CN117127040A - Purifying smelting method for high-chromium cast nickel-base superalloy return material - Google Patents
Purifying smelting method for high-chromium cast nickel-base superalloy return material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 143
- 238000003723 Smelting Methods 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 26
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 20
- 239000011651 chromium Substances 0.000 title claims abstract description 20
- 238000007670 refining Methods 0.000 claims abstract description 85
- 238000002844 melting Methods 0.000 claims abstract description 45
- 230000008018 melting Effects 0.000 claims abstract description 45
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 238000004381 surface treatment Methods 0.000 claims abstract description 13
- 229910000831 Steel Inorganic materials 0.000 claims description 73
- 239000010959 steel Substances 0.000 claims description 73
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 52
- 238000005520 cutting process Methods 0.000 claims description 28
- 238000005422 blasting Methods 0.000 claims description 27
- 239000000395 magnesium oxide Substances 0.000 claims description 27
- 238000005266 casting Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 23
- 239000000956 alloy Substances 0.000 abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 14
- 239000001301 oxygen Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001029 Hf alloy Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005495 investment casting Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 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
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- 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
- Y02P10/20—Recycling
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a purifying and smelting method for a high-chromium cast nickel-based superalloy return material, and belongs to the technical field of alloy smelting. The technical proposal is as follows: the method comprises the following steps: surface treatment of returned materials, vacuum smelting and pouring; wherein the vacuum smelting comprises a melting period, a high-temperature refining period and a low-temperature refining period. The invention reduces the O, N content of the high-temperature alloy return material to below 10ppm on the premise of meeting the related technical index requirements.
Description
Technical Field
The invention relates to the technical field of alloy smelting, in particular to a purifying smelting method for a high-chromium cast nickel-based superalloy return material.
Background
The yield of the superalloy precision casting is usually 20-30%, and some parts with complex shapes even only have 10%, namely more than 70% of superalloy products exist in the forms of stub bars, pouring gates, risers, scrapped parts, cuttings and the like, and are collectively called superalloy returns. The research on the high-temperature alloy return materials in China is less, a large amount of high Wen Taijin return materials are not fully utilized, and the backlog condition of the return materials is serious. Therefore, the recycling of the returned material of the high-temperature alloy can generate remarkable economic benefit, and how to utilize the purifying smelting process to realize the recycling of the returned material is always the focus of attention in the fields of high-temperature alloy production and research.
Chinese patent No. CN100387736C discloses a vacuum melting process for producing a return alloy of hafnium-containing nickel-base casting superalloy K488, wherein the return alloy is purified by adding rare earth elements, and is subjected to multiple return melting, wherein the N content is lower than 100ppm. The main disadvantages are that: the smelting method of the high-temperature alloy return material adopts rare earth as a final deoxidizing element, and the deoxidizing capability of the rare earth element is limited, so that the rare earth element cannot be fully deoxidized, the denitrification effect is closely related to the oxygen content of the surface active element, and the denitrification can be maximally performed only after the deoxidizing is fully performed. Therefore, the remelting method of the return material of the patent is adopted to remelt the return material of the high-temperature alloy, the nitrogen cannot be reduced to below 10ppm, and the remelting method of the return material of the high-temperature alloy of the patent can only be matched with new materials for use.
The Chinese patent No. 101440436B discloses a purifying smelting process of a high-temperature alloy return material, which adopts a double-deoxidizing double-cooling smelting process and specifically comprises the following steps: a pre-melting stage, a refining stage and a pouring stage. The adoption of the purification smelting process of the patent for vacuum induction smelting of the high-temperature alloy return material can reduce the O, N content of the high-temperature alloy return material to below 10 ppm. However, the process adopts a technical scheme of adding calcium for many times and adopts a magnesia crucible, and calcium addition in the smelting process can lead to severe reaction of molten steel and lead to reaction of calcium and the magnesia crucible, so that the content of metal magnesium in the process of reducing oxygen and nitrogen in the molten steel exceeds the standard, and the related technical index requirements are not met.
