CN105543621B - Raw nano ceramics enhancing high-entropy alloy composite and preparation method in a kind of - Google Patents
Raw nano ceramics enhancing high-entropy alloy composite and preparation method in a kind of Download PDFInfo
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- CN105543621B CN105543621B CN201610030430.7A CN201610030430A CN105543621B CN 105543621 B CN105543621 B CN 105543621B CN 201610030430 A CN201610030430 A CN 201610030430A CN 105543621 B CN105543621 B CN 105543621B
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- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 39
- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 230000002708 enhancing effect Effects 0.000 title abstract description 7
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000000428 dust Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000001238 wet grinding Methods 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 238000005275 alloying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 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
- 238000009837 dry grinding Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 239000006104 solid solution Substances 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 238000005204 segregation Methods 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
- 239000000463 material Substances 0.000 description 8
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 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
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000005070 sampling Methods 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
- 239000000126 substance Substances 0.000 description 1
- 239000002023 wood Substances 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
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- 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
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses raw nano ceramics enhancing high-entropy alloy composite and preparation method in one kind, matrix phase is used as using high-entropy alloy particle, simultaneously, in Process During High Energy Ball Milling, mechanical alloying energy promotes reaction in-situ generation nano ceramics TiC, make interior raw nano ceramics phase segregation in solid solution grain boundaries, produce ceramic phase enhancing, extruding is caused to the face-centered cubic solid solution of toughness simultaneously, form deformation twin, so as to realize that the strong modeling of high-entropy alloy composite is combined, prepare the high-entropy alloy composite of high-strength and high ductility, while its excellent in strength and hardness is kept, improve the plasticity of composite.
Description
Technical field
The invention belongs to metal-base composites technical field, and in particular to a kind of high-entropy alloy composite and its preparation
Method.
Background technology
Block high-entropy alloy (HEA) has high intensity, high rigidity, low modulus of elasticity and big elastic strain limit etc. one
Series is different from the excellent mechanical performance of traditional crystal alloy so that it is considered as the structural material of great potential.However, high
Fragility causes HEA materials that in the case of unobvious room temperature macroscopic view plastic deformation, calamity occurs in the way of catastrophic failure
Fracture；The processing of high fragility, high rigidity to material brings extreme difficulties.These all seriously govern HEA as advanced knot
Large-scale application of the structure material in engineering.Therefore, brittleness at room temperature, processing difficulties problem have been developed as HEA materials applications
Important bottleneck.
To improve the brittleness at room temperature of HEA materials and the problem of processing difficulties, researchers' metal member different by adding
Element, the block materials of dendritic segregation are prepared using arc cast, among these to add Cu effects substantially, its compression plastic strain
Reach within 8%.Then, Zhang Yong et al. prepares the high entropy alloy material with columanar structure by directional solidification technique, its
Compressive ductility increases；It is enhanced that Wang Yanping etc. is prepared for interior raw 10vol.%TiC particles using arc cast
CrFeCoNiCuAl high-entropy alloy-base composite materials（HEAMCs）, TiC is evenly distributed on matrix into graininess, and size is about
Several microns.The compressive strength and hardness of CrFeCoNiCuTi-TiC composites can respectively reach 2040MPa and 746HV,
Compression plasticity about 12%.But the acquisition of the plasticity of above-mentioned high entropy alloy material, be not considerably reduce intensity be exactly improve modeling
Property aspect it is unobvious.
The content of the invention
It is an object of the invention to provide a kind of high-entropy alloy composite and preparation method, keep its excellent in strength and
While hardness, the plasticity of composite is improved.
The high-entropy alloy composite of the present invention, using high-entropy alloy particle as matrix phase, meanwhile, in Process During High Energy Ball Milling
In, mechanical alloying energy promotes reaction in-situ generation nano ceramics TiC：Ti+CTiC, makes interior raw nano ceramics phase segregation
In solid solution grain boundaries, ceramic phase enhancing is produced, while causing extruding to the face-centered cubic solid solution of toughness, deformation is formed twin
Crystalline substance, so as to realize that the strong modeling of high-entropy alloy composite is combined, prepares the high-entropy alloy composite of high-strength and high ductility.
The interior raw nano ceramics enhancing high-entropy alloy composite, the alloying component atomic ratio expression formula of its composite
For：AlxFeCrCoyNi(Cu)mTiz/ (1-15) vol%TiC, wherein 0≤x≤0.7,0≤z≤0.7 and x+z=0.7,1≤y
≤ 1.5, m are 0 or 1.
