CN116426837A - High-strength high-toughness corrosion-resistant plastic die steel and preparation method thereof - Google Patents
High-strength high-toughness corrosion-resistant plastic die steel and preparation method thereof Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 56
- 239000010959 steel Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005260 corrosion Methods 0.000 title claims abstract description 20
- 230000007797 corrosion Effects 0.000 title claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 49
- 238000005242 forging Methods 0.000 claims abstract description 32
- 238000003723 Smelting Methods 0.000 claims abstract description 17
- 230000001681 protective effect Effects 0.000 claims abstract description 13
- 238000005496 tempering Methods 0.000 claims abstract description 10
- 230000006698 induction Effects 0.000 claims abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 6
- 239000000956 alloy Substances 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000002893 slag Substances 0.000 claims description 32
- 238000000137 annealing Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- 238000010079 rubber tapping Methods 0.000 claims description 20
- 229910008455 Si—Ca Inorganic materials 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 8
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000009792 diffusion process Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 5
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 5
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 239000010436 fluorite Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000004571 lime Substances 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 230000003009 desulfurizing effect Effects 0.000 claims description 2
- 238000010583 slow cooling Methods 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 24
- 229910001214 P-type tool steel Inorganic materials 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 229910001105 martensitic stainless steel Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000009849 vacuum degassing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- PKOMXLRKGNITKG-UHFFFAOYSA-L calcium;hydroxy(methyl)arsinate Chemical compound [Ca+2].C[As](O)([O-])=O.C[As](O)([O-])=O PKOMXLRKGNITKG-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002436 steel type 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
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/0006—Adding metallic additives
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/0037—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00 by injecting powdered material
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
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- C21C7/064—Dephosphorising; Desulfurising
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- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/10—Handling in a vacuum
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D1/26—Methods of annealing
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- 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
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Abstract
The invention discloses high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel and a preparation method thereof, and belongs to the technical field of alloy smelting. The plastic die steel comprises the following components in percentage by weight: c:0.37 to 0.42 percent of Mn:0.45 to 0.55 percent of Si:0.32 to 0.38 percent, S: less than or equal to 0.003 percent, P: less than or equal to 0.023 percent, cr:11.90 to 12.20 percent of Mo:2.25 to 2.35 percent of V: 0.45-0.55%, N:0.07 to 0.12 percent of residual element Ti: less than or equal to 0.01 percent, nb: less than or equal to 0.015 percent, and the balance being iron. The preparation method comprises the steps of firstly adopting a non-vacuum induction furnace, an LF furnace and a VD furnace to carry out primary smelting, then adopting a protective atmosphere electroslag furnace to carry out secondary remelting to obtain a uniform steel ingot with high purity, and finally obtaining a 4T large module with uniform structure and high purity through high-temperature homogenization, cooling forging and superfine treatment, wherein the content of inclusions is low, the grain size is high and can reach 10 levels, the impact of a transverse notch can reach 50J, the tempering hardness reaches 50HRC, and the corrosion resistance can reach less than or equal to 0.01mm/a.
Description
Technical Field
The invention relates to a preparation process of high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel, in particular to a die steel material for injection molding, and belongs to the technical field of die steel materials.
Background
With the rapid development of the Chinese die industry, a huge market is provided for domestic die steel, and the improvement of the yield, variety, specification and quality level of the domestic die steel is driven. A large number of steel grades required by the die industry are developed and introduced in the metallurgical industry in China, but the domestic die steel is still difficult to fully meet the demands of the domestic die market in terms of variety and quality.
With the increasing popularization of CAD, CAE, CAMA technology in mold design, plastic molds are developing towards large-scale, complex, precise and multi-cavity, and the novel plastic mold steel has enough surface hardness, strength and toughness; has excellent machinability and good polishing performance; the heat treatment deformation is small and the corrosion resistance is good.