In summary, there is a need to develop a new purifying and smelting method for high-temperature alloy return materials, which can reduce the O, N content of the high-temperature alloy return materials to below 10ppm on the premise of meeting the related technical index requirements.
Disclosure of Invention
The invention aims to solve the technical problems that: the purifying and smelting method for the high-chromium cast nickel-based superalloy return material overcomes the defects of the prior art, and achieves the aim of reducing the O, N content of the superalloy return material to below 10ppm on the premise of meeting the requirements of related technical indexes.
The technical scheme of the invention is as follows:
the purifying and smelting method for the high-chromium cast nickel-based superalloy return material comprises the following steps: surface treatment of returned materials, vacuum smelting and pouring; wherein the vacuum smelting comprises a melting period, a high-temperature refining period and a low-temperature refining period; the operation of the high temperature refining period is as follows: when the power is raised to 450+/-5 kW, a thermocouple is used for measuring the temperature, when the surface temperature of the molten steel of the return material after complete melting reaches 1640+/-10 ℃, the molten steel enters a high-temperature refining period, the power is reduced to 125+/-5 kW, the molten steel temperature is kept unchanged, the refining time is 30+/-2 min, and the vacuum degree is less than 1Pa. Wherein, the high-temperature refining temperature cannot be too high, and the reaction between molten steel and a magnesia crucible can be caused when the high-temperature refining temperature is too high; the operation of the low temperature refining period is as follows: after high-temperature refining is finished, cooling is carried out in a power failure mode, when the temperature of molten steel is reduced to 1400+/-10 ℃, the power is adjusted to 100+/-5 kW, the temperature of molten steel is kept unchanged at 1400+/-10 ℃, and the low-temperature refining time is 30+/-2 min; after the low-temperature refining is finished, maintaining the power of 100+/-5 kW unchanged, converting the vacuum melting furnace into an electromagnetic stirring mode from a melting mode, after the molten steel is completely covered, delivering the power of 450+/-5 kW, and when the temperature of the molten steel is 1480+/-10 ℃, adjusting the power to 125+/-5 kW, and maintaining the temperature of the molten steel unchanged for casting.
Preferably, the melting phase operates as follows: the melting phase operates as follows: firstly, putting 1/3 of return materials into a magnesium oxide crucible, vacuumizing by a furnace cover, and adjusting the power from 0kW to 100+/-5 kW for 30+/-2 min when the vacuum degree is less than 5 Pa; then the power is increased to 300+/-5 kW, the power is kept unchanged, and after the returned materials in the magnesia crucible are completely melted, 1/3 of the returned materials are added through a feeding bin; when the return materials in the magnesia crucible are melted, the power is increased to 400+/-5 kW, the power is kept unchanged, and then the rest 1/3 of the return materials are added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450+/-5 kW.
Preferably, the surface treatment operation of the return material is as follows: and selecting a return material, and cutting and shot blasting the return material. The purpose of the cutting treatment is to facilitate the return materials to be put into a vacuum smelting furnace, so that bridging phenomenon in the smelting process is prevented; the purpose of the shot blasting treatment is to remove slag inclusions, oil stains and the like on the surface of the return material.
Compared with the prior art, the invention has the following beneficial effects:
according to the purification smelting method for the high-chromium casting nickel-based superalloy return material, the purification smelting process is adopted in the process of smelting the high-chromium casting superalloy return material, so that the O, N content of the superalloy return material is reduced to below 10ppm on the premise of meeting the related technical index requirements.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the technical solution of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention.
The following examples all used a 500Kg vacuum melting furnace with K4648 alloy return.
Example 1
The purifying and smelting method for the high-chromium cast nickel-based superalloy return material comprises the following steps of:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is raised to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1640 ℃, the high-temperature refining period is entered, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1400 ℃, the power is adjusted to 100kW, the temperature of molten steel is kept unchanged at 1400 ℃, and the low-temperature refining time is 30min;
s3, pouring: after the low-temperature refining is finished, maintaining the power of 100kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, after the molten steel is completely formed into a film, delivering the power of 450kW, and when the temperature of the molten steel is 1480 ℃, adjusting the power to 125kW, and maintaining the temperature of the molten steel unchanged for pouring.