The interior raw nano ceramics strengthens the preparation method of high-entropy alloy composite, specifically includes following steps：
1. raw material is selected：Al, Fe, Cr, Co, Ni, Cu, Ti metal dust purity>99.9%, granularity≤45 μm；It is described
The purity of carbon dust>99.9%, granularity≤100 μm.According to AlxFeCrCoyNi(Cu)mTiz/ (1-15) vol%TiC nominal compositions
Weighed, load weighted metal-powder and carbon dust are placed in stainless steel or ceramic ball grinder in order, are filled with after vacuumizing
High purity inert gas, in case ball milling.
2. prepared by composite granule：Ready powder in step one is subjected to mechanical alloying in high energy ball mill, done
400 ~ 500r/min of rotating speed is ground, the dry grinding time is 40 ~ 50h, and 2 ~ 5h of wet-milling time, wet-milling rotating speed is 100 ~ 300r/min；Wet-milling
Afterwards, open after vacuum tank, 24 ~ 36h of vacuum drying, through 50 ~ 100r/min, 1 ~ 2h of ball milling, prepare high-entropy alloy composite powder
End.
3. composite is densified：
Above-mentioned high-entropy alloy composite powder is placed in graphite jig, is sintered using discharge plasma sintering stove, is burnt
Junction temperature is 1000 DEG C, and sintering time is 10min, and pressurize 30Mpa during sintering, vacuum<8Pa；Heating rate is：600℃/
4min；600-900 DEG C and 900-1000 DEG C of heating rate is respectively 75 DEG C/min and 50 DEG C/min；Room temperature is finally down to, is obtained
To the high-entropy alloy composite.
The high-entropy alloy composite is tested using XRD, TEM, testing machine for mechanical properties etc..
The interior raw nano ceramics enhancing high-entropy alloy composite of the present invention, makes alloy by composition design and preparation technology
Matrix is with high-ductility face-centered cubic solid solution（FCC）Based on high-entropy alloy matrix, while interior raw nano-ceramic particle segregation in
On simple solid solution crystal boundary, ceramic enhancement phase reinforcing is produced；During heating, cure under pressure, ceramic phase produces crowded to FCC phases
Compressive strain effect, forms deformation twin, so as to realize that the strong modeling of high-entropy alloy composite is combined, prepares the height of high-strength and high ductility
Entropy alloy composite materials or the part being molded according to dies cavity shape.
Brief description of the drawings
Fig. 1 is the tem analysis figure of composite prepared by embodiment 1；
Fig. 2 is the stress-strain curve of composite of the present invention.
Embodiment
The present invention is described further below in conjunction with the accompanying drawings.
The selection of raw material：According to the form below weighs Al, Fe, Cr, Co, Ni, Cu, Ti metal dust and purity that purity is 99.99%
For 99.99% carbon dust, granularity≤45 μm.
Table 1 prepares the quality that composite selects metal constituent element, 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）It is prepared by composite granule：Ready powder is subjected to mechanical alloying in high energy ball mill by upper table, dry grinded
Rotating speed is 450r/min, and dry grind time 45h, wet-milling time 5h, wet-milling rotating speed 200r/min, prepares high-entropy alloy composite powder
End.Comprise the following steps that：
a）The powder for waiting ball milling is put into stainless steel grinding jar, using stainless steel ball as abrasive body, according to 10:1 ball
Powder quality compares ball milling.Before ball milling, 10min is first vacuumized with vacuum machine, 0.5MPa argon gas is filled with afterwards as protective gas；Ball
The rotating speed of grinding machine is 450r/min, and needs adjustment direction of rotation once per 60min, in ball milling 5h, 15h, 30h, 45h difference
Sampling.
b）Wet-milling 5h is carried out in the powder that absolute ethyl alcohol is added to ball milling 45h.After ball milling terminates, ball grinder is taken out, will
Vacuum drying chamber is opened, and then opens ball grinder cover, and reserves certain gap, puts it into and chamber door is shut after drying box.
By temperature adjustment to 50 DEG C after being vacuumized with vacuum machine, taken out after 24h is dried.Powder after drying is put into
In ball mill, with 80r/min rotating speed ball milling 1.5h, take out stand-by after preparing the screening of high-entropy alloy composite powder.
