CN111893277A - Manufacturing method for obtaining dispersed carbide in medium-entropy high-speed steel structure - Google Patents
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Abstract
The invention provides a manufacturing method for obtaining dispersed carbide in a medium-entropy high-speed steel structure, belonging to the field of metal material manufacturing, and the manufacturing method comprises the following steps: the medium-entropy high-speed steel is firstly quenched within the temperature range of 1180-1230 ℃, and then is subjected to tempering treatment for 2-3 times at 480-520 ℃, the final heat treatment structure of the medium-entropy high-speed steel is hard carbide which is dispersed on a martensite matrix, the microhardness reaches above 820HV, and the difficult processing problems of crack initiation, brittle fracture and the like in the subsequent manufacturing process caused by coarse reticular carbide of the traditional high-speed steel can be solved. The medium-entropy high-speed steel contains C, W, Mo and other strong carbide forming elements, and the addition content of alloy elements Cr, V, Co, Ni, Al, Cu and matrix element Fe is regulated to set the alloy entropy value between 1.0R and 1.2R; the method is particularly suitable for the application fields of high-speed steel cutting tools, dies and the like which have high comprehensive performance requirements such as high hardness, high toughness and the like and are prepared by casting, smelting or spray forming and the like.
Description
Technical Field
The invention relates to the technical field of metal material manufacturing, in particular to a manufacturing method for obtaining dispersed carbide in a medium-entropy high-speed steel structure.
Background
High speed steel is a high hardness, high wear resistance, high performance tool steel containing a large amount of strong carbide forming elements (C, W, Mo), the hard carbide types of which mainly include: MC (2100-2800HV), M2C(1800-2250HV)、M6C (1800) -2250HV) and M7C3(1890-2060 HV). Wherein MC is taken as a pro-eutectic phase and can be dispersed and distributed in a martensite matrix in a granular manner, and other types of carbides are eutectic reaction products which are distributed in a net shape and then are solidified in an interdendritic region. The coarse meshed primary carbide is difficult to eliminate in the subsequent forging and heat treatment processes, stress concentration is easily caused, cracks are generated in the machining process, and the service life of the high-speed steel is seriously influenced. In order to obtain dispersed hard carbide (especially high hardness MC phase), it has been studied to promote the network metastable phase M by heat treatment or adding a small amount of alloy elements2C is decomposed into dispersed MC at high temperature, and the decomposition mechanism is M2C+Fe(γ)→M6C + MC, but the effect is not obvious. For example, it has been found that the addition of vanadium is most beneficial in promoting MC nucleation, M, during solidification2C is an alloy element decomposed at high temperature, but the addition of the V content is too high, so that a large amount of austenite is formed in a solidification structure, the hardness of the material is reduced, and carbides are still in net distribution when the addition is insufficient.
Studies on the improvement of the properties of high-speed steels by adding a large amount of alloying elements have also been reported. Chinese patent CN104271775A discloses a composition of high speed tool steel that covers almost all elements of the periodic table of elements, the steel is a tough bainite structure, but does not relate to a method and a composition design scheme for improving the growth morphology of network carbides in high speed steel. Chinese patent CN107513670A proposes a method for improving the anti-oxidation wear performance of high-speed steel by adding multi-component alloy elements, and researches show that after a certain amount of Cr, V, Co, Al, Ni, Cu, Ti and other elements are added into the conventional C-W-Mo series high-speed steel, the alloy still has higher hardness and the typical structure characteristics of martensite carbide-added high-speed steel, and the anti-oxidation wear performance of the multi-component high-speed steel can be improved by adding Cr, Co, Al and other elements. Therefore, the high-speed steel components have been reported to improve specific properties such as heat treatment structure, thermal wear, oxidation resistance and the like by adding a small amount or a large amount of alloy elements. However, there have been no proposals for a composition and a manufacturing process for eliminating the network primary carbides in the solidification structure and obtaining the carbides in a completely dispersed distribution in the final heat-treated structure.