The yield and variety specifications of some novel plastic die steels developed in China still fail to meet the development needs of the plastic die industry, and the main expression is as follows: (1) The existing plastic die steel cannot obtain a large steel ingot with uniform structure and high purity; (2) The existing plastic die steel has higher nonmetallic inclusion content and low grain size grade.
Therefore, there is a need for a new plastic mold steel with excellent properties, which is required to be diversified in specifications, refined and manufactured, and to be widely popularized, and a series of plastic mold steel types is continuously supplemented and perfected. And how to produce a large steel ingot with uniform structure and high purity and a plastic die steel with low inclusion content and high grain size grade becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problems, thereby providing the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel and the preparation process thereof, meeting the use requirements in the field of high-end plastic die steel products, solving the problems that the existing plastic die steel cannot produce large steel ingots with uniform tissues and high purity, and cannot reduce the inclusion content and improve the grain size grade of the plastic die steel.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the invention firstly provides a high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel, which comprises the following elements in percentage by weight: c:0.37 to 0.42 percent of Mn:0.45 to 0.55 percent of Si:0.32 to 0.38 percent, S: less than or equal to 0.003 percent, P: less than or equal to 0.023 percent, cr:11.90 to 12.20 percent of Mo:2.25 to 2.35 percent of V: 0.45-0.55%, N:0.07 to 0.12 percent of residual element Ti: less than or equal to 0.01 percent, nb: less than or equal to 0.015 percent, and the balance being iron.
The invention also provides a preparation method of the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel with the element composition, which comprises the following steps:
A. preparing alloy according to the above element component proportion, smelting molten steel uniformly by a non-vacuum induction furnace, wherein the smelting temperature is 1490-1510 ℃, continuously adding slag in the smelting process for deoxidizing and desulfurizing, removing slag to be more than or equal to 90% after the slag is melted, adding slag again for slagging, adding Al powder or Si-Ca powder for diffusion deoxidizing, fully stirring and heating to 1530-1560 ℃ for sampling analysis, heating to more than or equal to 1600 ℃, and tapping into an LF furnace;
B. adding lime and fluorite after the ladle is put into an LF station, heating and slag adjustment, adding carbon powder, al powder and Si-Ca powder, diffusing and deoxidizing to maintain a reducing atmosphere, keeping the white slag for more than or equal to 30min, adding a deoxidizer to maintain the reducing atmosphere, heating to 1710-1740 ℃, deslagging to more than or equal to 60%, and tapping into a VD station;
C. adding rare earth and Si-Ca to adjust Si components before evacuating in a VD furnace, wherein the total evacuating time is 20-25min, the ultimate vacuum is less than or equal to 133Pa, the holding time is more than or equal to 8min, adding N-Cr after breaking, and statically blowing argon for more than or equal to 12min, and tapping and casting at the temperature of 1520-1525 ℃;
D. pouring the electrode rod for 4 hours, demolding, air-cooling to 200-300 ℃, immediately charging and annealing, and carrying out flat head and surface polishing treatment on two ends of the electrode rod after annealing is finished;
E. placing the electrode rod treated in the step D as an electrode in an electroslag remelting furnace in protective atmosphere for secondary remelting purification to form an electroslag ingot;
F. placing the steel ingot treated in the step E into a heating furnace, heating to 500 ℃ at a speed of 80 ℃/h or less, preserving heat for 5 hours, heating to 850 ℃ at a speed of 150 ℃/h or less, preserving heat for 30 hours at a speed of 1250 ℃ or less, cooling to 1180 ℃ and preserving heat for 2 hours, and discharging from the furnace for forging;
G. air cooling to 350+/-50 ℃ after forging, then placing in a hot pit or charging and slow cooling to 100-150 ℃, charging into a furnace in time, immediately charging and annealing at 350+/-20 ℃, and performing flaw detection, flat head grinding treatment after annealing;
H. and C, carrying out superfine treatment on the module treated in the step G to obtain the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel.