（2）Composite is densified：Above-mentioned high-entropy alloy composite powder is placed in graphite jig, using plasma discharging
Sintering furnace is sintered, and sintering temperature is 1000 DEG C：Sintering time is 10min, and pressurize 30Mpa during sintering, vacuum<8Pa；Rise
Warm speed is：600℃/4min；600-900 DEG C and 900-1000 DEG C of heating rate is respectively 75 DEG C/min and 50 DEG C/min,
Room temperature is cooled to, the high-entropy alloy composite is made, its alloying component atomic ratio expression formula is Al0.7FeCrCo1.5Ni/
15vol%TiC。
（3）Structure and performance characterization, are tested above-mentioned sample using XRD, TEM, testing machine for mechanical properties etc..With reference to
Fig. 1, endogenous TiC distribution of particles is extruded crystal grain in grain boundaries, and in alloy compaction process, causes the appearance of deformation twin,
Wherein Fig. 1 a are shape appearance figure, and Fig. 1 b are the selected diffraction figures of twin；The compression yield strength of the composite, fracture strength and
Plastic strain respectively reaches 2050 ± 15 Mpa, 2410 ± 15 MPa and 17 ± 0.50%, micro-hardness average out to 650
± 15Hv。
Embodiment 2
Alloy powder and carbon dust are weighed by upper table, high-entropy alloy composite wood is prepared using identical method in embodiment 1
Material, alloying component is Al0.4FeCrCoCuNiTi0.3/ 5vol%TiC, the room temperature compressed rupture strength and plasticity of the composite
Strain respectively reaches 2220MPa and 22.8%.
Embodiment 3
Alloy powder and carbon dust are weighed by upper table, high-entropy alloy composite is prepared using identical method in embodiment 1,
Alloying component is FeCrCoCuNiTi0.7/ 10vol%TiC, the room temperature compressed rupture strength of the composite and plastic strain point
2310MPa and 20.4% are not reached.
Claims (2)
1. a kind of interior raw nano ceramics strengthens the preparation method of high-entropy alloy composite, it is characterised in that the composite
Alloying component atomic ratio expression formula be：AlxFeCrCoyNi(Cu)mTiz/ (1-15) vol%TiC, wherein 0≤x≤0.7,0
≤ z≤0.7 and x+z=0.7,1≤y≤1.5, m are 0 or 1；Comprise the following steps：
1. load weighted metal-powder and carbon dust are placed in stainless steel or ceramic ball grinder in order, are filled with after vacuumizing high-purity
Inert gas, in case ball milling；
2. above-mentioned powder is subjected to mechanical alloying in high energy ball mill, dry grind 400 ~ 500r/min of rotating speed, the dry grinding time is
40 ~ 50h, 2 ~ 5h of wet-milling time, wet-milling rotating speed are 100 ~ 300r/min；After wet-milling, vacuum tank is opened, 24 ~ 36h is dried in vacuo
Afterwards, through 50 ~ 100r/min, 1 ~ 2h of ball milling, high-entropy alloy composite powder is prepared；
3. above-mentioned high-entropy alloy composite powder is placed in graphite jig, be sintered using discharge plasma sintering stove, sintered
Temperature is 1000 DEG C, and sintering time is 10min, and pressurize 30MPa during sintering, vacuum<8Pa；Heating rate is：600℃/
4min；600-900 DEG C and 900-1000 DEG C of heating rate is respectively 75 DEG C/min and 50 DEG C/min；Room temperature is finally down to, is obtained
To the high-entropy alloy composite.
2. interior raw nano ceramics according to claim 1 strengthens the preparation method of high-entropy alloy composite, its feature exists
In the purity of Al, Fe, Cr, Co, Ni, Cu, Ti metal dust>99.9%, granularity≤45 μm；The purity of the carbon dust>
99.9%, granularity≤100 μm.
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| CN117305829B (en) * | 2023-11-10 | 2024-03-12 | 西安工程大学 | Preparation method of nano ceramic particle reinforced high-entropy alloy-based composite powder suitable for cold spraying |
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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 |
| CN109180188B (en) * | 2018-10-08 | 2021-01-29 | 中南大学 | High-entropy boron-containing carbide ultra-high temperature ceramic powder and preparation method thereof |
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| CN105543621A (en) | 2016-05-04 |
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