Disclosure of Invention
The invention aims to provide a manufacturing method for obtaining dispersed carbide in a medium-entropy high-speed steel structure. The medium-entropy high-speed steel not only contains C, W, Mo and other strong carbide forming elements which are conventionally added in the traditional high-speed steel, but also needs to adjust the adding contents of Cr, V, Co, Ni, Al, Cu and other alloy elements and a matrix element Fe so as to set the alloy entropy value between 1.0R and 1.2R. After the medium-entropy high-speed steel is treated, hard carbides are dispersed and distributed on a martensite matrix, the microhardness reaches more than 820HV, and the medium-entropy high-speed steel has more excellent crack initiation resistance compared with the traditional high-speed steel.
In order to obtain the hard carbides in dispersed distribution in the final heat treatment structure, the invention discloses a technical means for promoting the pyrolysis of the reticular primary carbides in the solidification structure to obtain the dispersed carbide distribution by utilizing the entropy effect, and the decomposition mechanism is as follows: m2C+Fe(γ)→M6C + MC, the mid-entropy effect can greatly increase the thermodynamic driving force for the reaction to occur. Therefore, a fully dispersed carbide distribution, which is difficult to obtain by conventional high speed steel development, can be obtained by a simple heat treatment. By using the entropy of the medium entropy alloyThe value is generally set at the existing definition between 1.0R and 1.5R, and the invention defines the disclosed high speed steel as medium entropy high speed steel.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a manufacturing method for obtaining dispersed carbides in a medium-entropy high-speed steel structure comprises the following steps: quenching the medium-entropy high-speed steel at 1180-1230 ℃, and then tempering for 2-3 times at 480-520 ℃, wherein the final heat treatment structure of the medium-entropy high-speed steel is hard carbide dispersed on a martensite matrix.
Preferably, the heat preservation time is 0.5-2 hours during quenching treatment; and during tempering, the heat preservation time is 1-2 hours.
A manufacturing method for obtaining dispersed carbides in a medium-entropy high-speed steel structure comprises the following steps: carrying out hot forging treatment on the medium-entropy high-speed steel subjected to quenching treatment in a temperature range of 1180-1230 ℃ at a temperature range of 850-1180 ℃ to obtain better crack initiation resistance;
or heating the smelted sample to 1180-1230 ℃ before hot forging, preserving the temperature for 0.5-2 hours, and then carrying out hot forging treatment at 1180-850 ℃ to obtain better crack initiation resistance.
Preferably, the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃.
For the manufacturing method, the components of the medium-entropy high-speed steel comprise the following components in percentage by weight: 0.7 to 1.5% of C, 5 to 8% of W, and 3 to 6% of Mo.
Preferably, Cr, V, Co, Ni, Al and Cu alloy elements are added into the components of the medium-entropy high-speed steel so as to adjust the entropy value of the alloy components to be between 1.0R and 1.2R, the weight percentage of the added alloy elements is between 0.1 and 4 percent, and the weight percentage of the residual Fe element is controlled to be between 71 and 78 percent.
Preferably, the medium-entropy high-speed steel further comprises Si, Mn, P and S alloy elements, and the weight percentage of each alloy element is as follows: si < 0.5%, Mn < 1.0%, S < 0.05%, P < 0.05%.
Preferably, the medium-entropy high-speed steel is prepared by a fusion casting, smelting or spray forming method.
The invention has the beneficial effects that:
1. in the invention, the medium-entropy high-speed steel can eliminate the wide existence of network primary carbides which are unfavorable for toughness in the traditional high-speed steel through simple quenching treatment in a narrow temperature range of 1180-1230 ℃, and finally, the heat treatment structure is hard carbides which are dispersedly distributed on a martensite matrix.
2. In the invention, the microhardness of the medium-entropy high-speed steel after heat treatment reaches the hardness level of W6Mo5Cr4V2 high-speed steel widely sold in the market, and is higher than 820 HV. Meanwhile, the carbide in the structure is in a dispersion distribution form, so that the steel has better crack initiation resistance, and the difficult processing problems of crack initiation, brittle fracture and the like in the subsequent manufacturing process caused by coarse reticular carbide in the traditional high-speed steel can be solved. Is particularly suitable for the application fields of high-speed steel cutting tools, die manufacturing and the like which have higher requirements on high hardness and high toughness.