Preferably, in step A, the melting of the molten steel is carried out in a 20T non-vacuum induction furnace, and Al ingot (20 Kg/branch) is added with flow during tapping.
Preferably, in the step B, the Al powder, the C powder and the Si-Ca powder are added in a mode of small batches.
Preferably, in step C, the rare earth is added in an amount of 0.5Kg/T before the VD furnace is evacuated.
Preferably, in the step D, the annealing temperature is 700-750 ℃, the heat preservation time is more than or equal to 24 hours, and the furnace cooling is carried out at the speed of less than or equal to 30 ℃/h to 500 ℃, and the furnace is taken out for air cooling.
Preferably, in step E, a protective atmosphere electroslag remelting is used 66 # And pre-slag, wherein the melting speed is 7.0-6.7 Kg/min, the electroslag is finished, the furnace cooling is not less than 90min, and then the cooling time is not less than 72h.
Preferably, in the step F, the forging process is two-pier two-drawing two-fire forming, the forging temperature is more than or equal to 1050 ℃, and the final forging temperature is more than or equal to 850 ℃.
Preferably, in the step G, the annealing temperature is 700-750 ℃, the heat preservation time is more than or equal to 30 hours, and the furnace cooling is carried out at the speed of less than or equal to 30 ℃/hour until the temperature reaches 500 ℃, and the furnace is taken out for air cooling.
Preferably, in the step H, the ultra-fine process is one-time quenching and tempering.
The beneficial effects of the invention are as follows:
(1) According to the preparation process of the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel, the obtained die steel material is uniform in structure, high in purity and good in corrosion resistance, and the purity of the die steel material is higher through LF ladle refining, VD furnace vacuum degassing and secondary remelting by a protective atmosphere electroslag furnace. Finally, adopting a 6000T press for forging, and carrying out cooling forging, two-pier two-drawing two-fire forging and superfine to improve the uniformity of metallographic structure of the material and reduce banding and reticulation.
(2) The die steel material produced by the invention has very low inclusion grade, the band structure grade can reach SA1 grade by sampling and checking according to a microscopic examination evaluation standard rating chart microscopic examination method of SEP1614 hot work die steel, the grain size grade can reach 10 grade by rating according to an ASTM E112 metal average grain size measuring method, and after quenching at 1030 ℃ and tempering at 250 ℃ for two times, the notch-free impact can reach 50J, and the tempering hardness reaches 50HRC. As the martensitic stainless steel containing N and high Mo, the corrosion resistance is very excellent, and can reach less than or equal to 0.01mm/a.
(3) The die steel material produced by the preparation method provided by the invention has good economic and social benefits in the high-end plastic die steel market, and is suitable for popularization and application.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. 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
A preparation process of high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel comprises the following element components in percentage by weight:
TABLE 1
Example 2
The preparation method of the 4Cr12Mo2VN plastic die steel corresponding to the sample 1 comprises the following steps:
preparing alloy according to the component proportions of the elements, smelting and homogenizing by a 20T non-vacuum induction furnace, wherein the smelting temperature is 1490 ℃, continuously adding slag to carry out deoxidation and desulfurization in the smelting process, deslagging by 90% after the slag is converted and removing slag, adding a proper amount of Al powder or Si-Ca powder to carry out diffusion deoxidation, fully stirring and heating to 1530 ℃, sampling and analyzing, heating to 1600 ℃, and tapping into an LF furnace; adding 1 Al ingot (20 Kg) along with the flow during tapping;
step B, adding a proper amount of lime and fluorite after the seat bag is put into an LF station, heating and slag adjustment, adding carbon powder, al powder and Si-Ca powder in batches for multiple times, diffusing and deoxidizing to maintain a reducing atmosphere, keeping the white slag for 30min, adjusting components according to the sampling result of the step A, adding a proper amount of deoxidizer to maintain the reducing atmosphere (strictly forbidden to use Al final deoxidization), heating to 1710 ℃, deslagging by 60%, tapping, and putting into a VD station;
