CN105543621A - Endogenous nano ceramic reinforcement high-entropy alloy composite material and preparing method - Google Patents
Endogenous nano ceramic reinforcement high-entropy alloy composite material and preparing method Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 40
- 239000000919 ceramic Substances 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 10
- 230000002787 reinforcement Effects 0.000 title abstract 3
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims description 35
- 239000000843 powder Substances 0.000 claims description 21
- 238000005245 sintering Methods 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001238 wet grinding Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 7
- 238000005275 alloying Methods 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 6
- 238000009837 dry grinding Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 4
- 238000000713 high-energy ball milling Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000006104 solid solution Substances 0.000 abstract 2
- 239000000463 material Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910017060 Fe Cr Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- C22C1/00—Making non-ferrous alloys
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Abstract
The invention discloses an endogenous nano ceramic reinforcement high-entropy alloy composite material and a preparing method. High-entropy alloy particles serve as a base body phase, and meanwhile, in the high-energy ball milling process, mechanical alloying energy promotes the in-situ reaction to generate nano ceramic TiC, and an endogenous nano ceramic phase is segregated on the solid solution grain boundary, and ceramic phase reinforcement is generated; meanwhile, a flexible face-centered cubic solid solution is extruded to form a deformation twin, and therefore strength and plasticity combination of the high-entropy alloy composite material is achieved; and the high-strength high-toughness high-entropy alloy composite material is prepared, the excellent strength and the excellent strength are kept, and meanwhile, the plasticity of the composite material is improved.
Description
Technical field
The invention belongs to metal-base composites technical field, be specifically related to a kind of high-entropy alloy matrix material and preparation method thereof.
Background technology
Block high-entropy alloy (HEA) has a series of excellent mechanical performances being different from traditional crystal alloy such as high strength, high rigidity, low Young's modulus and large elastic strain limit, makes it be considered to the structured material of great potential.But high fragility makes HEA material when not having the viscous deformation of obvious room temperature macroscopic view, in the mode of sudden failure, calamitous fracture occurs; The processing to material of high fragility, high rigidity brings extreme difficulties.These all seriously govern HEA as the large-scale application of advanced configuration material in engineering.Therefore, brittleness at room temperature, processing difficulties problem have developed into the important bottleneck of HEA materials application.
For the problem of the brittleness at room temperature and processing difficulties that improve HEA material, investigators are by adding different metallic elements, and adopt arc cast to prepare the block materials of dendritic segregation, this is wherein to add Cu successful, and its compression plastic strain reaches within 8%.Subsequently, the people such as Zhang Yong prepare the high entropy alloy material with columanar structure by directional solidification technique, and its compressive ductility increases; Wang Yanping etc. adopt arc cast to prepare the CrFeCoNiCuAl high-entropy alloy-base composite material (HEAMCs) of interior raw 10vol.%TiC particle reinforce, and TiC becomes particulate state to be evenly distributed on matrix, and size is about several micron.The compressive strength of CrFeCoNiCuTi-TiC matrix material and hardness can reach 2040MPa and 746HV respectively, compression plasticity about 12%.But the acquisition of the plasticity of above-mentioned high entropy alloy material, be not considerably reduce intensity be exactly raising plasticity in and not obvious.
Summary of the invention
The object of the present invention is to provide a kind of high-entropy alloy matrix material and preparation method, while its excellent in strength of maintenance and hardness, improve the plasticity of matrix material.
High-entropy alloy matrix material of the present invention, using high-entropy alloy particle as matrix phase, meanwhile, in Process During High Energy Ball Milling, mechanical alloying energy promotes that reaction in－situ generates nano ceramics TiC:Ti+C
tiC, makes interior raw nano ceramics phase segregation at sosoloid grain boundaries, produces ceramic phase and strengthens, extruding is caused to the face-centered cubic sosoloid of toughness simultaneously, form mechanical twin, thus realize high-entropy alloy matrix material mould combination by force, prepare the high-entropy alloy matrix material of high-strength and high ductility.
Described interior raw nano ceramics strengthens high-entropy alloy matrix material, and the alloying constituent atomic ratio expression formula of its matrix material is: Al
xfeCrCo
yni (Cu)
mti
z/ (1-15) vol%TiC, wherein 0≤x≤0.7,0≤z≤0.7 and x+z=0.7,1≤y≤1.5, m is 0 or 1.
Described interior raw nano ceramics strengthens the preparation method of high-entropy alloy matrix material, specifically comprises the following steps:
1. material choice: described Al, Fe, Cr, Co, Ni, Cu, Ti metal-powder purity >99.9%, granularity≤45 μm; The purity >99.9% of described carbon dust, granularity≤100 μm.According to Al
xfeCrCo
yni (Cu)
mti
z/ (1-15) vol%TiC nominal composition weighs, and load weighted metal-powder and carbon dust is placed in stainless steel or Ceramic Balls grinding jar in order, is filled with high purity inert gas, in order to ball milling after vacuumizing.
