CN113122763B - Preparation method of high-strength high-toughness high-entropy alloy - Google Patents
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Abstract
The invention discloses a preparation method of a high-strength high-toughness high-entropy alloy, and relates to the technical field of alloy material production; the method comprises the following specific steps: preparing high-entropy alloy powder of 27-30 atomic percent of Mn, 8-12 atomic percent of Co, 8-12 atomic percent of Cr and 0.4-1.3 atomic percent of C, and the balance being Fe; performing ball milling treatment on the high-entropy alloy powder, then prepressing under the pressure of 300-500 MPa for 200-300 s to obtain a prepressing block of the high-entropy alloy; vacuum annealing the prepressing block, then performing vacuum hot-pressing sintering, and then performing cold rolling deformation; carrying out constraint carbon distribution treatment on the cold-rolled and deformed high-entropy alloy sheet at 400-550 ℃ to diffuse free carbon elements; the non-equiatomic FeMnCoCrC high-entropy alloy containing C prepared by the method has excellent strength and plasticity combination, and simultaneously solves the problems of uneven components and unstable structure of the high-entropy alloy prepared by the traditional process.
Description
Technical Field
The invention belongs to the technical field of alloy material production, and particularly relates to a preparation method of a high-strength high-toughness high-entropy alloy.
Background
The high-entropy alloy is originally thought to be composed of five or more main elements in equal atomic ratio or near equal atomic ratio, and later, with further research, the definition is expanded to non-equal atomic ratio alloy and the structure and the performance of the high-entropy alloy can be adjusted by adding some trace elements, and the content of the trace elements is not more than 5 percent generally. High entropy alloys, because of their high entropy of mixing, inhibit the formation of intermetallic compounds, and thus the alloys generally tend to form solid solution phases of simple FCC, BCC and HCP crystal structures, which cause the high entropy alloys to exhibit some unique physical and chemical properties. In some cases, the addition of elements can lead to the formation of intermetallic phases or amorphous phases in the high-entropy alloy, which is both detrimental to the beneficial aspects of the alloy and also depends on the particular conditions of use. At present, researchers at home and abroad have made some progress on the research of high-entropy alloys, and mainly focus on the research of microstructures and properties of AlCoCrCuFeNi series, CoCrFeMnNi series and WNbMoTaV series alloys.
The development of metal materials with both high strength and high plasticity has been the focus of research, and many strengthening methods such as solid solution strengthening and precipitation strengthening can improve the strength of the materials, but the ductility and toughness are sacrificed correspondingly. In conventional metal materials, the twin induced plasticity (TWIP) and transformation induced plasticity (TRIP) effects solve this problem well. The TWIP effect is that deformation twins are induced when the material is deformed under the action of an external force, so that the material can obtain high elongation while maintaining high strength. The TWIP effect is affected by the stacking fault energy of the material, resulting in the material changing from the original dislocation slip mechanism to the second deformation mechanism, i.e. twinning deformation, during the deformation process. Therefore, the TWIP effect can promote the deformation mechanism of the alloy to change, and further improve the mechanical property of the alloy. In recent years, much research on high-entropy alloys has been focused on developing novel high-entropy alloy components, and attempts have been made to introduce the TWIP effect into high-entropy alloys, thereby obtaining high-entropy alloys having high strength and plasticity.
In the high-entropy alloy reported at present, FeMnCoCr has excellent mechanical properties, and the FeMnCoCr high-entropy alloy is a novel alloy obtained by changing the components of a classical CoCrFeMnNi alloy. According to the research of the existing high-entropy alloy, the sigma phase is precipitated when Cr and Ni or Co exist simultaneously under some systems.