adding 0.5Kg/T of rare earth and Si-Ca to adjust Si components before evacuating in a C, VD furnace, wherein the total evacuating time is 20min, the ultimate vacuum is 133Pa, the holding time is 8min, adding N-Cr (the N-Cr can be added after baking) after breaking, and carrying out static argon blowing for 12min, and tapping and pouring at the temperature of 1520 ℃;
step D, pouring the electrode rod for 4 hours, demolding, immediately charging and annealing after air cooling to 200 ℃, wherein the annealing temperature is 700 ℃, the heat preservation time is 24 hours, and discharging and air cooling after furnace cooling to 500 ℃ at 30 ℃/h; after annealing is finished, the flat ends of the two ends of the electrode rod are subjected to surface finishing treatment;
e, placing the electrode rod treated in the step D as an electrode in a protective atmosphere electroslag remelting furnace for secondary remelting purification to form an electroslag ingot; protective atmosphere electroslag application 66 # Pre-slag, wherein the melting speed is 7.0Kg/min, electroslag is finished, furnace cooling is performed for 90min, and cooling time is 72h;
step F, placing the steel ingot treated in the step E into a heating furnace, heating to 500 ℃ at 80 ℃/h for 5 hours, heating to 850 ℃ at 150 ℃/h for 5 hours, heating to 1250 ℃ at 200 ℃/h for 30 hours, cooling to 1180 ℃ at the furnace door, and discharging from the furnace for forging; the forging process is two-pier two-drawing two-fire forming, the forging temperature is 1050 ℃, and the final forging temperature is 850 ℃;
step G, air cooling to 350+/-50 ℃ after forging, then heating to pit or charging to 100 ℃ slowly, charging into a furnace in time, immediately charging into the furnace for annealing at 350 ℃, wherein the annealing temperature is 700 ℃, the heat preservation time is 30 hours, and discharging from the furnace for air cooling after furnace cooling to 500 ℃ at 30 ℃/h; performing flaw detection, flat head and grinding treatment after annealing;
and step H, carrying out superfine treatment on the module treated in the step G, wherein the superfine treatment is one-time quenching and tempering treatment, and thus the required material is prepared.
Example 3
The preparation method of the 4Cr12Mo2VN plastic die steel corresponding to the sample 2 comprises the following steps:
preparing alloy according to the component proportions of the elements, smelting and homogenizing by a 20T non-vacuum induction furnace, wherein the smelting temperature is 1510 ℃, continuously adding slag materials for deoxidization and desulfurization in the smelting process, removing slag by 92% after the slag materials are melted, adding slag materials again for slagging, adding a proper amount of Al powder or Si-Ca powder for diffusion deoxidization, fully stirring and heating to 1560 ℃ for sampling analysis, heating to 1610 ℃, and tapping into an LF furnace; adding 1 Al ingot (20 Kg) along with the flow during tapping;
step B, adding a proper amount of lime and fluorite after the seat bag is put into an LF station, heating and slag adjustment, adding carbon powder, al powder and Si-Ca powder in small batches for diffusion deoxidization for 35min, adjusting components according to the sampling result of the step A, adding a proper amount of deoxidizer for maintaining the reducing atmosphere (strictly forbidden to use Al final deoxidization), heating to 1740 ℃, deslagging and tapping 63 percent into a VD station;
adding 0.5Kg/T of rare earth and Si-Ca to adjust Si components before evacuating in a C, VD furnace, wherein the total evacuating time is 25min, the ultimate vacuum is 130Pa, the holding time is 10min, adding N-Cr (the N-Cr can be added after baking) after breaking, and tapping and pouring at the temperature of 1525 ℃ after static argon blowing for 15 min;
step D, demolding after the electrode rod is poured for 4 hours, immediately charging and annealing after air cooling to 300 ℃, wherein the annealing temperature is 750 ℃, the heat preservation time is 25 hours, and discharging and air cooling after furnace cooling to 500 ℃ at 28 ℃/h; after annealing is finished, the flat ends of the two ends of the electrode rod are subjected to surface finishing treatment;
e, placing the electrode rod treated in the step D as an electrode in a protective atmosphere electroslag remelting furnace for secondary remelting purification to form an electroslag ingot; protective atmosphere electroslag application 66 # Pre-slag, wherein the melting speed is 6.7Kg/min, electroslag is finished, furnace cooling is performed for 92min, and cooling time is 74h;