3. The invention discloses a technical approach for promoting the pyrolysis of reticular primary carbides in high-speed steel and spheroidizing the reticular primary carbides into dispersed carbides by utilizing a medium entropy effect, which has the technical principle that: the medium-entropy high-speed steel solidification structure is mainly a martensite matrix and M2C-based network primary carbide, but the medium entropy effect causes the network primary carbide to be subjected to pyrolysis reaction M2C+Fe(γ)→M6Compared with the traditional high-speed steel, the C + MC is easier to carry out, the reaction in the medium-entropy high-speed steel has higher reaction thermodynamic driving force, and the reaction is more thorough. This is because M2C+Fe(γ)→M6The Gibbs free energy change in the C + MC reaction equation is shown in formula (1):
ΔG＝ΔH-TΔS (1)
wherein Δ H and Δ S are respectively:
compared with the traditional high-speed steel, the delta G depends on the change of the delta S under the premise that the reaction equation is the same and the enthalpy change delta H in the reaction process is constant. The research of the invention finds that the carbide components in the medium-entropy high-speed steel solidification structure are mainly strong carbide forming elements such as W, Mo, V, C and the like, and are basically similar to the carbide components in the traditional high-speed steel, and the impurity infiltration amount of the added Cr, Ni, Co, Al and Cu alloy elements in the carbide is very small. Thus, in the formation of M6C. MC and M2On the premise of basically unchanging entropy change of C and other carbides, the main difference of Delta S in the reaction process of the traditional high-speed steel and the medium-entropy high-speed steel is from a solid solution phase SFe(γ)Change of (1), Δ SFe(γ)The value of (d) can be calculated by equation 4:
in the formula, ciIs the molar concentration of i members in solid solution, n is the number of members, and R is a constant 8.314.
The Fe (gamma) phase factor of the medium-entropy high-speed steel contains a large amount of alloy elements such as Cr, Ni, Co, Cu, Al and the like, and SFe(γ)The entropy increases rapidly with increasing additions of alloying elements, resulting in more negative Δ S values and a more positive Δ G value for the overall reaction process. It can be seen that M2The C pyrolysis reaction equation (1) has a more negative Δ G in conventional high speed steels and is more stable and difficult to perform. Increasing the mid-entropy effect increases the Δ G value of the reaction, requiring less energy for the reaction. Thus, the network-like primary carbides M are accelerated2The dispersion distribution of carbide in the medium-entropy high-speed steel can be more easily obtained by the pyrolysis process of C.
However, the research of the invention also finds that when the entropy value of the medium-entropy high-speed steel composition system is lower than 1.0R, the dispersion effect of the obtained carbide is not obvious. When the entropy exceeds 1.2R or the Fe content in the components is reduced too much, a complete martensite matrix cannot be obtained in the structure, so that the hardness of the medium-entropy high-speed steel is reduced. Therefore, the entropy value of the medium-entropy high-speed steel disclosed by the invention needs to be adjusted to be between 1.0R and 1.2R through components.
Drawings
FIG. 1 is XRD diffraction patterns of 1210 ℃ quenched structures of a control sample M2 and typical composition samples No.1, No.4 and No.7 in example 1 of the present invention.
FIG. 2 shows the SEM morphology phases of 1210 ℃ quenched tissue of a control sample M2, and typical composition samples No.1, No.4 and No.7 in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a manufacturing method for obtaining dispersed carbide in medium-entropy high-speed steel and a structure thereof, which can be manufactured by conventional or rapid solidification methods such as casting, metallurgical melting, spray forming and the like, and can also be formed by a hot forging method. The fusion casting and forming methods and techniques for preparing these alloys are well known to those skilled in the art, and will not be described in detail herein, and the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
Example 1:
in the composition of Table 1, M2 is a typical composition of commercial W6Mo5Cr4V2 high-speed steel, and the entropy value of the composition of M2 high-speed steel is 0.69R according to formula 4. The samples No.1 to No.7 are different high-speed steel compositions designed in the embodiment, the entropy value of the samples No.1 to No.7 is adjusted by reducing the Fe content from 83 percent to 69 percent and adding other alloy elements at the same time, and the entropy value change of the samples No.1 to No.7 is calculated to be increased from 0.72R to 1.27R according to the formula 4. In the smelting process, the raw materials with prepared components are placed in a copper crucible in a WK type non-consumable vacuum arc furnace developed by Shenyang vacuum technical research, the furnace body is vacuumized, and when the vacuum degree reaches 5 multiplied by 10-3Introducing argon gas (high purity argon gas, purity is more than or equal to 99.9%) under MPa, and repeatedly introducing argon gas for three times to ensure that the raw material is not oxidizedAnd (4) transforming. And after the alloy blocks are uniformly smelted and cooled, turning over the alloy blocks and repeatedly smelting for five times to ensure that all elements in the alloy are uniformly smelted, and finally casting the smelted raw materials into a water-cooled copper mould to obtain 20g of round ingot-shaped samples.
