20ppm, the O content is about 11ppm, the N content is about 27ppm, and the vacuum induction electrode is similar to the triple smelting vacuum induction electrode.
Step 2, vacuum consumable smelting of VAR
After forging an electroslag remelting cast ingot, carrying out surface treatment, welding, then carrying out vacuum consumable three remelting, detecting that the vacuum degree is 0.05Pa, the leak rate is 0.094Pa/min after charging, and starting smelting;
the smelting parameters are set as follows:
technological parameters of the arcing stage: current flow: 3.0kA→11.5kA→10.4kA→9.2kA→8.6kA, voltage: 23.8V→24.2V→23.8V→23.6V→23.0V, time: 5min, 10min, 20min, 10min and 15min;
steady state stage process parameters: melting speed: 3.7kg/min, melt drop: 6.0 1/s, he gas pressure: 600Pa;
technological parameters of the heat capping stage: current flow: 6.2kA→3.6kA→3.2kA→2.4kA→1.8kA, solution drops: 6.0 1/s- & gt 7.21/s- & gt 8.7/s- & gt 13.4/s- & gt 14.5/s, and the time is 25 min- & gt 15 min- & gt 20 min- & gt 15 min- & gt 25min; the heat seal top starts with 300kg and ends with 60kg.
After the ingot is taken out of the furnace and cooled, sampling is carried out on the head, middle and tail of the ingot respectively, and the composition detection is carried out, and the results are shown in Table 5.
TABLE 5GH4169 vacuum consumable cast ingot composition
It can be seen that after vacuum consumable secondary remelting, the extreme differences of the head, the middle and the tail of main elements and trace elements in the cast ingot are reduced, and the uniformity of components is improved. The S content of the impurity element in the cast ingot is about 17ppm, the O content is about 9ppm, the N content is about 24ppm, and the gas element content is reduced.
By comparing the data of the embodiment 1 with the data of the comparative example 1, it can be obviously seen that the composition uniformity of the triple cast ingot is obviously superior to that of the double cast ingot by comparing the triple smelting and the double smelting finished cast ingot results, the gas elements O and N in the triple cast ingot are slightly lower, more importantly, the impurity element S content can be removed by about 50% through protective atmosphere electroslag remelting, and the novel triple smelting process can obtain purer cast ingot on the basis of ensuring larger ingot size.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The large-size deformed superalloy cast ingot is characterized in that the deformed superalloy is GH4169 superalloy, and the large-size deformed superalloy cast ingot comprises the following chemical components in percentage by mass: 0.015-0.06% of C, 17.0-21.0% of Cr, 50.0-55.0% of Ni, 0.75-1.15% of Ti, 0.30-0.70% of Al, 2.80-3.30% of Mo, 4.75-5.50% of Nb, less than or equal to 0.0020% of S, less than or equal to 0.0060% of B, less than or equal to 0.30% of Cu, less than or equal to 0.0050% of Mg, less than or equal to 0.0050% of O, less than or equal to 0.010% of N and the balance of Fe.
2. A triple smelting method for a large-size deformed superalloy ingot, which is used for preparing the large-size deformed superalloy ingot according to claim 1, and comprises the following steps:
s1, vacuum induction melting: the raw materials for vacuum induction smelting and the weight thereof are as follows: 3100-3348kg of nickel plate, 1054-1116kg of vacuum degassing chromium, 46-65kg of titanium ingot, 19-37kg of aluminum ingot, 173-183kg of molybdenum strip, 295-340kg of niobium strip, 1.30-1.50kg of ferroboron intermediate alloy, 14-17kg of nickel magnesium intermediate alloy, 1100-1500kg of ultra-pure iron and 0.5-1.0kg of graphite carbon;
the mass fraction of B element of the ferroboron intermediate alloy is not less than 18.5%, and the mass fraction of Mg element of the nickel-magnesium intermediate alloy is not less than 17%;
s2, protective atmosphere electroslag smelting: the protective atmosphere electroslag smelting comprises a slag melting stage, a first steady-state stage and a first heat-seal top stage;
s3, vacuum consumable smelting: the vacuum consumable smelting comprises an arcing stage, a second steady-state stage and a second heat-seal top stage, wherein the pre-vacuum of the vacuum consumable smelting is less than 0.1Pa, and the leak rate is less than 0.13Pa/min.