2. composite granule preparation: powder ready in step one is carried out mechanical alloying in high energy ball mill, dry grinding rotating speed 400 ~ 500r/min, the dry grinding time is 40 ~ 50h, wet-milling time 2 ~ 5h, and wet-milling rotating speed is 100 ~ 300r/min; After wet-milling, open vacuum tank, after vacuum-drying 24 ~ 36h, through 50 ~ 100r/min ball milling, 1 ~ 2h, prepare high-entropy alloy composite powder.
3. matrix material densification:
Above-mentioned high-entropy alloy composite powder is placed in graphite jig, and adopt discharge plasma sintering stove to sinter, sintering temperature is 1000 DEG C, and sintering time is 10min, and pressurize during sintering 30Mpa, vacuum tightness <8Pa; Temperature rise rate is: 600 DEG C/4min; The temperature rise rate of 600-900 DEG C and 900-1000 DEG C is respectively 75 DEG C/min and 50 DEG C/min; Finally be down to room temperature, obtain described high-entropy alloy matrix material.
XRD, TEM, testing machine for mechanical properties etc. is adopted to test described high-entropy alloy matrix material.
Interior raw nano ceramics of the present invention strengthens high-entropy alloy matrix material, make alloy substrate based on the high-entropy alloy matrix of high-ductility face-centered cubic sosoloid (FCC) by Composition Design and preparation technology, simultaneously, raw nano-ceramic particle segregation is on simple sosoloid crystal boundary, produces ceramic enhancement phase strengthening; In heating, cure under pressure process, ceramic phase produces crimp effect to FCC phase, form mechanical twin, thus realize high-entropy alloy matrix material mould combination by force, prepare the high-entropy alloy matrix material of high-strength and high ductility or the part according to dies cavity shape.
Accompanying drawing explanation
Fig. 1 is the tem analysis figure of matrix material prepared by embodiment 1;
Fig. 2 is the stress-strain curve of matrix material of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further.
The selection of raw material: according to the form below take purity be 99.99% Al, Fe, Cr, Co, Ni, Cu, Ti metal-powder and purity be the carbon dust of 99.99%, granularity≤45 μm.
The quality that metal constituent element selected by matrix material prepared by table 1, and unit is g.
| Alloying element | Al | Fe | Cr | Co | Cu | Ni | Ti | C |
| Embodiment 1 | 18.9 | 56 | 52 | 88.5 | 0 | 59 | 48 | 12 |
| Embodiment 2 | 10.8 | 56 | 52 | 59 | 64 | 59 | 38.4 | 6 |
| Embodiment 3 | 0 | 56 | 52 | 59 | 64 | 59 | 72 | 12 |
Embodiment 1
(1) composite granule preparation: by upper table, ready powder is carried out mechanical alloying in high energy ball mill, dry grinding rotating speed is 450r/min, dry grinding time 45h, wet-milling time 5h, wet-milling rotating speed 200r/min, prepares high-entropy alloy composite powder.Concrete steps are as follows:
A) by waiting for that the powder of ball milling puts into stainless steel grinding jar, using Stainless Steel Ball as grinding element, ball milling is compared according to the ball powder quality of 10:1.Before ball milling, first vacuumize 10min with vacuum machine, be filled with 0.5MPa argon gas afterwards as shielding gas; The rotating speed of ball mill is 450r/min, and every 60min needs adjustment sense of rotation once, samples respectively at ball milling 5h, 15h, 30h, 45h.
B) dehydrated alcohol is added in the powder of ball milling 45h and carry out wet-milling 5h.After ball milling terminates, take out ball grinder, vacuum drying oven is opened, then opens ball grinder cover, and reserve certain gap, after putting it into loft drier, close upper chamber door.After vacuumizing with vacuum machine, temperature is adjusted to 50 DEG C, takes out after 24h drying.Powder after super-dry is put into ball mill, with the rotating speed ball milling 1.5h of 80r/min, takes out stand-by after preparing the screening of high-entropy alloy composite powder.
(2) matrix material densification: above-mentioned high-entropy alloy composite powder is placed in graphite jig, discharge plasma sintering stove is adopted to sinter, sintering temperature is 1000 DEG C: sintering time is 10min, and pressurize during sintering 30Mpa, vacuum tightness <8Pa; Temperature rise rate is: 600 DEG C/4min; The temperature rise rate of 600-900 DEG C and 900-1000 DEG C is respectively 75 DEG C/min and 50 DEG C/min, cool to room temperature, and obtained described high-entropy alloy matrix material, its alloying constituent atomic ratio expression formula is Al
0.7feCrCo
1.5ni/15vol%TiC.
(3) stuctures and properties characterizes, and adopts XRD, TEM, testing machine for mechanical properties etc. to test above-mentioned sample.Composition graphs 1, endogenous TiC size distribution is in grain boundaries, and to crystal grain extruding in alloy compaction process, cause the appearance of mechanical twin, wherein Fig. 1 a is shape appearance figure, and Fig. 1 b is the selected diffraction figure of twin; The compression yield strength of described matrix material, breaking tenacity and plastix strain reach 2050 ± 15Mpa, 2410 ± 15MPa and 17 ± 0.50%, micro-hardness average out to 650 ± 15Hv respectively.
