CN112501403A - Cold-work die steel surface super-hardening treatment process - Google Patents
Cold-work die steel surface super-hardening treatment process Download PDFInfo
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- CN112501403A CN112501403A CN202011379961.XA CN202011379961A CN112501403A CN 112501403 A CN112501403 A CN 112501403A CN 202011379961 A CN202011379961 A CN 202011379961A CN 112501403 A CN112501403 A CN 112501403A
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- C—CHEMISTRY; METALLURGY
- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C—CHEMISTRY; METALLURGY
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C—CHEMISTRY; METALLURGY
- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/56—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
- C21D1/607—Molten salts
Abstract
The invention discloses a surface super-hardening treatment process for cold-work die steel, wherein the cold-work die steel is Crl2MoV die steel and comprises the steps of preheating, TD furnace treatment, salt bath furnace quenching, high-temperature tempering, subsequent treatment and the like. The invention can effectively change the crystal phase structure of the surface of the Crl2MoV die steel, obtain higher surface hardness, effectively eliminate internal stress in the whole heat treatment process and effectively improve the toughness of the Crl2MoV die steel.
Description
Technical Field
The invention belongs to the technical field of die steel, and particularly relates to a surface super-hardening treatment process of cold-work die steel.
Background
Cold work die steel refers to die steel used to deform or shape a metal in a cold state. The most common special cold-work die steel is Crl2 type steel, the carbon content of which is 1.45-2.30%, and the chromium content is 11-13%. Because the hardness and the structure of the die material are important factors influencing the wear resistance of the die, in order to improve the wear resistance of the cold-work die, the hardness of the die is generally required to be 30-50% higher than that of a workpiece, and the structure of the material is tempered martensite or lower bainite on which uniform and fine granular carbides are distributed. To achieve this, the mass fraction of carbon in steel is generally above 0.60%. The die has large stress during working, requires high wear resistance, high hardenability, small deformation and complex shape, and is made of high-carbon high-chromium steel (Crl2, Crl2MoV and the like) in many ways.
For Crl2MoV die steel, the die steel is generally used for manufacturing a die with larger stress during working, and has higher requirement on the surface hardness. According to the regulations of the existing national standard GB/T1299-2014 in China, the Rockwell hardness HRC of the surface of the steel is not lower than 58 after the steel of the Crl2MoV die steel is quenched in an oil medium at 207-255 and 950-1000 ℃. With the development of high-strength materials in the automobile industry, metal processing dies are applied to more severe working conditions, and for common die steel, higher strength and toughness are required to prolong the service life of the dies. The existing Crl2MoV steel has the problems of serious structure segregation, poor toughness and the like. Therefore, how to simultaneously improve the surface hardness and the overall toughness of the existing Crl2MoV die steel is a technical problem which needs to be solved in the field.
Disclosure of Invention
Aiming at least one technical problem in the prior art, the invention provides a surface super-hardening treatment process for cold-work die steel, which has the advantages of simple process and high treatment efficiency, and can simultaneously improve the surface hardness and the overall toughness of Crl2MoV die steel.
The technical scheme for solving the technical problems is as follows: a surface super-hardening treatment process for cold-work die steel, which is Crl2MoV die steel, comprises the following steps:
s1, preheating: heating the cold-work die steel to 750-800 ℃ at a heating rate of 10-20 ℃/min, and then maintaining the temperature at 750-800 ℃ for 1.5-2 h;
s2, TD furnace treatment: putting the cold-work die steel preheated in the step S1 into a TD furnace, heating to 960-1020 ℃ at a heating rate of 10-25 ℃/min, and then maintaining for 9.5-10 h at the temperature of 960-1020 ℃;
s3, quenching in a salt bath furnace: putting the cold-work die steel treated in the step S2 into a salt bath furnace for quenching, wherein the quenching time is 0.5-1.5 h;
s4, high-temperature tempering: heating the cold-work die steel quenched in the step S3 to 540-560 ℃ at a heating rate of 10-20 ℃/min, tempering at a high temperature for 4-4.5 h, and naturally cooling to room temperature;
s5, subsequent treatment: and cleaning and polishing the cold-work die steel tempered in the step S4 to obtain the cold-work die steel with the surface subjected to super-hardening treatment.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step S1, preheating is performed in a vacuum furnace.