Example 2
The purifying and smelting method for the high-chromium cast nickel-based superalloy return material comprises the following steps of:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 95kW for 28min when the vacuum degree is less than 5 Pa; then the power is increased to 295kW, the power is kept unchanged, and 1/3 of K4648 return material is added through a feeding bin after the return material in the crucible is completely melted; when the K4648 return material in the crucible is melted, the power is increased to 395kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 445kW;
s22 high-temperature refining period: when the power is raised to 445kW, a thermocouple is adopted to measure the temperature, when the surface temperature of molten steel after the return material is melted reaches 1630 ℃, the high-temperature refining period is entered, the power is reduced to 120kW, the molten steel temperature is kept unchanged, the refining time is 28min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1390 ℃, the power is adjusted to 95kW, the temperature of molten steel is kept unchanged at 1390 ℃, and the low-temperature refining time is 28min;
s3, pouring: after the low-temperature refining is finished, the power of 95kW is kept unchanged, the vacuum melting furnace is changed into an electromagnetic stirring mode from a melting mode, 445kW of power is sent after the molten steel is completely covered, the power is adjusted to 120kW when the temperature of the molten steel is 1470 ℃, and the molten steel is poured without changing the temperature.
Example 3
The purifying and smelting method for the high-chromium cast nickel-based superalloy return material comprises the following steps of:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 105kW for 32min when the vacuum degree is less than 5 Pa; then the power is increased to 305kW, the power is kept unchanged, and 1/3 of K4648 return material is added through a feeding bin after the return material in the crucible is completely melted; when 2/3 of the K4648 return material in the crucible is melted, the power is increased to 405kW, the power is kept unchanged, and then the rest 1/3 of the return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 455kW;
s22 high-temperature refining period: when the power is raised to 455kW, adopting a thermocouple to measure the temperature, when the surface temperature of molten steel reaches 1650 ℃ after the return material is melted, entering a high-temperature refining period, reducing the power to 130kW, keeping the temperature of the molten steel unchanged, and keeping the refining time at 32min and the vacuum degree at 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1410 ℃, the power is adjusted to 105kW, the temperature of molten steel is kept unchanged at 1410 ℃, and the low-temperature refining time is 32min;
s3, pouring: after the low-temperature refining is finished, maintaining the power of 105kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, after the molten steel is completely covered, delivering the power of 455kW, and when the temperature of the molten steel is up to 1490 ℃, adjusting the power to 130kW, and maintaining the temperature of the molten steel unchanged, and pouring.
Comparative example 1
The purifying and smelting method of the high-chromium casting nickel-based superalloy return material of the comparative example 1 comprises the following steps:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is raised to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1640 ℃, the high-temperature refining period is entered, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s3, pouring: after high-temperature refining is finished, maintaining the power of 100kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, electrifying to send the power of 450kW after the molten steel is completely covered, and adjusting the power to 125kW when the temperature of the molten steel is 1480 ℃ to maintain the temperature of the molten steel unchanged for pouring.
Comparative example 2
The purifying and smelting method of the high-chromium casting nickel-based superalloy return material of comparative example 2 comprises the following steps:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is raised to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1640 ℃, the high-temperature refining period is entered, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1400 ℃, the power is adjusted to 100kW, the temperature of molten steel is kept unchanged at 1400 ℃, and the low-temperature refining time is 30min;
s3, pouring: after the low-temperature refining is finished, the power is cut off for cooling treatment, after the molten steel is completely covered, the power is sent to 450kW, when the temperature of the molten steel is 1480 ℃, the power is adjusted to 125kW, and the casting is carried out while the temperature of the molten steel is kept unchanged.
Comparative example 3
The purifying and smelting method of the high-chromium casting nickel-based superalloy return material of the comparative example 3 comprises the following steps:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is increased to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1600 ℃, the molten steel enters a high-temperature refining period, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1400 ℃, the power is adjusted to 100kW, the temperature of molten steel is kept unchanged at 1400 ℃, and the low-temperature refining time is 30min;
s3, pouring: after the low-temperature refining is finished, maintaining the power of 100kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, after the molten steel is completely formed into a film, delivering the power of 450kW, and when the temperature of the molten steel is 1480 ℃, adjusting the power to 125kW, and maintaining the temperature of the molten steel unchanged for pouring.