3. The triple smelting method of large-size deformed superalloy ingot according to claim 2, wherein in step S1, the vacuum induction smelting includes the steps of:
1) Cold charge baking stage: firstly, carrying out furnace opening cold charging on nickel plates, graphite carbon, metallic chromium, molybdenum strips and ultrapure iron in the raw materials, sequentially spreading the raw materials at the bottom of a crucible from bottom to top, sealing the furnace for evacuation after charging is finished, and roasting the raw materials with power of 100-300kW after the vacuum degree is lower than 5Pa, and slowly increasing the power to 800-1200kW until the materials are completely melted;
2) A first refining stage: controlling the temperature within 1520-1560 ℃ and the vacuum degree to be less than or equal to 1Pa, simultaneously carrying out electromagnetic stirring, adding niobium strips, stirring for 0.5h, then reducing the power to 50-150kW, adding aluminum ingots and titanium ingots after the film forming on the surface of molten steel, and heating with 500-800kW until the materials are completely melted;
3) And a second refining stage: controlling the temperature within 1440-1500 ℃ and the vacuum degree less than or equal to 1Pa, simultaneously carrying out electromagnetic stirring, and then reducing the power to 300-500kW for heat preservation;
4) Adding volatile and easily burnt raw materials: filling Ar gas with the pressure of 15000-30000Pa, adding the nickel-magnesium intermediate alloy and the ferroboron intermediate alloy, and measuring the temperature after 10-15 min;
5) Casting steel: and (5) regulating the temperature to 1460-1480 ℃ and casting steel.
4. The triple smelting method of large-size deformed superalloy ingots according to claim 3, wherein the baking time is 0.5-2h in the cold charge baking stage.
5. The triple smelting method of large-size deformed superalloy ingots according to claim 3, wherein in the first refining stage, the refining time is 0.8-1.5h.
6. A triple smelting method of large-scale deformed superalloy ingots according to claim 3, wherein in the second refining stage, the refining time is 1-2 hours.
7. The triple smelting method of large-size deformed superalloy ingot according to claim 2, wherein in step S2, the slag system of the protective atmosphere electroslag smelting is: caF (CaF) 2 :MgO:Al 2 O 3 CaO=50%: 5%:25%:20%, the slag amount of the protective atmosphere electroslag smelting is 90-120kg, the specification of the copper crystallizer is phi 550mm, and the protective atmosphere electroslag smelting comprises the following stages:
1) Slag melting stage: charging the slag into a slag charging bin, wherein the initial slag charging amount is 20-50%, charging and charging are started after power transmission is carried out for 2-5min, and charging time is 15-20min;
2) First steady-state phase: the melting speed and slag pendulum control are adopted, the melting speed is 300-420kg/h, and the slag pendulum is 0.5-0.7mohm;
3) A first heat-seal top stage: the current and slag resistance control is adopted, the current is reduced to 30-45% of the first steady-state stage, and the slag resistance is increased to 160-180% of the first steady-state stage.
8. The triple smelting method of the large-size deformed superalloy ingot according to claim 2, wherein the slagging stage is controlled by current and slag resistance, the slagging current is 3000-11000A, the slag resistance is 3-6mohm, and the slagging time is 50-80min.
9. The triple smelting method of a large-size deformed superalloy ingot according to claim 2, wherein in the first steady-state stage, ar gas with a pressure of 2000Pa is introduced for protection.