Further, in the step S2, the temperature rise rate is controlled to be 18-20 ℃/min.
Further, in the step S2, the temperature is raised to 980 ℃, and then the temperature is maintained at 980 ℃ for 9.5 to 10 hours.
Further, in the step S3, the quenching temperature is 560 to 580 ℃.
Further, in the step S3, the quenching time is controlled to be 0.5 to 0.75 hours.
Further, in the step S3, the salt used for the salt bath quenching is a low melting point nitride salt, and the melting point is lower than 450 ℃.
Further, in the step S4, the temperature increase rate is 15 ℃/min.
Further, in step S5, the subsequent processing further includes a detection operation.
Further, in the step S1, the cold-work die steel is a cold-work die steel die workpiece blank which is subjected to casting molding and size finishing treatment.
The invention has the beneficial effects that: the method does not adopt middle-high temperature preheating, TD furnace heat treatment and one-time high-temperature tempering treatment after salt bath quenching, can greatly improve the surface hardness of Crl2MoV die steel, and does not generate carbon loss in the whole treatment process; the treatment process fully utilizes the hardenability of the Crl2MoV die steel, and after salt bath quenching, the internal crystal phase structure of the Crl2MoV die steel can be effectively changed, so that the toughness of the die steel is enhanced; the process can effectively improve the overall performance of the Crl2MoV die steel, so that the service life of the prepared die is greatly prolonged.
Drawings
FIG. 1 is a microscopic picture of the crystal phase structure of the die steel after the process of the present invention;
FIG. 2 is a crystal phase structure microscope picture of the existing Crl2MoV type die steel.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
The invention relates to a surface super-hardening treatment process of cold-work die steel, which is Crl2MoV die steel and comprises the following steps:
s1, preheating: heating the cold-work die steel to 750-800 ℃ at a heating rate of 10-20 ℃/min, and then maintaining the temperature at 750-800 ℃ for 1.5-2 h;
s2, TD furnace treatment: putting the cold-work die steel preheated in the step S1 into a TD furnace, heating to 960-1020 ℃ at a heating rate of 10-25 ℃/min, and then maintaining for 9.5-10 h at the temperature of 960-1020 ℃;
s3, quenching in a salt bath furnace: putting the cold-work die steel treated in the step S2 into a salt bath furnace for quenching, wherein the quenching time is 0.5-1.5 h;
s4, high-temperature tempering: heating the cold-work die steel quenched in the step S3 to 540-560 ℃ at a heating rate of 10-20 ℃/min, tempering at a high temperature for 4-4.5 h, and naturally cooling to room temperature;
s5, subsequent treatment: and cleaning and polishing the cold-work die steel tempered in the step S4 to obtain the cold-work die steel with the surface subjected to super-hardening treatment.
The Crl2MoV die steel is a first-type cold-work die steel, and comprises the following components according to the regulation of the existing national standard GB/T1299-2014: 1.40-1.60% of C, not more than 0.6% of Si, not more than 0.6% of Mn, 11.00-13.00% of Cr, 0.70-1.20% of Mo, 0.50-1.10% of V, not more than 1.00% of Co, and the balance of Fe. The annealed Brinell hardness HBW is 207-255, the Rockwell hardness HRC of the steel surface is not lower than 58 after quenching treatment and oil medium quenching at 950-1000 ℃.
According to the treatment mode specified by the national standard GB/T1299-2014, the crystalline phase structure of the Crl2MoV type die steel is mainly martensite and is distributed with carbides, the carbides are not formed into a net shape or a strip shape and are aggregated in a block shape, and a microscopic image of the crystalline phase structure is observed by an LEICA optical microscope, and is shown as figure 2. Therefore, the existing Crl2MoV die steel has high hardness after quenching treatment, the Rockwell hardness HRC of the surface can reach 58-62, but the structure segregation is serious, and the toughness is poor. Along with present automobile industry constantly promotes to the requirement of spare part intensity, also more and more high to the toughness requirement of mould, toughness is low excessively can lead to mould fracture in the production process, and when the mould of current Crl2MoV type die steel production was used in the automobile industry field, life can't satisfy the production needs gradually. Although other types of die steel can meet the current requirements on toughness, the die steel has lower hardness than Crl2MoV die steel, is inferior to Crl2MoV die steel in hardenability, and has larger difference from Crl2MoV die steel in surface hardness after the hardness is enhanced by heat treatment.
Through experimental research, the inventor finds that after Crl2MoV die steel is heated at a high temperature, medium-temperature cold quenching is assisted with high-temperature tempering, so that austenite residues are not left in a crystal phase structure of the whole die steel, and the hardness and the toughness are effectively improved. The inventor speculates that the above effects are realized by quenching based on a larger temperature difference, so that carbon can form finer particles, the aggregation degree is reduced, the distribution is more uniform, the nucleation rate can be effectively improved, austenite grains after quenching are finer and more uniform, and after high-temperature tempering is assisted, austenite can be completely converted into martensite, so that the hardness of the die steel is greatly enhanced. And the moderate-temperature cold quenching after the high-temperature heating can also increase the amount of alloy melted into a crystalline phase structure, and a large amount of needle-shaped tempered martensite can be formed in the subsequent heating, so that the toughness of the die steel is effectively improved. The inventor speculates that the high-temperature tempering enables a large amount of carbon to be separated out while the quenched martensite is decomposed, and the carbon can play a certain role in catalyzing in the process, so that the decomposition of austenite and the fusion of alloy are promoted.
Based on the findings, the invention selects the TD furnace for heating treatment instead of oil medium quenching specified by the national standard, and then carries out salt bath quenching, so that the surface hardness of the die steel can be further improved on the basis of improving the overall hardness and toughness, the material hardness, the surface hardness and the toughness of the finally processed die steel are far superior to those of the existing die steel, the overall material performance and the service life are greatly improved, and the technical bias in the field is effectively overcome. The core of the invention is that the synergistic effect generated by the technical processes of TD furnace treatment, salt bath quenching, high-temperature heating, medium-temperature cold quenching and high-temperature tempering is utilized, and the generated technical effect is not the expected superposition of the simple effect. The invention combines the above processes together, the hardness of the whole material is further improved, the surface hardness is further improved, the toughness of the material is enhanced, and the improvement of the performance and the service life of the whole material is beyond expectation.
In a preferred embodiment of the present invention, in step S1, the cold-work die steel is a cold-work die steel die workpiece blank which is formed by casting and subjected to size finishing.
In a preferred embodiment of the present invention, in step S1, the preheating is performed in a vacuum furnace. Avoiding the material from being oxidized.
In a preferred technical scheme of the invention, in the step S2, the temperature rise rate is controlled to be 18-20 ℃/min.
More preferably, in the step S2, the temperature is raised to 980 ℃, and then maintained at 980 ℃ for 9.5 to 10 hours.
In the invention, the temperature control in the heating process of the TD furnace is very important, the temperature rise rate needs to be accurately controlled, carbon precipitation loss can be caused at an excessively high speed, and insufficient surface alloying degree and insufficient hardness can be caused at an excessively low speed. The core purpose of the invention is to harden the surface, improve the hardness and toughness of the base material, and the hardening and toughness of the base material need to utilize the alloying of the material during the transformation of the crystal phase structure, so that the amount of the alloy precipitated on the surface needs to be accurately controlled.
The inventor conducts a large amount of experimental research and adjusts parameters according to personal experience, the TD furnace heat treatment can effectively ensure that carbon element is not lost by adopting the parameter range, and meanwhile, the aggregation amount of alloy elements on the surface is controlled, so that enough alloy elements are reserved in the base material, and the alloying of the base material can be realized during subsequent quenching and tempering treatment. Through detection, about 50% of alloy elements in the die steel are gathered on the surface under the control of the process parameters, about 50% of the alloy elements can still remain in the base material, and the realization of subsequent treatment alloying is ensured.
In a preferred embodiment of the present invention, in the step S3, the quenching temperature is 560 to 580 ℃.
In a preferred embodiment of the present invention, in the step S3, the quenching time is controlled to be 0.5 to 0.75 hours.
In a preferred embodiment of the present invention, in step S3, the salt used in the salt bath quenching is a low melting point nitride salt, and the melting point is lower than 450 ℃.
Based on the purpose and the core principle of the invention, the quenching control is also a more key core point of the invention. The selection of the quenching temperature and time is more critical.
The invention needs to form large temperature difference quenching to ensure that carbon can be scattered to form particles, secondly, the invention also needs a certain quenching temperature to ensure the temperature condition of the alloying process, and finally, the quenching time of the invention needs to ensure the full completion of the alloying process. The inventor finally determines that under the condition of the parameters, the austenite grains after quenching are finer, and the amount of the alloy elements blended in the crystal phase structure of the base material is better and more uniform. The inventor also unexpectedly finds that the carbon element can play a certain role in catalyzing the alloying process at the temperature, so that the time of the whole alloying process is shortened, the quenching time is effectively shortened, and the surface element is prevented from migrating.
And the nitriding treatment of the material surface can be completed in the quenching process by adopting the low-melting-point nitride salt, so that the surface hardness can be further improved, and the surface hardness of the material can be ensured even if the elements on the material surface slightly migrate.
In a preferred embodiment of the present invention, in the step S4, the temperature increase rate is 15 ℃/min.
Tempering treatment is also the core of the invention, and the temperature rise rate of tempering needs to be accurately controlled. The tempering treatment of the invention is a process of final transformation of a material crystal phase structure, and needs to form needle-shaped tempered martensite to ensure the stability and non-migration of alloy elements in the process of crystal phase structure decomposition transformation and simultaneously needs to ensure complete austenite removal. Too high or too low a temperature rise rate can lead to poor or even incomplete overall process results.
In a preferred embodiment of the present invention, in step S5, the subsequent processing further includes a detection operation.
As shown in figure 1, the cold-work die steel prepared by the process contains a large amount of acicular tempered martensite in a crystal phase structure, the carbon element structure is fine and is distributed uniformly, and the whole crystal phase structure is completely martensite and does not contain pearlite and austenite.
The following are specific embodiments of the invention
The following examples adopt Crl2MoV type die steel, and the element ratios are as follows: 1.580 percent of C, 0.2 percent of Si, 0.56 percent of Mn, 12.50 percent of Cr, 0.98 percent of Mo, 0.98 percent of V, 0.80 percent of Co and the balance of Fe.
The following examples were prepared by preparing a stainless steel vessel drawing die, first preparing a die blank by casting, and then performing dimensional finishing and polishing to obtain a stainless steel vessel drawing die blank.
Example 1
S1, preheating: heating the stainless steel vessel drawing die blank to 750 ℃ at the heating rate of 20 ℃/min, and then maintaining the temperature at 750 ℃ for 2 h;
s2, TD furnace treatment: putting the stainless steel vessel drawing die blank preheated in the step S1 into a TD furnace, heating to 1020 ℃ at the heating rate of 25 ℃/min, and then maintaining for 9.5h at the temperature of 1020 ℃;
s3, quenching in a salt bath furnace: putting the stainless steel ware drawing die blank treated in the step S2 into a salt bath furnace for quenching, wherein the quenching time is 1.2 h;
s4, high-temperature tempering: heating the stainless steel vessel drawing die blank quenched in the step S3 to 540 ℃ at a heating rate of 20 ℃/min, tempering at high temperature for 4.5h, and then naturally cooling to room temperature;
s5, subsequent treatment: and cleaning and polishing the stainless steel vessel drawing die blank tempered in the step S4 to obtain the stainless steel vessel drawing die blank with the surface subjected to super-hardening treatment.
Example 2
S1, preheating: heating the stainless steel vessel drawing die blank to 780 ℃ at the heating rate of 15 ℃/min, and then maintaining the temperature at 780 ℃ for 1.7 h;
s2, TD furnace treatment: putting the stainless steel vessel drawing die blank preheated in the step S1 into a TD furnace, heating to 980 ℃ at the heating rate of 18 ℃/min, and then maintaining for 9.5h at the temperature of 980 ℃;
s3, quenching in a salt bath furnace: putting the stainless steel ware drawing die blank processed in the step S2 into a salt bath furnace for quenching, wherein the quenching temperature is 580 ℃, and the quenching time is 0.75 h;
s4, high-temperature tempering: heating the stainless steel vessel drawing die blank quenched in the step S3 to 550 ℃ at a heating rate of 15 ℃/min, tempering at a high temperature for 4.2h, and naturally cooling to room temperature;
s5, subsequent treatment: and (5) cleaning, detecting and polishing the stainless steel ware drawing die blank tempered in the step S4 to obtain the stainless steel ware drawing die blank with the surface being subjected to super-hardening treatment.
Example 3
S1, preheating: heating the stainless steel vessel drawing die blank to 800 ℃ at the heating rate of 10 ℃/min, and then maintaining the temperature at 800 ℃ for 1.5 h;
s2, TD furnace treatment: putting the stainless steel vessel drawing die blank preheated in the step S1 into a TD furnace, heating to 960 ℃ at a heating rate of 10 ℃/min, and then maintaining at the temperature of 960 ℃ for 10 h;
s3, quenching in a salt bath furnace: putting the stainless steel ware drawing die blank treated in the step S2 into a salt bath furnace for quenching, wherein the quenching time is 1.5 h;
s4, high-temperature tempering: heating the stainless steel vessel drawing die blank quenched in the step S3 to 560 ℃ at a heating rate of 10 ℃/min, tempering at high temperature for 4h, and then naturally cooling to room temperature;
s5, subsequent treatment: and cleaning and polishing the stainless steel vessel drawing die blank tempered in the step S4 to obtain the stainless steel vessel drawing die blank with the surface subjected to super-hardening treatment.
Example 4
S1, preheating: heating the stainless steel vessel drawing die blank to 770 ℃ at the heating rate of 15 ℃/min, and then maintaining the temperature at 770 ℃ for 1.8 h;
s2, TD furnace treatment: putting the stainless steel vessel drawing die blank preheated in the step S1 into a TD furnace, heating to 980 ℃ at the heating rate of 20 ℃/min, and then maintaining for 10h at the temperature of 980 ℃;
s3, quenching in a salt bath furnace: putting the stainless steel ware drawing die blank treated in the step S2 into a salt bath furnace for quenching, wherein the quenching temperature is 560 ℃, and the quenching time is 0.5 h;
s4, high-temperature tempering: heating the stainless steel vessel drawing die blank quenched in the step S3 to 550 ℃ at a heating rate of 15 ℃/min, tempering at a high temperature for 4.4h, and naturally cooling to room temperature;
s5, subsequent treatment: and (5) cleaning, detecting and polishing the stainless steel ware drawing die blank tempered in the step S4 to obtain the stainless steel ware drawing die with the surface being subjected to super-hardening treatment.
A stainless steel vessel drawing die prepared by a treatment mode specified in the national standard GB/T1299-2014 is used as a comparative example 1; a stainless steel vessel drawing die prepared by treating in a TD furnace, performing oil cold quenching and then performing conventional low-temperature tempering is taken as a comparative example 2; after quenching in the quenching mode specified in the state GB/T1299-2014, the stainless steel vessel drawing die subjected to high-temperature tempering treatment is taken as a comparative example 3. The performances of the stainless steel vessel drawing dies of the three comparative examples are compared with those of the stainless steel vessel drawing dies manufactured in the embodiments 1 to 4 of the invention, the surface hardness, the overall hardness and the austenite allowance are compared, and the obtained results are shown in the following table 1.
| Categories of | Comparative example 1 | Comparative example 2 | Comparative example 3 | Example 1 | Example 2 | Example 3 | Example 4 |
| Surface hardness HRC | 58 | 64 | 61 | 62 | 66 | 62 | 67 |
| Hardness of base Material HBW | 224 | 206 | 248 | 288 | 309 | 292 | 308 |
| Balance of austenite | 21％ | 18％ | 22％ | 4.2％ | 2.1％ | 4.6％ | 1.7％ |
TABLE 1 comparison of material properties
As can be seen from the data in Table 1, the cold-work die steel treated by the process of the invention is far superior to the existing Crl2MoV die steel in the aspects of base material hardness and surface hardness performance. The Crl2MoV die steel treated by the process has no austenite residue basically, the martensite content is extremely high, and compared with the Crl2MoV die steel treated by the prior art, the austenite residue of which is more than 15%, the toughness of the Crl2MoV die steel treated by the process is also greatly improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A surface super-hardening treatment process for cold-work die steel, wherein the cold-work die steel is Crl2MoV die steel, and is characterized by comprising the following steps:
s1, preheating: heating the cold-work die steel to 750-800 ℃ at a heating rate of 10-20 ℃/min, and then maintaining the temperature at 750-800 ℃ for 1.5-2 h;
s2, TD furnace treatment: putting the cold-work die steel preheated in the step S1 into a TD furnace, heating to 960-1020 ℃ at a heating rate of 10-25 ℃/min, and then maintaining for 9.5-10 h at the temperature of 960-1020 ℃;
s3, quenching in a salt bath furnace: putting the cold-work die steel treated in the step S2 into a salt bath furnace for quenching, wherein the quenching time is 0.5-1.5 h;
s4, high-temperature tempering: heating the cold-work die steel quenched in the step S3 to 540-560 ℃ at a heating rate of 10-20 ℃/min, tempering at a high temperature for 4-4.5 h, and naturally cooling to room temperature;
s5, subsequent treatment: and cleaning and polishing the cold-work die steel tempered in the step S4 to obtain the cold-work die steel with the surface subjected to super-hardening treatment.
2. The process of claim 1, wherein the preheating in step S1 is performed in a vacuum furnace.
3. The cold-work die steel surface super-hardening treatment process according to claim 1, wherein in the step S2, the temperature rise rate is controlled to be 18-20 ℃/min.
4. The process of claim 1, wherein in step S2, the temperature is raised to 980 ℃ and then maintained at 980 ℃ for 9.5-10 h.
5. The process for super-hardening the surface of cold-work die steel according to claim 1, wherein the quenching temperature in step S3 is 560 to 580 ℃.
6. The cold-work die steel surface super-hardening treatment process according to claim 1, wherein in the step S3, the quenching time is controlled to be 0.5-0.75 h.
7. The cold-work die steel surface super-hardening treatment process according to claim 1, wherein in the step S3, the salt used for salt bath quenching is a low-melting-point nitride salt, and the melting point is lower than 450 ℃.
8. The process of claim 1, wherein the temperature increase rate in step S4 is 15 ℃/min.
9. The process of claim 1, wherein the post-treatment step S5 further includes a detection operation.
10. The process of claim 1, wherein the step S1 is to form the work piece blank of the cold-work die steel by casting and size finishing.
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