Comparative example 4
The purifying and smelting method of the high-chromium casting nickel-based superalloy return material of comparative example 4 comprises the following steps:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is raised to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1640 ℃, the high-temperature refining period is entered, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1430 ℃, the power is adjusted to 100kW, the temperature of molten steel is kept unchanged at 1400 ℃, and the low-temperature refining time is 30min;
s3, pouring: after the low-temperature refining is finished, maintaining the power of 100kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, after the molten steel is completely formed into a film, delivering the power of 450kW, and when the temperature of the molten steel is 1480 ℃, adjusting the power to 125kW, and maintaining the temperature of the molten steel unchanged for pouring.
Comparative example 5
The purifying and smelting method of the high-chromium casting nickel-based superalloy return material of comparative example 5 comprises the following steps:
s1, surface treatment of returned materials: selecting a return material K4648, and cutting and shot blasting the return material by adopting a cutting machine and a shot blasting machine;
s2 vacuum melting of return materials
S21 melting period: firstly, putting 1/3 of the return material subjected to cutting and shot blasting into a magnesia crucible of a vacuum smelting furnace, vacuumizing by closing a furnace cover, and adjusting the power from 0kW to 100kW for 30min when the vacuum degree is less than 5 Pa; then the power is increased to 300kW, the power is kept unchanged, and after the returned materials in the crucible are completely melted, 1/3 of the returned materials of K4648 are added through a feeding bin; when the K4648 return material in the crucible is melted, the power is increased to 400kW, the power is kept unchanged, and then the rest 1/3 return material is added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450kW;
s22 high-temperature refining period: when the power is raised to 450kW, a thermocouple is adopted to measure the temperature, when the temperature of molten steel reaches 1640 ℃, the high-temperature refining period is entered, the power is reduced to 125kW, the temperature of the molten steel is kept unchanged, the refining time is 30min, and the vacuum degree is 0.1Pa;
s23, low-temperature refining period: after high-temperature refining is finished, cooling is performed in a power failure, when the temperature of molten steel is reduced to 1380 ℃, the power is adjusted to 100kW, the temperature of molten steel is kept unchanged at 1400 ℃, and the low-temperature refining time is 30min;
s3, pouring: after the low-temperature refining is finished, maintaining the power of 100kW unchanged, converting the vacuum melting furnace from a melting mode to an electromagnetic stirring mode, after the molten steel is completely formed into a film, delivering the power of 450kW, and when the temperature of the molten steel is 1480 ℃, adjusting the power to 125kW, and maintaining the temperature of the molten steel unchanged for pouring.
The oxygen and nitrogen content of the K4648 alloy ingots of examples 1-3 and comparative examples 1-5 were detected by an oxygen-nitrogen-hydrogen instrument, four samples were taken for detection, and the standard of GB/T14265 general rule for analysis of hydrogen, oxygen, nitrogen, carbon and sulfur in metallic materials was executed, and the detection results are shown in Table 1:
TABLE 1 detection results of oxygen and Nitrogen content of K4648 alloy ingots of examples 1 to 3 and comparative examples 1 to 5
As can be seen from Table 1, in examples 1-3, the oxygen and nitrogen contents in the return materials of the high-chromium casting superalloy are less than or equal to 10ppm by adopting the high-temperature refining, low-temperature refining and electromagnetic stirring technologies, so that the better level is achieved. Meanwhile, the low-temperature refining has the effect of deoxidizing nitrogen, so that the oxygen and nitrogen content of the alloy ingot of the comparative example 1 which is not subjected to the low-temperature refining is higher. In comparative example 2 in which the low-temperature electromagnetic stirring treatment was not performed, the alloy ingot had a high oxygen and nitrogen content because of the denitrification effect by the electromagnetic stirring. The high-temperature refining temperature of the invention has the effect of reducing oxygen and nitrogen, while the high-temperature refining temperature of the comparative example 3 is lower, so that the oxygen and nitrogen content of the prepared alloy ingot is higher. In comparative example 4, high temperature is adopted in both the high temperature refining and the low temperature refining processes, so that oxygen and nitrogen are not easy to remove, and finally the oxygen and nitrogen content of the prepared alloy ingot is high. In comparative example 5, low-temperature melting was used in the low-temperature refining step, which resulted in difficulty in removal of oxygen and nitrogen, and finally resulted in high oxygen and nitrogen content of the alloy ingot.
