CN107829007B - A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block - Google Patents
A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 239000000843 powder Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 239000011651 chromium Substances 0.000 claims abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 6
- 239000010941 cobalt Substances 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 239000011572 manganese Substances 0.000 claims abstract description 3
- 239000004615 ingredient Substances 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 229910000604 Ferrochrome Inorganic materials 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 238000004663 powder metallurgy Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910001199 N alloy Inorganic materials 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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Abstract
A kind of powder metallurgy high-entropy alloy, atomic percentage are as follows: iron: 5~35%;Cobalt: 5~35%;Chromium: 5~35%;Nickel: 5~35%;Manganese: 5~35%;Nitrogen: 0.1~5%.Preparation method includes: the preparation of high-entropy alloy powder, and high-entropy alloy powder is prepared, and is put into ball mill after mixing and carries out ball milling, and the granule-morphology of high-entropy alloy powder is even-grained spherical or almost spherical after ball milling, and particle size range is 20~30 μm;High-entropy alloy powder after ball milling is placed in a high-strength graphite mold and carries out vacuum heating-press sintering, last furnace cooling.The present invention obtains the tiny high-entropy alloy of even tissue, crystal grain using the method for powder metallurgy, to improve the performance of alloy.
Description
[technical field]
The invention belongs to field of material technology, in particular to a kind of high-entropy alloy and powder metallurgic method to prepare high-entropy alloy block
The method of body.
[background technique]
Traditional alloy based on one or two kinds of elements, and high-entropy alloy be using five kinds or five kinds or more metals as
Essential element, the molar fraction of every kind of element have simple solid solution phase structure, such as face-centered cubic between 5% to 35%
Structure (FCC) phase, body-centered cubic structure (BCC) phase.Compared with conventional alloys, high-entropy alloy has more pivot effects, main table
Be now the high entropy effect in terms of thermodynamics, the slow effect of diffusion in terms of dynamics, the tight distortion of lattice effect of configuration aspects with
And the Cocktail effect of aspect of performance.By reasonable ingredient and technological design, high-entropy alloy can show conventional alloys without
The superior comprehensive performance of method analogy, such as high intensity and hardness, excellent wearability, corrosion resistance, high temperature oxidation resistance are good
Good thermal stability.
FeCoCrNiMn high-entropy alloy is typical high-entropy alloy, has good plasticity and toughness, but its intensity is low.It can
To improve intensity by the method for adding interstitial atom, but nitrogenous FeCoCrNiMn high entropy is prepared using common method of smelting
Alloy, the easy gasification volatilization of nitrogen, additional amount are few, and control is difficult, while being easy to appear component segregation, the compound of formation
Grain is coarse.It can obtain that crystal grain is tiny, ingredient is uniformly organized using high-entropy alloy prepared by powder metallurgy process, to make to close
Fitting has higher intensity and hardness and wearability.
Existing high-entropy alloy mostly uses smelting process to prepare greatly, and there are component segregation, organizational coarseness, contractings for acquired cast alloy
The disadvantages of pine, cavity and product size limit.
[summary of the invention]
The first technical problem to be solved by the present invention is to provide the high-entropy alloy of Nitrogen element FeCoCrNiMn a kind of
Powder.
The present invention, which adopts the following technical scheme that, solves one of above-mentioned technical problem:
A kind of high-entropy alloy powder, atomic percentage are as follows: iron: 5~35%;Cobalt: 5~35%;Chromium: 5~35%;Nickel: 5
~35%;Manganese: 5~35%;Nitrogen: 0.1~5%.
The second technical problem to be solved by the present invention is that providing three kinds of powder metallurgy methods prepares Nitrogen element
The method of FeCoCrNiMn high-entropy alloy block.
Technical solution one:
A kind of method that powder metallurgic method prepares high-entropy alloy block, includes the following steps:
Step 1: the preparation of high-entropy alloy powder
Alloy powder ingredient is carried out by the alloying component proportion of design, wherein nitrogen is mixed in the form of nitrided ferro-chromium,
The high-entropy alloy powder of the claims 1 is prepared, ball mill is put into after mixing and carries out ball milling, milling parameters
Are as follows: ratio of grinding media to material is 10~15:1, and rotational speed of ball-mill is 230~280rpm, and Ball-milling Time is 40~50h;High-entropy alloy powder after ball milling
The granule-morphology at end is even-grained spherical or almost spherical, and particle size range is 20~30 μm;
Step 2: the preparation of high-entropy alloy block:
High-entropy alloy powder after ball milling is placed in a high-strength graphite mold and carries out vacuum heating-press sintering, agglomerant
Skill parameter are as follows: the rate of heat addition is 5~10 DEG C/min, and sintering temperature is 850~950 DEG C, and soaking time is 0.5~2h, constant pressure
Power is 30~60MPa, last furnace cooling.
Technical solution two:
A kind of method that powder metallurgic method prepares high-entropy alloy block, includes the following steps:
Step 1: the preparation of high-entropy alloy powder
Alloy powder ingredient is carried out by the alloying component proportion of design, wherein nitrogen is mixed in the form of nitrided ferro-chromium,
The high-entropy alloy powder of the claims 1 is prepared, ball mill is put into after mixing and carries out ball milling, milling parameters
Are as follows: ratio of grinding media to material is 10~15:1, and rotational speed of ball-mill is 230~280rpm, and Ball-milling Time is 40~50h;High-entropy alloy powder after ball milling
The granule-morphology at end is even-grained spherical or almost spherical, and particle size range is 20~30 μm;
Step 2: the preparation of high-entropy alloy block:
High-entropy alloy powder after ball milling is placed in a high-strength graphite mold and carries out discharge plasma sintering, agglomerant
Skill parameter are as follows: the rate of heat addition is 70~80 DEG C/min, and sintering temperature is 850~950 DEG C, and soaking time is 5~10min, constant
Pressure is 30~50Mpa, last furnace cooling.
Technical solution three:
A kind of method that powder metallurgic method prepares high-entropy alloy block, includes the following steps:
Step 1: the preparation of high-entropy alloy powder
Alloy powder ingredient is carried out by the alloying component proportion of design, wherein nitrogen is mixed in the form of nitrided ferro-chromium,
The high-entropy alloy powder of the claims 1 is prepared, ball mill is put into after mixing and carries out ball milling, milling parameters
Are as follows: ratio of grinding media to material is 10~15:1, and rotational speed of ball-mill is 230~280rpm, and Ball-milling Time is 40~50h;High-entropy alloy powder after ball milling
The granule-morphology at end is even-grained spherical or almost spherical, and particle size range is 20~30 μm;
Step 2: the preparation of high-entropy alloy block:
High-entropy alloy powder after ball milling is placed in progress vacuum HIP sintering in a high-strength graphite mold, sintering
Technological parameter are as follows: the rate of heat addition is 5~10 DEG C/min, and sintering temperature is 850~950 DEG C, and soaking time is 0.5~1h, constant
Pressure is 30~60MPa, last furnace cooling.
The present invention has the advantages that the present invention prepares the conjunction of Nitrogen element FeCoCrNiMn high entropy using the method for powder metallurgy
Gold obtains the tiny high-entropy alloy of even tissue, crystal grain using the method for powder metallurgy, to improve the performance of alloy.Using
Powder metallurgic method can prepare that crystal grain is tiny, the uniform high-intensitive large scale high-entropy alloy block with high rigidity of ingredient,
Middle mechanical alloying is more advantageous to form high-entropy alloy solid solution, is also easier to prepare uniform nanocrystalline high-entropy alloy powder
End.
[Detailed description of the invention]
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the alloy powder figure after ball milling of the invention.
Fig. 2 is the XRD spectra of the sintered block high-entropy alloy of first embodiment of the invention.
Fig. 3 is the high-entropy alloy microstructure morphology of first embodiment of the invention.
Fig. 4 is the high-entropy alloy room temperature Compressive Mechanical Properties figure of first embodiment of the invention.
[specific embodiment]
First embodiment:
Firstly, proportion alloy powder raw material (molar fraction): 19.2% iron, 19.2% cobalt, 19.2% chromium, 19.2% nickel,
19.2% manganese, 4% nitrogen carry out ball milling by ball milling design technology parameter after mixing, alloy powder such as Fig. 1 after ball milling,
Particle shape looks are even-grained spherical or almost spherical, and particle size range is 20~30 μm.
Vacuum heating-press sintering is carried out secondly, high-entropy alloy powder after ball milling is placed in a high-strength graphite mold, is burnt
Tie technological parameter are as follows: the rate of heat addition is 8 DEG C/min, and sintering temperature is 900 DEG C, soaking time 1h, constant pressure 50Mpa.
The XRD spectra of sintered block high-entropy alloy as shown in Fig. 2, microstructure morphology (SEM) as shown in figure 3, aobvious
Microhardness is 485HV, room temperature Compressive Mechanical Properties such as Fig. 4, and wherein compressive strength is 2145MPa, plasticity 14%.
Finally, furnace cooling.
Second embodiment:
Firstly, proportion alloy powder raw material (molar fraction): 19.2% iron, 19.2% cobalt, 19.2% chromium, 19.2% nickel,
19.2% manganese, 4% nitrogen carry out ball milling by ball milling design technology parameter after mixing, alloy powder such as Fig. 1 after ball milling,
Particle shape looks are even-grained spherical or almost spherical, and particle size range is 20~30 μm.
Discharge plasma sintering is carried out secondly, high-entropy alloy powder after ball milling is placed in a high-strength graphite mold,
Sintering process parameter are as follows: the rate of heat addition is 70 DEG C/min, and sintering temperature is 900 DEG C, soaking time 10min, and constant pressure is
50Mpa。
Finally, furnace cooling.
3rd embodiment:
Firstly, proportion alloy powder raw material (molar fraction): 19.2% iron, 19.2% cobalt, 19.2% chromium, 19.2% nickel,
19.2% manganese, 4% nitrogen carry out ball milling by ball milling design technology parameter after mixing, alloy powder such as Fig. 1 after ball milling,
Particle shape looks are even-grained spherical or almost spherical, and particle size range is 20~30 μm.
High-entropy alloy powder after ball milling is placed in progress vacuum HIP sintering in a high-strength graphite mold, sintering
Technological parameter are as follows: the rate of heat addition is 8 DEG C/min, and sintering temperature is 900 DEG C, soaking time 1h, constant pressure 50MPa.
Finally, furnace cooling.
The present invention prepares Nitrogen element FeCoCrNiMn high-entropy alloy using the method for powder metallurgy, utilizes powder metallurgy
Method obtains the tiny high-entropy alloy of even tissue, crystal grain, to improve the performance of alloy.It can be prepared using powder metallurgic method
Crystal grain is tiny out, the uniform high-intensitive large scale high-entropy alloy block with high rigidity of ingredient, and wherein mechanical alloying is more advantageous
In forming high-entropy alloy solid solution, it is also easier to prepare uniform nanocrystalline high-entropy alloy powder.
The foregoing is merely preferable implementation use-cases of the invention, are not intended to limit the scope of the present invention.It is all
Within the spirit and principles in the present invention, made any modification, equivalent replacement and improvement etc., should be included in of the invention
Within protection scope.
Claims (1)
1. a kind of method that powder metallurgic method prepares high-entropy alloy block, characterized by the following steps:
Step 1: the preparation of high-entropy alloy powder
Alloy powder ingredient is carried out by the alloying component proportion of design, wherein nitrogen is mixed in the form of nitrided ferro-chromium, will be former
Sub- percentage are as follows: iron: 5~35%;Cobalt: 5~35%;Chromium: 5~35%;Nickel: 5~35%;Manganese: 5~35%;Nitrogen: 0.1~5%
High-entropy alloy powder prepare, be put into after mixing ball mill carry out ball milling, milling parameters are as follows: ratio of grinding media to material be 10~
15:1, rotational speed of ball-mill are 230~280rpm, and Ball-milling Time is 40~50h;The granule-morphology of high-entropy alloy powder is grain after ball milling
The uniform spherical or almost spherical of degree, particle size range are 20~30 μm;
Step 2: the preparation of high-entropy alloy block:
High-entropy alloy powder after ball milling is placed in a high-strength graphite mold and carries out vacuum heating-press sintering, sintering process ginseng
Number are as follows: the rate of heat addition is 5~10 DEG C/min, and sintering temperature is 850~950 DEG C, and soaking time is 0.5~2h, and constant pressure is
30~60MPa, last furnace cooling.
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CN110548869B (en) * | 2018-06-04 | 2022-03-04 | 中南大学 | Nitrogen-containing high-entropy alloy composite material and preparation method thereof |
CN108866417B (en) * | 2018-06-07 | 2020-02-18 | 东南大学 | High-strength corrosion-resistant medium-entropy alloy and preparation method thereof |
CN109867525A (en) * | 2019-01-28 | 2019-06-11 | 广东工业大学 | A kind of high-entropy alloy boride ceramics and its preparation method and application |
CN110219002B (en) * | 2019-07-02 | 2021-07-13 | 爱柯迪股份有限公司 | High-entropy alloy composite coating material for repairing die and die repairing method |
CN110218929A (en) * | 2019-07-08 | 2019-09-10 | 广西大学 | A kind of method of Strengthening and Toughening FeMnNiCoCr high-entropy alloy |
CN111636025A (en) * | 2020-04-28 | 2020-09-08 | 苏州鑫旭合智能科技有限公司 | High-entropy alloy containing Ti and C and preparation method thereof |
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CN113351866B (en) * | 2021-04-25 | 2023-03-28 | 西安交通大学 | Powder metallurgy preparation method of oxide-reinforced high-entropy alloy |
CN113755736A (en) * | 2021-08-05 | 2021-12-07 | 西安交通大学 | High-corrosion-resistance non-equimolar high-entropy alloy and preparation method thereof |
CN113798495B (en) * | 2021-08-12 | 2023-07-18 | 西安理工大学 | High-entropy alloy sintering molding process with equivalent conversion of double elements |
CN114210984A (en) * | 2021-12-18 | 2022-03-22 | 金川集团股份有限公司 | Method for preparing high-entropy alloy powder by mechanical alloying |
CN115011827B (en) * | 2022-05-11 | 2024-05-14 | 北京工业大学 | NbMoTaWCu high-entropy alloy and preparation method thereof |
CN115874104B (en) * | 2022-11-25 | 2024-05-03 | 常州大学 | Medical degradable ZnFeMn medium entropy alloy and preparation method and application thereof |
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