Table 1 chemical composition (wt.%) as described in specific example 1 of the present invention
The control samples M2 and No.1 to No.7 were first quenched at 1210 ℃ for 30 minutes, and then tempered at 500 ℃ for 3 times, each for 1.5 hours.
FIGS. 1 and 2 are XRD diffraction and secondary electron topography images of 1210 ℃ quenched structures of a control sample M2 and sample Nos. 1, 4 and 7, respectively. As can be seen from FIG. 1, the phase structure compositions of the entropy high-speed steels of No.1, No.4 and No.7 are basically similar to that of M2 high-speed steel, and are martensite, retained austenite and M6C、M2C and MC carbides. The carbides in the M2 high-speed steel shown in FIG. 2a are in coarse net distribution at the grain boundaries, and the net carbides in the sample No.1 shown in FIG. 2b have been fractured to some extent. FIG. 2c shows that the carbide in component No.4 is in a particulate form with a dispersion, which is significantly better than that of the M2 and component No. 1. In the No.7 composition shown in FIG. 2d, the carbide is distributed more sparsely and finely at the grain boundary, and is also distributed substantially dispersedly.
Table 2 shows the maximum temper hardness and carbide distribution morphology of the samples of example 1 after the quenching treatment and the tempering treatment.
TABLE 2 maximum hardness and carbide distribution morphology of the samples described in example 1
As can be seen from Table 2, the carbide morphology of the M2 control sample and the samples Nos. 1 to 3 remained in a network distribution, and the carbide distribution of the samples Nos. 4 to 7 was in a dispersion distribution. The maximum temper hardness values of the samples No.1 to No.6 were all greater than 820HV, but the hardness value of the sample No.7 was slightly lower than 820HV due to too much reduced iron content. Thus, as can be seen from the texture and hardness results of example 1, to meet the claims of the present invention: the structure is that hard carbide is dispersed on a martensite matrix, and the maximum tempering hardness is larger than 820 HV. The entropy value of the medium-entropy high-speed steel needs to be adjusted to be between 1.0R and 1.2R, and meanwhile, the Fe content is higher than 68 percent.
And (2) carrying out high-temperature hot forging deformation treatment on the high-speed steel prepared in the embodiment 1, heating the smelted solidification sample to 1180-1230 ℃, preserving heat for 0.5-2 hours, promoting the solidification structure network carbide to be converted into dispersion carbide, and then discharging from a furnace for hot forging, wherein the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃. The samples No.4 to No.7 all had significantly better crack initiation tendencies than the M2 control. Or heating the smelted solidification sample to 1180-1230 ℃, preserving heat for 0.5-2 hours, quenching, reheating the sample, discharging from the furnace, and carrying out hot forging, wherein the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃. The crack initiation tendencies of the samples Nos. 4 to 7 were also significantly better than that of the M2 control.
Example 2:
in the smelting process of the sample in the embodiment, the raw materials with prepared components are placed in a copper crucible in a WK type non-consumable vacuum arc furnace developed by Shenyang vacuum technology research, the furnace body is vacuumized, and when the vacuum degree reaches 5 multiplied by 10-3Introducing argon (high purity argon, the purity is more than or equal to 99.9%) under MPa, and repeatedly introducing argon for three times to ensure that the raw materials are not oxidized. And after the alloy blocks are uniformly smelted and cooled, turning over the alloy blocks and repeatedly smelting for five times to ensure that all elements in the alloy are uniformly smelted, and finally casting the smelted raw materials into a water-cooled copper mould to obtain 20g of round ingot-shaped samples.
The samples No.8 to No.10 were first quenched at 1210 ℃ for 30 minutes, and then tempered at 500 ℃ for 3 times, each time for 1.5 hours.
Table 3 component nos. 8 to 10 are different medium entropy high speed steels designed in this example, and maximum temper hardness and carbide distribution forms after quenching at 1210 ℃ and 3 times tempering at 500 ℃. Wherein the sample No.9 further contains Si: 0.5%, Mn: 1.0%, S: 0.05%, P: common elements such as 0.05% of additive elements and impurity elements in the steel materials are respectively calculated to be 1.01R, 1.19R and 1.19R according to a formula 4. It can be seen from the table that the final heat treatment structure of the samples No.8 to No.10 is hard carbide which is dispersed on a martensite matrix, and the maximum tempering hardness is larger than 820 HV.
Table 3 sample chemistry, entropy and final heat treatment status (wt.%)
The high-speed steel prepared in the embodiment 2 is subjected to high-temperature hot forging deformation treatment, the melted solidification sample is heated to 1180-1230 ℃ and is subjected to heat preservation for 0.5-2 hours, the solidification structure reticular carbide is promoted to be converted into dispersion carbide, and then hot forging is performed, wherein the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃. The samples No.8 to No.10 all had significantly better crack initiation tendencies than the M2 control. Or heating the smelted solidification sample to 1180-1230 ℃, preserving heat for 0.5-2 hours, quenching, reheating the sample, and then performing hot forging, wherein the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃. The crack initiation tendencies of the samples No. 8-No. 10 were also significantly better than the M2 control.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A manufacturing method for obtaining dispersed carbide in a medium-entropy high-speed steel structure is characterized by comprising the following steps: quenching the medium-entropy high-speed steel at 1180-1230 ℃, and then tempering for 2-3 times at 480-520 ℃, wherein the final heat treatment structure of the medium-entropy high-speed steel is hard carbide dispersed on a martensite matrix.
2. The manufacturing method for obtaining the dispersed carbide in the medium-entropy high-speed steel structure according to claim 1, wherein the heat preservation time is 0.5-2 hours during quenching treatment; and during tempering, the heat preservation time is 1-2 hours.
3. A manufacturing method for obtaining dispersed carbide in a medium-entropy high-speed steel structure is characterized by comprising the following steps: carrying out hot forging treatment on the medium-entropy high-speed steel subjected to quenching treatment in a temperature range of 1180-1230 ℃ at a temperature range of 850-1180 ℃ to obtain better crack initiation resistance;
or heating the smelted sample to 1180-1230 ℃ before hot forging, preserving the temperature for 0.5-2 hours, and then carrying out hot forging treatment at 1180-850 ℃ to obtain better crack initiation resistance.
4. The method for producing the dispersion carbide in the medium-entropy high-speed steel structure according to claim 3, wherein the initial forging temperature is 1100-1180 ℃, and the final forging temperature is 850-1050 ℃.
5. The manufacturing method for obtaining the dispersion carbides in the medium-entropy high-speed steel structure according to any one of claims 1 to 4, wherein the medium-entropy high-speed steel comprises the following components in percentage by weight: 0.7 to 1.5% of C, 5 to 8% of W, and 3 to 6% of Mo.
6. The method for manufacturing the dispersion carbides in the medium-entropy high-speed steel structure according to any one of claims 1 to 4, wherein the components of the medium-entropy high-speed steel are added with Cr, V, Co, Ni, Al and Cu alloy elements so as to adjust the entropy value of the alloy components to be between 1.0R and 1.2R, the weight percentage of the alloy elements is between 0.1 and 4 percent, and the weight percentage of the balance Fe element is controlled to be between 71 and 78 percent.
7. The manufacturing method for obtaining the dispersion carbides in the medium-entropy high-speed steel structure according to claim 6, wherein the medium-entropy high-speed steel further comprises Si, Mn, P and S alloy elements, and the weight percentages of the alloy elements are as follows: si < 0.5%, Mn < 1.0%, S < 0.05%, P < 0.05%.
8. The manufacturing method for obtaining the dispersion carbides in the medium-entropy high-speed steel structure is characterized in that the medium-entropy high-speed steel is prepared by a fusion casting, smelting or spray forming method.
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