Embodiment 2
Take alloy powder and carbon dust by upper table, adopt identical method in embodiment 1 to prepare high-entropy alloy matrix material, alloying constituent is Al
0.4feCrCoCuNiTi
0.3/ 5vol%TiC, the room temperature compressed rupture strength of described matrix material and plastix strain reach 2220MPa and 22.8% respectively.
Embodiment 3
Take alloy powder and carbon dust by upper table, adopt identical method in embodiment 1 to prepare high-entropy alloy matrix material, alloying constituent is FeCrCoCuNiTi
0.7/ 10vol%TiC, the room temperature compressed rupture strength of described matrix material and plastix strain reach 2310MPa and 20.4% respectively.
Claims (3)
1. in, raw nano ceramics strengthens a high-entropy alloy matrix material, and it is characterized in that, the alloying constituent atomic ratio expression formula of described matrix material is: Al
xfeCrCo
yni (Cu)
mti
z/ (1-15) vol%TiC, wherein 0≤x≤0.7,0≤z≤0.7 and x+z=0.7,1≤y≤1.5, m is 0 or 1.
2. prepare the method that interior raw nano ceramics according to claim 1 strengthens high-entropy alloy matrix material, it is characterized in that, comprise the following steps:
1. load weighted metal-powder and carbon dust are placed in stainless steel or Ceramic Balls grinding jar in order, are filled with high purity inert gas after vacuumizing, in order to ball milling;
2. above-mentioned powder is carried out mechanical alloying in high energy ball mill, dry grinding rotating speed 400 ~ 500r/min, the dry grinding time is 40 ~ 50h, wet-milling time 2 ~ 5h, and wet-milling rotating speed is 100 ~ 300r/min; After wet-milling, open vacuum tank, after vacuum-drying 24 ~ 36h, through 50 ~ 100r/min ball milling, 1 ~ 2h, prepare high-entropy alloy composite powder;
3. above-mentioned high-entropy alloy composite powder is placed in graphite jig, adopt discharge plasma sintering stove to sinter, sintering temperature is 1000 DEG C, and sintering time is 10min, and pressurize during sintering 30Mpa, vacuum tightness <8Pa; Temperature rise rate is: 600 DEG C/4min; The temperature rise rate of 600-900 DEG C and 900-1000 DEG C is respectively 75 DEG C/min and 50 DEG C/min; Finally be down to room temperature, obtain described high-entropy alloy matrix material.
3. interior raw nano ceramics according to claim 2 strengthens the preparation method of high-entropy alloy matrix material, it is characterized in that, the purity >99.9% of described Al, Fe, Cr, Co, Ni, Cu, Ti metal-powder, granularity≤45 μm; The purity >99.9% of described carbon dust, granularity≤100 μm.
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Cited By (25)
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| CN105950945A (en) * | 2016-06-29 | 2016-09-21 | 华南理工大学 | High-strength high-entropy alloy NbMoTaWVCr and preparation method thereof |
| CN106001566A (en) * | 2016-06-29 | 2016-10-12 | 华南理工大学 | High-strength high-entropy alloy NbMoTaWV and preparation method thereof |
| CN107043884A (en) * | 2017-04-13 | 2017-08-15 | 贵州理工学院 | A kind of TiO particles enhancing CoCrCuFeNi high-entropy alloys and preparation method thereof |
| CN107142475A (en) * | 2017-04-22 | 2017-09-08 | 南京工程学院 | A kind of laser cladding strengthens new A lFeCrCoNiTi alloy-base composite materials coating and preparation method with TiC |
| CN107267845A (en) * | 2017-06-21 | 2017-10-20 | 南京理工大学 | Nano particle TiC strengthens the microwave synthesis method of high-entropy alloy-base composite material |
| CN107904439A (en) * | 2017-11-16 | 2018-04-13 | 淮阴工学院 | A kind of in-situ nano multiphase composite toughening titanium matrix composite and preparation method thereof |
| CN108018550A (en) * | 2016-11-04 | 2018-05-11 | 叶均蔚 | multi-layer film structure |
| CN108103381A (en) * | 2018-01-25 | 2018-06-01 | 华南理工大学 | A kind of high-strength F eCoNiCrMn high-entropy alloys and preparation method thereof |
| CN108383507A (en) * | 2018-03-09 | 2018-08-10 | 辽阳市粉末冶金研究所 | The method that one step prepares high emissivity complex phase ceramic and FeCrCoNi high-entropy alloys |
| CN108504890A (en) * | 2018-05-17 | 2018-09-07 | 哈尔滨工业大学 | One kind having base high-entropy alloy composite material and preparation method |
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| CN109180188A (en) * | 2018-10-08 | 2019-01-11 | 中南大学 | A kind of high entropy carbide containing boron ultra-high temperature ceramic powder and preparation method thereof |
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