Claims (3)
1. The purifying and smelting method for the high-chromium cast nickel-based superalloy return material is characterized by comprising the following steps of: surface treatment of returned materials, vacuum smelting and pouring; wherein the vacuum smelting comprises a melting period, a high-temperature refining period and a low-temperature refining period;
the operation of the high temperature refining period is as follows: when the power is increased to 450+/-5 kW, when the temperature of the molten steel reaches 1640+/-10 ℃, the high-temperature refining period is entered, the power is reduced to 125+/-5 kW, the temperature of the molten steel is kept unchanged, the refining time is 30+/-2 min, and the vacuum degree is less than 1Pa;
the operation of the low temperature refining period is as follows: after high-temperature refining is finished, cooling is carried out in a power failure mode, when the temperature of molten steel is reduced to 1400+/-10 ℃, the power is adjusted to 100+/-5 kW, the temperature of molten steel is kept unchanged at 1400+/-10 ℃, and the low-temperature refining time is 30+/-2 min;
after the low-temperature refining is finished, maintaining the power of 100+/-5 kW unchanged, converting the vacuum melting furnace into an electromagnetic stirring mode from a melting mode, after the molten steel is completely covered, delivering the power of 450+/-5 kW, and when the temperature of the molten steel is 1480+/-10 ℃, adjusting the power to 125+/-5 kW, and maintaining the temperature of the molten steel unchanged for casting.
2. The method for purifying and smelting a high chromium cast nickel-base superalloy return charge according to claim 1, wherein the melting phase is operated as follows: firstly, putting 1/3 of return materials into a magnesium oxide crucible, vacuumizing by a furnace cover, and adjusting the power from 0kW to 100+/-5 kW for 30+/-2 min when the vacuum degree is less than 5 Pa; then the power is increased to 300+/-5 kW, the power is kept unchanged, and after the returned materials in the magnesia crucible are completely melted, 1/3 of the returned materials are added through a feeding bin; when the return materials in the magnesia crucible are melted, the power is increased to 400+/-5 kW, the power is kept unchanged, and then the rest 1/3 of the return materials are added into the magnesia crucible; after the returned materials are completely melted, the power is increased to 450+/-5 kW.
3. The method for purifying and smelting a high-chromium cast nickel-base superalloy return material according to claim 1, wherein the surface treatment of the return material is performed as follows: and selecting a return material, and cutting and shot blasting the return material.
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| CN102965535A (en) * | 2012-11-15 | 2013-03-13 | 沈阳黎明航空发动机(集团)有限责任公司 | Method for preparing alloy K414 from return scraps of cast high-temperature alloy K414 |
| WO2021036226A1 (en) * | 2019-08-28 | 2021-03-04 | 北京钢研高纳科技股份有限公司 | Large-size high-niobium and high-temperature 706 alloy ingot and smelting process thereof |
| CN115948657A (en) * | 2022-12-26 | 2023-04-11 | 江苏美特林科特殊合金股份有限公司 | Purification and recovery method of high-temperature alloy return material |
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| WO2021036226A1 (en) * | 2019-08-28 | 2021-03-04 | 北京钢研高纳科技股份有限公司 | Large-size high-niobium and high-temperature 706 alloy ingot and smelting process thereof |
| CN115948657A (en) * | 2022-12-26 | 2023-04-11 | 江苏美特林科特殊合金股份有限公司 | Purification and recovery method of high-temperature alloy return material |
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