step F, placing the steel ingot treated in the step E into a heating furnace, heating to 500 ℃ at 78 ℃/h for 5 hours, heating to 850 ℃ at 145 ℃/h for 5 hours, heating to 1250 ℃ at 190 ℃/h for 30 hours, cooling to 1180 ℃ at the furnace door, and discharging from the furnace for forging; the forging process is two-pier two-drawing two-fire forming, and the forging temperature is 1060 ℃ and the final forging temperature is 860 ℃;
step G, air cooling to 350 ℃ after forging, then placing in a hot pit or charging and slowly cooling to 150 ℃, immediately charging and annealing in a furnace when the temperature of the material is 350 ℃, keeping the annealing temperature at 750 ℃ for 32 hours, and discharging and air cooling after the material is cooled to 500 ℃ at 28 ℃/h; performing flaw detection, flat head and grinding treatment after annealing;
and step H, carrying out superfine treatment on the module treated in the step G, wherein the superfine treatment is one-time quenching and tempering treatment, and thus the required material is prepared.
Example 4
The preparation method of the 4Cr12Mo2VN plastic die steel corresponding to the sample 3 comprises the following steps:
preparing alloy according to the component proportions of the elements, smelting and homogenizing by a 20T non-vacuum induction furnace, wherein the smelting temperature is 1500 ℃, continuously adding slag materials for deoxidization and desulfurization in the smelting process, deslagging by 95% after the slag materials are melted, adding slag materials again for slagging, adding a proper amount of Al powder or Si-Ca powder for diffusion deoxidization, fully stirring and heating to 1550 ℃ for sampling analysis, heating to 1630 ℃, and tapping into an LF furnace; adding 1 Al ingot (20 Kg) along with the flow during tapping;
step B, adding a proper amount of lime and fluorite after the seat bag is put into an LF station, heating and slag adjustment, adding carbon powder, al powder and Si-Ca powder in batches for multiple times, diffusing and deoxidizing to maintain a reducing atmosphere, keeping the white slag for 40min, adjusting components according to the sampling result of the step A, adding a proper amount of deoxidizer to maintain the reducing atmosphere (strictly forbidden to use Al final deoxidization), heating to 1720 ℃, deslagging 65%, and tapping into a VD station;
adding 0.5Kg/T of rare earth and Si-Ca to adjust Si components before evacuating in a C, VD furnace, wherein the total evacuating time is 22min, the ultimate vacuum is 130Pa, the holding time is 12min, adding N-Cr (the N-Cr can be added after baking) after breaking, and tapping and pouring at the temperature of 1522 ℃ after static argon blowing for 16 min;
step D, pouring the electrode rod for 4 hours, demolding, immediately charging and annealing after air cooling to 260 ℃, wherein the annealing temperature is 730 ℃, the heat preservation time is 28 hours, and discharging and air cooling after furnace cooling to 500 ℃ at 25 ℃/h; after annealing is finished, the flat ends of the two ends of the electrode rod are subjected to surface finishing treatment;
e, placing the electrode rod treated in the step D as an electrode in a protective atmosphere electroslag remelting furnace for secondary remelting purification to form an electroslag ingot; protective atmosphere electroslag application 66 # Premelting slag with melting speed of 6.9Kg/min, finishing electroslag, cooling in a furnace for 100min, and cooling for 80h;
step F, placing the steel ingot treated in the step E into a heating furnace, heating to 500 ℃ at 65 ℃/h for 5 hours, heating to 850 ℃ at 130 ℃/h for 5 hours, heating to 1250 ℃ at 160 ℃/h for 30 hours, cooling to 1180 ℃ at the furnace door, and discharging from the furnace for forging; the forging process is that two piers are formed by pulling out two pieces of fire, the forging temperature is 1052 ℃, and the final forging temperature is 855 ℃;
step G, air cooling to 360 ℃ after forging, then placing in a hot pit or charging and slowly cooling to 130 ℃, immediately charging and annealing in a furnace until the temperature of the material is 330 ℃, keeping the annealing temperature at 720 ℃ for 35 hours, and discharging and air cooling after cooling to 500 ℃ at 26 ℃/h; performing flaw detection, flat head and grinding treatment after annealing;
and step H, carrying out superfine treatment on the module treated in the step G, wherein the superfine treatment is one-time quenching and tempering treatment, and thus the required material is prepared.