10. The triple smelting method of large-size deformed superalloy ingot according to claim 2, wherein in step S3, the size of the copper crystallizer for vacuum consumable smelting is Φ508mm, and the vacuum consumable smelting comprises the following steps:
1) Arc starting stage: the current and the molten drop are adopted for control, the current is 3.0-8.0kA, the voltage is 23.0-24.0V, and the time of the arcing stage is 50-80min;
2) Second steady-state phase: adopting melting speed and droplet control, wherein the melting speed is 3.5-3.9kg/min, the droplet is 4-6 droplets per second, he gas is introduced, and the air pressure is controlled to be 400-800Pa;
3) The second heat-seal top stage: with current + droplet control, the current is reduced to 1.4-2.0kA and the droplet is increased from the second steady state phase to 10-16 droplets per second.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310921855.7A CN116904803A (en) | 2023-07-26 | 2023-07-26 | Triple smelting method for deformed superalloy GH4169 large-size cast ingot |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310921855.7A CN116904803A (en) | 2023-07-26 | 2023-07-26 | Triple smelting method for deformed superalloy GH4169 large-size cast ingot |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116904803A true CN116904803A (en) | 2023-10-20 |
Family
ID=88364491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310921855.7A Pending CN116904803A (en) | 2023-07-26 | 2023-07-26 | Triple smelting method for deformed superalloy GH4169 large-size cast ingot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116904803A (en) |
-
2023
- 2023-07-26 CN CN202310921855.7A patent/CN116904803A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110004312B (en) | Triple smelting process of nickel-based high-temperature alloy GH4698 large-size cast ingot | |
| CN111519068B (en) | Triple smelting process of difficult-deformation nickel-based high-temperature alloy GH4151 | |
| CN111235434B (en) | Preparation method of nickel-based deformed superalloy wheel disc forging used at high temperature | |
| CN106947908B (en) | A kind of method of continuous casting electroslag production 4Cr5MoSiV1 die steels | |
| CN110592506B (en) | GH4780 alloy blank and forging and preparation method thereof | |
| CN106636758B (en) | A kind of smelting process of small dimension nickel base superalloy FGH4097 ingot castings | |
| CN109022925B (en) | Method for reducing Laves phase in nickel-based superalloy steel ingot | |
| CN111663064B (en) | Cast high-temperature alloy and smelting method thereof | |
| CN114457270A (en) | L12Medium-entropy alloy with particles strongly plasticized and preparation method thereof | |
| CN110964990A (en) | High-performance large-diameter thick-wall austenitic stainless steel forged pipe for nuclear power and short-process preparation method thereof | |
| CN114657398A (en) | Large-size nickel-based high-temperature alloy ingot difficult to deform and preparation method thereof | |
| CN110284042A (en) | Superplasticity high-entropy alloy, plate and preparation method thereof | |
| CN113832363A (en) | Titanium alloy ingot and preparation method thereof | |
| CN106591684A (en) | Preparation method for iron, chromium and aluminum alloy ingot castings | |
| CN114934205B (en) | Smelting method for nickel-based superalloy with high purity | |
| CN110735067A (en) | Purification smelting process of nickel-based high-temperature alloys rich in active elements | |
| CN114875253B (en) | Smelting process of nickel-based powder superalloy FGH4096 large-specification ingot | |
| CN110230002B (en) | Martensite steel and preparation method thereof | |
| CN112359251A (en) | Preparation method and application of nickel-chromium-tungsten intermediate alloy | |
| CN116904803A (en) | Triple smelting method for deformed superalloy GH4169 large-size cast ingot | |
| JP7292211B2 (en) | Superalloy manufacturing method | |
| CN115058629A (en) | GH2026 alloy smelting process with high use proportion of return materials | |
| CN108179340B (en) | A kind of low C, H, O, aluminum chromium of N element content and preparation method thereof | |
| CN115491615B (en) | High-temperature alloy large-specification consumable ingot and preparation method thereof | |
| CN115896506A (en) | Preparation technology of low segregation GH3230 alloy high-quality slab |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |