CN109136601A - A kind of high hardware heart cubic phase enhances the high-entropy alloy composite material and preparation method of tough modeling face-centred cubic structure - Google Patents
A kind of high hardware heart cubic phase enhances the high-entropy alloy composite material and preparation method of tough modeling face-centred cubic structure Download PDFInfo
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- 239000000843 powder Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 25
- 239000006104 solid solution Substances 0.000 claims abstract description 10
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- C—CHEMISTRY; METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention discloses the high-entropy alloy composite material and preparation methods that a kind of high hardware heart cubic phase enhances tough modeling face-centred cubic structure.Preparation process includes the high-entropy alloy for designing high rigidity and the high-entropy alloy system of tough modeling face-centred cubic structure, prepares two kinds of high-entropy alloy powders according to progress vacuum high-energy ball milling after calculating proportion;High hard phase and toughness phase are added according to the proportion and carries out mixed powder;Two-phase high-entropy alloy composite material is prepared using discharge plasma sintering technique.The composite material of acquisition can improve reinforced phase and tough matrix phase interface bonding strength, overcome the wetting out problems between heterogeneous reinforced phase and matrix phase, the body-centered cubic structure solid solution of hard causes to squeeze to the face-centered cubic solid solution of toughness simultaneously, form deformation twin, to realize that the strong modeling of high-entropy alloy composite material combines, make two-phase high-entropy alloy composite material that there is good mechanical property.
Description
Technical field
The invention belongs to metal-base composites technical fields, and in particular to a kind of high hardware heart cubic phase (BCC) enhancing
The high-entropy alloy composite material and preparation method of tough modeling face-centred cubic structure (FCC).
Background technique
Block high-entropy alloy (HEA) has high intensity, high rigidity, low elasticity modulus 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, body
The high brittleness of the alloy system of heart cubic structure makes HEA material in the case where not obvious room temperature macroscopic view plastic deformation, with prominent
Catastrophic fracture occurs for the mode of crash;Face-centred cubic structure alloy system good toughness, but intensity and hardness are all lower.This
All seriously restrict large-scale application of the HEA as advanced configuration material in engineering a bit.Therefore, how high-strength and high ductility is obtained
High entropy alloy material be high-entropy alloy area research emphasis.
Currently, the reinforcement for preparing metal-base composites generally uses the Al of hard2O3, the ceramic particles such as SiC, TiC,
But its performance does not reach theoretical value, study carefully its main cause be exactly composite material boundary strength it is low.Yang Chao et al. research
Precipitation hardening non-crystalline material belongs to the composite material scope of metal enhancing metal;Wang Zhi et al. has studied
Mg65Cu20Zn5Y10Amorphous reinforced aluminum matrix composites, the very good solution interface problem of composite material, and mechanical property
Also it is improved compared with matrix.But, it is contemplated that non-crystalline material is limited (amorphous metal material crystallization temperature one by crystallization temperature
As be lower than 650 DEG C), composite material interface be difficult by improve sintering temperature be improved, therefore, such material is not from basic
Upper solution metal enhances metallic composite interface problem.Based on the studies above, the present invention devises one kind with high-strength high rigidity
Body-centered cubic structure BCC high-entropy alloy (such as FeNiCoCrCuAl2.8Hardness is 655HV) enhancing face-centred cubic structure FCC high
Entropy alloy, high-entropy alloy have high-temperature stability, can improve the boundary of composite material by improving preparation temperature (being higher than 600 DEG C)
Face bond strength.
Summary of the invention
In order to achieve the above objectives, the present invention provides a kind of high hardware heart cubic phase (BCC) enhancing tough modeling face-centered cubic knot
The high-entropy alloy composite material and preparation method of structure (FCC) improve composite material while keeping its excellent in strength and hardness
Plasticity.