The patent CN111235454A discloses an AlCoCrFeMn high-entropy alloy with unequal atomic ratio and a preparation method thereof, wherein the atomic ratio of the alloy is Al: Co: Cr: Fe: Mn = (0.3-0.7): 2:1:1:1, arc melting is carried out under the protection of inert gas, copper mold suction casting is carried out to obtain an alloy ingot, and then solid solution, water quenching, rolling deformation and vacuum annealing are carried out to obtain the AlCoCrFeMn high-entropy alloy with unequal atomic ratio. The patent CN111172446A discloses a high-entropy alloy with high corrosion resistance and unequal atomic ratio and a preparation method thereof, wherein the alloy comprises the following components of 34-36 at% of Fe, 9-11 at% of Mn, 19-21 at% of Cr, and 34-36% of Ni. And (3) repeatedly carrying out vacuum arc melting in Ar atmosphere, carrying out homogenization treatment on the cast ingot, carrying out water quenching, carrying out hot forging at 800-1000 ℃, carrying out heat preservation for 1-5 h after the completion of the hot forging, carrying out recrystallization annealing, and finally carrying out water quenching to normal temperature to obtain the high-entropy alloy with non-equal atomic ratio. The corrosion resistance of the alloy in 3.5 wt% sodium chloride water solution and 0.5mol/L sulfuric acid water solution is better than that of 304 stainless steel (cold rolled annealed state).
The above patents all obtain the non-isoatomic high-entropy alloy with ideal performance by adjusting the components of the high-entropy alloy. However, the alloy prepared by the traditional arc melting process generally needs to be repeatedly melted for many times and cast ingots are subjected to long-time high-temperature homogenization annealing to eliminate the component segregation generated in the solidification process, so that the components and the structure tend to be uniform. Therefore, the high-entropy alloy prepared by the arc melting method has defects, so that the alloy performance is not high, the preparation process is complicated, the cost is high, and the application range of the high-entropy alloy is limited.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a preparation method of a high-strength high-toughness high-entropy alloy. The non-equiatomic FeMnCoCrC high-entropy alloy containing C prepared by the method has excellent combination of strength and plasticity, and simultaneously solves the problems of uneven components, unstable structure and the like of the high-entropy alloy prepared by the traditional process.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a high-strength high-toughness high-entropy alloy comprises the following steps:
a) the high-entropy alloy powder is prepared from 27-30 atomic percent of Mn, 8-12 atomic percent of Co, 8-12 atomic percent of Cr, 0.4-1.3 atomic percent of C and the balance of Fe.
b) And performing ball milling treatment on the high-entropy alloy powder to mechanically alloy the high-entropy alloy powder to obtain the high-entropy alloy powder.
c) And prepressing the high-entropy alloy powder at the pressure of 300-500 MPa, and maintaining the pressure for 200-300 s to obtain a prepressing block of the high-entropy alloy.
d) And (4) annealing the prepressed block in vacuum, and then performing vacuum hot-pressing sintering to obtain the high-entropy alloy.
e) And carrying out cold rolling deformation on the high-entropy alloy.
f) And (3) carrying out constraint carbon distribution treatment on the high-entropy alloy sheet subjected to cold rolling deformation at 400-550 ℃ to diffuse free carbon elements, so as to stabilize the microstructure.
Preferably, in the step b, the high-entropy alloy powder and n-heptane accounting for 10% of the total mass of the high-entropy alloy powder are put into a ball milling tank and then ball milled after being sealed.
Preferably, stainless steel balls and stainless steel tanks are used for ball milling treatment, the ball-material ratio is 15-20: 1, the rotating speed is 250-300 r/min, and the ball milling time is 30-40 h.
Preferably, the powder after ball milling treatment is put into a vacuum drying oven for drying at the temperature of 100 ℃, and the temperature is kept for 20h to remove the n-heptane.
Preferably, in the step d, the temperature of the vacuum annealing is 400-600 ℃, and the annealing is carried out for 1-2 hours.
Preferably, in the step d, the vacuum hot-pressing sintering is carried out, wherein the vacuum degree is 40Pa, the sintering temperature is 950-1050 ℃, the sintering pressure is 40-50 MPa, the heating rate is 10 ℃/min, and the heat preservation time is 1-1.5 h.
Preferably, in step e, the cold rolling deformation has a deformation amount of 60%.
Preferably, in the step e, the high-entropy alloy sheet with the thickness of 1-2mm is manufactured after cold rolling deformation treatment.
Preferably, in the step f, the high-entropy alloy sheet after cold rolling deformation is placed into a Gleeble thermal simulator for constraint carbon distribution treatment.
According to the non-equiatomic FeMnCoCrC high-entropy alloy prepared by the invention, in order to avoid the precipitation of a sigma phase, Ni is not added into the alloy, meanwhile, the contents of Co and Cr are reduced, the generation of a Cr-rich intermetallic compound is avoided, and the deterioration of the alloy performance caused by the formation of a hard and brittle sigma phase with Co and Cr is avoided. The research of the invention finds that the stacking fault energy of an alloy system can be changed by adjusting the content of Mn, so that transformation induced plasticity (TRIP) or twin induced plasticity (TWIP) is triggered in the deformation process, and the toughness of the alloy is improved. Therefore, in order to trigger the TWIP effect, the content of Mn in the alloy is increased, and the stacking fault energy is improved. The addition of interstitial C in the alloy can also improve the stacking fault energy, increase the phase stability and trigger the TWIP effect in subsequent deformation, and secondly, C can cause solid solution strengthening and can form nano carbide to play an Orowan strengthening role.
The content of Co and Cr is reduced, and the generation of Cr-rich intermetallic compounds is avoided. Increasing the Mn content increases the stacking fault energy and strongly promotes the TWIP effect. The addition of the C element improves the phase stability of the high-entropy alloy, increases the stacking fault energy, promotes the generation of the TWIP effect, simultaneously generates solid solution strengthening of interstitial C atoms, and forms nano-scale carbide to play a role in dispersion strengthening. The carbide is distributed in the crystal boundary to play a pinning role on the crystal boundary and prevent the crystal grain from growing.
The invention adopts the methods of mechanical alloying and vacuum hot-pressing sintering to prepare the high-entropy alloy, the high-entropy alloy can obtain nanoscale alloy powder by the preparation of the mechanical alloying method, the high-temperature melting and solidification processes of the traditional smelting are avoided, the high-melting-point metal can be alloyed at low temperature, the uniform high-entropy alloy powder with a fine structure is prepared, and the sintered high-entropy alloy has uniform components, less segregation, stable microstructure and smaller internal stress. The ball milling tank is added with n-heptane as a control agent to prevent oxidation and cold welding of the powder. The high-entropy alloy powder is pre-pressed and annealed before sintering, so that the density of the alloy is improved, the defects are reduced, and the high-entropy alloy with excellent performance is obtained.
The invention rolls the sintered high-entropy alloy and performs the constraint carbon distribution treatment to diffuse the free carbon element, thereby stabilizing the microstructure and being beneficial to improving the toughness of the alloy.
Compared with the prior art, the invention has the following beneficial effects:
1. the non-equiatomic FeMnCoCrC high-entropy alloy avoids the generation of brittle intermetallic compounds by adjusting the content of each principal element, increases the fault energy of the alloy, stabilizes the phase structure, promotes the generation of twin induced plasticity (TWIP) effect, shows excellent strength and plastic cooperation, has tensile yield strength of over 956MPa, elongation of over 50 percent after fracture and high toughness.
2. The C element is added into the high-entropy alloy, so that the stability of an FCC phase is improved, and the twinning behavior can be promoted by increasing the stacking fault energy. Interstitial C atoms generate a solid solution strengthening effect, and simultaneously can form nano-scale carbide to play a role in dispersion strengthening, and nano-scale carbide particles are distributed in a crystal boundary after annealing to play a pinning effect on the crystal boundary and prevent the crystal grain from growing.
3. The high-entropy alloy prepared by adopting the mechanical alloying and vacuum hot-pressing sintering methods has the characteristics of fine microstructure, uniform components, stable structure and small internal stress, and the prepared high-entropy alloy does not need long-time high-temperature homogenizing annealing. The alloy is subjected to cold rolling and carbon distribution restraint treatment to obtain a recrystallized structure, and grains are fine and uniform and play a role in fine grain strengthening.
Drawings
FIG. 1 is a microstructure diagram of the FeMnCoCrC high-entropy alloy prepared by the method.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
Example 1
A high-entropy alloy with high strength and toughness is prepared fromThe following elementary metals in atomic percentage: fe49.5%, Mn30%, Co10%, Cr10%, C0.5%, expressed as Fe49.5Mn30Co10Cr10C0.5。
The first step is as follows: the high-entropy alloy of the above components and n-heptane accounting for 10% of the total mass of the powder were placed in a glove box filled with Ar gas, and the glove box was sealed after being placed in a ball mill jar.
The second step is that: and (3) putting the sealed ball milling tank into a high-energy planetary ball mill for mechanical alloying. Stainless steel balls and stainless steel tanks are used, the ball-material ratio is 15:1, the rotating speed is 300r/min, and the ball milling time is 32 h.
The third step: and (3) putting the powder obtained in the second step into a vacuum drying oven for drying at the temperature of 100 ℃, and keeping the temperature for 20 hours to remove n-heptane, thereby obtaining the high-entropy alloy powder.
The fourth step: and putting the high-entropy alloy powder into a die for prepressing under the pressure of 300MPa for 240s to obtain a prepressing block of the high-entropy alloy.
The fifth step: putting the prebuckled block into a vacuum tube furnace for vacuum annealing at the temperature of 600 ℃ for 1 h.
And a sixth step: and putting the annealed precast block into a high-strength graphite die, carrying out vacuum hot-pressing sintering, wherein the vacuum degree is 40Pa, the sintering temperature is 1050 ℃, the sintering pressure is 40MPa, the heating rate is 10 ℃/min, carrying out heat preservation for 1h, and then carrying out furnace cooling on the unloading pressure to room temperature to obtain the cylindrical high-entropy alloy with the size of phi 20mm multiplied by 5 mm.
The seventh step: and (3) placing the obtained high-entropy alloy into a rolling mill for cold rolling, and rolling into a sheet with the thickness of 2mm, wherein the deformation is 60%, so as to obtain the high-entropy alloy after rolling deformation.
Eighth step: and (3) placing the rolled and deformed high-entropy alloy sheet into a Gleeble thermal simulator for constraint carbon distribution treatment, clamping the sheet on a chuck, and carrying out constraint carbon distribution within the range of 400-420 ℃ to diffuse free carbon elements, thereby stabilizing the microstructure. The high-toughness non-equiatomic FeMnCoCrC high-entropy alloy is obtained, and the microstructure of the high-toughness non-equiatomic FeMnCoCrC high-entropy alloy is shown in figure 1.
Example 2
High-entropy alloy with high strength and toughnessThe gold comprises the following metal simple substances in atomic percentage: fe49.6%, Mn27.4%, Co11.6%, Cr10.8%, C0.6%, which can be expressed as Fe49.6Mn27.4Co11.6Cr10.8C0.6。
The first step is as follows: high-entropy alloy powder of the above components and n-heptane accounting for 10% of the total mass of the powder were placed in a glove box filled with Ar gas, and the glove box was sealed after being placed in a ball mill pot.
The second step is that: and (3) putting the sealed ball milling tank into a high-energy planetary ball mill for mechanical alloying. Stainless steel balls and stainless steel tanks are used, the ball-material ratio is 20:1, the rotating speed is 280r/min, and the ball milling time is 34 h.
The third step: and (3) putting the powder obtained in the second step into a vacuum drying oven for drying at the temperature of 100 ℃, and keeping the temperature for 20 hours to remove n-heptane, thereby obtaining the high-entropy alloy powder.
The fourth step: and putting the high-entropy alloy powder into a die for prepressing under the pressure of 400MPa for 200s to obtain a prepressing block of the high-entropy alloy.
The fifth step: putting the prebuckled block into a vacuum tube furnace for vacuum annealing at the temperature of 500 ℃ for 1.5 h.
And a sixth step: and putting the annealed precast block into a high-strength graphite mold, carrying out vacuum hot-pressing sintering, wherein the vacuum degree is 40Pa, the sintering temperature is 1000 ℃, the sintering pressure is 50MPa, the heating rate is 10 ℃/min, keeping the temperature for 1.5h, and then unloading the pressure to cool to the room temperature along with the furnace to obtain the cylindrical high-entropy alloy with the size of phi 20mm multiplied by 5 mm.
The seventh step: and (3) placing the obtained high-entropy alloy into a rolling mill for cold rolling, and rolling into a sheet with the thickness of 2mm, wherein the deformation is 60%, so as to obtain the high-entropy alloy after rolling deformation.
Eighth step: and (3) placing the rolled and deformed high-entropy alloy sheet into a Gleeble thermal simulator for constraint carbon distribution treatment, clamping the sheet on a chuck, and carrying out constraint carbon distribution within the range of 450-460 ℃ to diffuse free carbon elements, thereby stabilizing the microstructure. Obtaining the high-entropy non-equiatomic FeMnCoCrC alloy with high strength and toughness.
Example 3
High toughness of high toughnessThe entropy alloy comprises the following metal simple substances in atomic percentage: fe49.7%, Mn29.6%, Co9.6%, Cr10.2%, C0.9%, can be expressed as Fe49.7Mn29.6Co9.6Cr10.2C0.9。
The first step is as follows: high-entropy alloy powder of the above components and n-heptane accounting for 10% of the total mass of the powder were placed in a glove box filled with Ar gas, and the glove box was sealed after being placed in a ball mill pot.
The second step is that: and (3) putting the sealed ball milling tank into a high-energy planetary ball mill for mechanical alloying. Stainless steel balls and stainless steel tanks are used, the ball-material ratio is 20:1, the rotating speed is 300r/min, and the ball milling time is 35 h.
The third step: and (3) putting the powder obtained in the second step into a vacuum drying oven for drying at the temperature of 100 ℃, and keeping the temperature for 20 hours to remove n-heptane, thereby obtaining the high-entropy alloy powder.
The fourth step: and putting the high-entropy alloy powder into a die for prepressing under the pressure of 500MPa for 300s to obtain a prepressing block of the high-entropy alloy.
The fifth step: putting the prebuckled block into a vacuum tube furnace for vacuum annealing at the temperature of 600 ℃ for 2 hours.
And a sixth step: and putting the annealed precast block into a high-strength graphite mold, carrying out vacuum hot-pressing sintering, wherein the vacuum degree is 40Pa, the sintering temperature is 900 ℃, the sintering pressure is 50MPa, the heating rate is 10 ℃/min, keeping the temperature for 1.5h, and then unloading the pressure to cool to the room temperature along with the furnace to obtain the cylindrical high-entropy alloy with the size of phi 20mm multiplied by 5 mm.
The seventh step: and (3) placing the obtained high-entropy alloy into a rolling mill for cold rolling, and rolling into a sheet with the thickness of 2mm, wherein the deformation is 60%, so as to obtain the high-entropy alloy after rolling deformation.
Eighth step: and (3) placing the rolled and deformed high-entropy alloy sheet into a Gleeble thermal simulator for constraint carbon distribution treatment, clamping the sheet on a chuck, and carrying out constraint carbon distribution within the range of 530-550 ℃ to diffuse free carbon elements, thereby stabilizing the microstructure. Obtaining the high-entropy non-equiatomic FeMnCoCrC alloy with high strength and toughness.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of a high-strength high-toughness high-entropy alloy is characterized by comprising the following steps:
a) preparing high-entropy alloy powder of 30 atomic percent of Mn, 10 atomic percent of Co, 10 atomic percent of Cr and 0.5 atomic percent of C, and the balance being Fe;
b) performing ball milling treatment on the high-entropy alloy powder to mechanically alloy the high-entropy alloy powder to obtain high-entropy alloy powder;
c) prepressing the high-entropy alloy powder at the pressure of 300-500 MPa, and maintaining the pressure for 200-300 s to obtain a prepressing block of the high-entropy alloy;
d) vacuum annealing the prepressing block, and then performing vacuum hot-pressing sintering to obtain a high-entropy alloy;
e) carrying out cold rolling deformation on the high-entropy alloy; after cold rolling deformation treatment, manufacturing a high-entropy alloy sheet with the thickness of 1-2 mm;
f) placing the cold-rolled and deformed high-entropy alloy sheet into a Gleeble thermal simulator for constraint carbon distribution treatment; the temperature for the constrained carbon distribution treatment is 400-550 ℃, so that the free carbon element is diffused, and the aim is to stabilize the microstructure.
2. The preparation method of the high-strength high-toughness high-entropy alloy as claimed in claim 1, wherein in the step b, the high-entropy alloy powder and n-heptane accounting for 10% of the total mass of the high-entropy alloy powder are put into a ball milling tank and sealed for ball milling.
3. The preparation method of the high-strength high-toughness high-entropy alloy as claimed in claim 2, wherein stainless steel balls and a stainless steel tank are used for ball milling treatment, the ball-material ratio is 15-20: 1, the rotating speed is 250-300 r/min, and the ball milling time is 30-40 h.
4. The preparation method of the high-strength high-toughness high-entropy alloy according to claim 3, wherein the powder subjected to ball milling treatment is placed in a vacuum drying oven to be dried, the temperature is 100 ℃, and the temperature is kept for 20 hours to remove n-heptane.
5. The preparation method of the high-strength high-toughness high-entropy alloy as claimed in claim 1, wherein in the step d, the temperature of vacuum annealing is 400-600 ℃, and the annealing is carried out for 1-2 hours.
6. The preparation method of the high-strength high-toughness high-entropy alloy according to claim 1, wherein in the step d, the vacuum hot-pressing sintering is carried out, the vacuum degree is 40Pa, the sintering temperature is 950-1050 ℃, the sintering pressure is 40-50 MPa, the heating rate is 10 ℃/min, and the temperature is kept for 1-1.5 h.
7. The method for preparing the high-strength high-toughness high-entropy alloy as claimed in claim 1, wherein in the step e, the deformation amount of cold rolling deformation is 60%.
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| CN114085969B (en) * | 2021-11-15 | 2023-03-10 | 太原科技大学 | Preparation process of high-entropy alloy plate with heterogeneous laminated structure |
| CN114086142A (en) * | 2021-11-29 | 2022-02-25 | 亚芯半导体材料(江苏)有限公司 | High-entropy alloy rotary target and preparation method of cold spraying thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107829007A (en) * | 2017-10-26 | 2018-03-23 | 福建工程学院 | A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block |
| KR20190068916A (en) * | 2017-12-11 | 2019-06-19 | 한국기계연구원 | High entropy alloy and method for manufacturing the same |
| CN110284042A (en) * | 2019-08-05 | 2019-09-27 | 西安工业大学 | Superplasticity high-entropy alloy, plate and preparation method thereof |
| CN111519079A (en) * | 2020-04-15 | 2020-08-11 | 燕山大学 | CoCrNiCuFeMnAl high-entropy alloy and preparation method thereof |
| CN112376043A (en) * | 2020-10-26 | 2021-02-19 | 中北大学 | Method for preparing high-entropy alloy composite coating on surface of low-carbon steel |
-
2021
- 2021-04-14 CN CN202110401899.8A patent/CN113122763B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107829007A (en) * | 2017-10-26 | 2018-03-23 | 福建工程学院 | A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block |
| KR20190068916A (en) * | 2017-12-11 | 2019-06-19 | 한국기계연구원 | High entropy alloy and method for manufacturing the same |
| CN110284042A (en) * | 2019-08-05 | 2019-09-27 | 西安工业大学 | Superplasticity high-entropy alloy, plate and preparation method thereof |
| CN111519079A (en) * | 2020-04-15 | 2020-08-11 | 燕山大学 | CoCrNiCuFeMnAl high-entropy alloy and preparation method thereof |
| CN112376043A (en) * | 2020-10-26 | 2021-02-19 | 中北大学 | Method for preparing high-entropy alloy composite coating on surface of low-carbon steel |
Non-Patent Citations (1)
| Title |
|---|
| "C/Mo元素合金化Fe50Mn30Co10Cr10系高熵合金TWIP/TRIP效应研究";赵雪柔;《万方数据知识服务平台》;20201119;第12-14页 * |
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