Experimental example 1
The high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel material prepared by the method of the embodiment 2-4 has uniform structure, high purity and good corrosion resistance, is subjected to LF ladle refining and VD furnace vacuum degassing, and is subjected to secondary remelting by a protective atmosphere electroslag furnace, so that the purity of the die steel material is higher. Finally, adopting a 6000T press for forging, and carrying out cooling forging, two-pier two-drawing two-fire forging and superfine to improve the uniformity of metallographic structure of the material and reduce banding and reticulation.
The inclusion grade of the die steel material produced by the method of the invention can reach the level of the following table 2 by sampling and checking according to the standard rating chart microscopic checking method for measuring the nonmetallic inclusion content of the ASTM E45 steel grade:
TABLE 2
The strip structure grade can reach SA1 grade by sampling and checking according to a microscopic inspection evaluation standard rating chart microscopic inspection method of SEP1614 hot work die steel, the grain size grade can reach 10 grade by rating according to an ASTM E112 metal average grain size measuring method, and after quenching at 1030 ℃ and tempering at 250 ℃ for two times, the notch-free impact can reach 50J, and the tempering hardness reaches 50HRC. As the martensitic stainless steel containing N and high Mo, the corrosion resistance is very excellent, and can reach less than or equal to 0.01mm/a.
The die steel material produced by the method has good economic and social benefits in the high-end plastic die steel market, and is suitable for popularization and application.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate technical solution, and this description is provided for clarity only, and those skilled in the art should consider the disclosure as a whole, and the technical solutions in the embodiments may be combined appropriately to form other ways that will be understood by those skilled in the art.
Claims (10)
1. The high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel is characterized by comprising the following elements in percentage by weight:
c:0.37 to 0.42 percent of Mn:0.45 to 0.55 percent of Si:0.32 to 0.38 percent, S: less than or equal to 0.003 percent, P: less than or equal to 0.023 percent, cr:11.90 to 12.20 percent of Mo:2.25 to 2.35 percent of V: 0.45-0.55%, N:0.07 to 0.12 percent of residual element Ti: less than or equal to 0.01 percent, nb: less than or equal to 0.015 percent, and the balance being iron.
2. A method for preparing the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel according to claim 1, comprising the following steps:
(1) Preparing alloy according to the above element component proportion, smelting molten steel uniformly by a non-vacuum induction furnace, wherein the smelting temperature is 1490-1510 ℃, continuously adding slag in the smelting process for deoxidizing and desulfurizing, removing slag to be more than or equal to 90% after the slag is melted, adding slag again for slagging, adding Al powder or Si-Ca powder for diffusion deoxidizing, fully stirring and heating to 1530-1560 ℃ for sampling analysis, heating to more than or equal to 1600 ℃, and tapping into an LF furnace;
(2) Adding lime and fluorite after the ladle is put into an LF station, heating and slag adjustment, adding carbon powder, al powder and Si-Ca powder, diffusing and deoxidizing to maintain a reducing atmosphere, keeping the white slag for more than or equal to 30min, adding a deoxidizer to maintain the reducing atmosphere, heating to 1710-1740 ℃, deslagging to more than or equal to 60%, and tapping into a VD station;
(3) Adding rare earth and Si-Ca to adjust Si components before evacuating in a VD furnace, wherein the total evacuating time is 20-25min, the ultimate vacuum is less than or equal to 133Pa, the holding time is more than or equal to 8min, adding N-Cr after breaking, and statically blowing argon for more than or equal to 12min, and tapping and casting at the temperature of 1520-1525 ℃;
(4) Pouring the electrode rod for 4 hours, demolding, air-cooling to 200-300 ℃, immediately charging and annealing, and carrying out flat head and surface polishing treatment on two ends of the electrode rod after annealing is finished;
(5) Placing the electrode rod treated in the step (4) as an electrode in an electroslag remelting furnace in protective atmosphere for secondary remelting purification to form an electroslag ingot;
(6) Placing the steel ingot processed in the step (5) into a heating furnace, heating to 500 ℃ at a speed of 80 ℃ or less and keeping the temperature for 5 hours, heating to 850 ℃ at a speed of 150 ℃ or less and keeping the temperature for 5 hours, heating to 1250 ℃ at a speed of 200 ℃ or less and keeping the temperature for 30 hours, cooling to 1180 ℃ and keeping the temperature for 2 hours, and discharging from the furnace for forging;
(7) Air cooling to 350+/-50 ℃ after forging, then placing in a hot pit or charging and slow cooling to 100-150 ℃, charging into a furnace in time, immediately charging and annealing at 350+/-20 ℃, and performing flaw detection, flat head grinding treatment after annealing;
(8) And (3) carrying out superfine treatment on the module treated in the step (7) to obtain the high-strength high-toughness corrosion-resistant 4Cr12Mo2VN plastic die steel.
3. The preparation method according to claim 2, characterized in that: in the step (1), molten steel is smelted in a 20T non-vacuum induction furnace, and Al ingot is added along with the flow during tapping.
4. The preparation method according to claim 2, characterized in that: in the step (2), carbon powder, al powder and Si-Ca powder are added in batches and small batches.
5. The preparation method according to claim 2, characterized in that: in the step (3), the rare earth is added in an amount of 0.5Kg/T before the VD furnace is evacuated.
6. The preparation method according to claim 2, characterized in that: in the step (4), the annealing temperature is 700-750 ℃, the heat preservation time is more than or equal to 24 hours, and the furnace cooling is carried out at the speed of less than or equal to 30 ℃/h until the temperature reaches 500 ℃, and then the furnace is taken out for air cooling.
7. The preparation method according to claim 2, characterized in that: in the step (5), the protective atmosphere electroslag is 66 # And pre-slag, wherein the melting speed is 7.0-6.7 Kg/min, the electroslag is finished, the furnace cooling is not less than 90min, and then the cooling time is not less than 72h.
8. The preparation method according to claim 2, characterized in that: in the step (6), the forging process is two-pier two-drawing two-fire forming, the forging temperature is more than or equal to 1050 ℃, and the final forging temperature is more than or equal to 850 ℃.
9. The preparation method according to claim 2, characterized in that: in the step (7), the annealing temperature is 700-750 ℃, the heat preservation time is more than or equal to 30 hours, and the furnace cooling is carried out at the speed of less than or equal to 30 ℃/hour until the temperature reaches 500 ℃, and then the furnace is taken out for air cooling.
10. The preparation method according to claim 2, characterized in that: in the step (8), the superfine treatment is one-time quenching and tempering treatment.
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