In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical scheme that:
A kind of high hardware heart cubic phase enhances the high-entropy alloy composite material of tough modeling face-centred cubic structure, which is characterized in that
Using the face-centred cubic structure FCC high-entropy alloy of high-ductility as matrix, the body-centered cubic structure BCC high-entropy alloy of high-strength high rigidity is
Reinforced phase, high-entropy alloy are the nanocrystalline or Ultra-fine Grained high-entropy alloy powder after high-energy ball-milling alloying.
The high-entropy alloy is that body center cubic solid solution (BCC) alloy system that each alloy compositions are generated according to atomic ratio is
AlxFeCrCoNiCu, face-centred cubic structure (FCC) alloy system are AlxFeCrCoyNizCu;In high-entropy alloy, Al, Fe, Cr,
Co, Ni, Cu, Ti metal powder purity > 99.9%, granularity≤45 μm.
In composite material, the mass content of BCC high-entropy alloy is 10-40wt%, and the mass content of FCC high-entropy alloy is
60-90wt%.
The microstructure of composite material is twin by the nanometer or Ultra-fine Grained BCC solid solution phase and partial deformation nanometer FCC of hard
Crystalline substance tissue collectively constitutes.
High rigidity BCC high-entropy alloy ingredient is AlxFeCrCoNiCu, wherein each element content is molar ratio, aluminium content 0.7
<x>3;Plasticity FCC high-entropy alloy system is AlvFeCrCoyNizCu, aluminium content 0 < v < 0.7, the sum of cobalt element and nickel element content
Are as follows: 2 < z+y < 5.
The matrix and reinforced phase is the alloyed powder obtained after vacuum high-energy ball milling.
A kind of high-entropy alloy composite material of tough modeling face-centred cubic structure (FFC) of high hardware heart cubic phase (BBC) enhancing
Preparation method, which comprises the following steps:
1) raw material selects: metal powders purity > 99.9% such as Al, Fe, Cr, Co, Ni, Cu, Ti, granularity≤45 μm;According to
The atom ratio of each element carries out weighing each metal powder;
2) metal powder of load weighted two kinds of systems is placed in stainless-steel vacuum grinding jar, is filled with indifferent gas after vacuumizing
Body carries out mechanical alloying in high energy ball mill, first dry grinds, rear wet-milling: dry grinding 300~500r/min of revolving speed dry grinds the time
For 40~50h, 2~5h of wet-milling time, wet-milling revolving speed is 100~300r/min;After wet-milling, vacuum tank, vacuum drying 24 are opened
After~36h, through 50~100r/min, 1~2h of ball milling, two kinds of high-entropy alloy powders of BCC and FCC solid solution structure are prepared;
3) prepared by composite material powder: example weighing in mass ratio being added in two kinds of high-entropy alloy powders that step 2) obtains
It is good, by the mechanical mixture 3-5h of 150~200r/min, prepare composite material powder;In composite material powder, composite material
In, the mass content of BCC high-entropy alloy powder is 10-40wt%, and the mass content of FCC high-entropy alloy powder is 60-90wt%;
4) discharge plasma sintering shapes: above-mentioned high-entropy alloy composite powder being placed in graphite jig, using electric discharge etc.
Ion sintering technology carries out vacuum-sintering, and sintering temperature is 1000-1100 DEG C, sintering time 10min, and when sintering pressurizes 30-
50Mpa, vacuum degree < 8Pa obtain the high-entropy alloy composite material.
Step 4) is composite material densification steps.
The high-entropy alloy composite material is tested using XRD, TEM, testing machine for mechanical properties etc..
Further, the specific steps of preparation method are as follows:
A) each metal-powder of ball milling will be waited to be put into stainless steel grinding jar, using stainless steel ball as abrasive body, according to not
Ball powder quality lower than 10:1 compares ball milling;Before ball milling, 10min first is vacuumized with vacuum machine, is filled with 0.5MPa argon gas work later
For protective gas;The revolving speed of ball mill be 350r/min, and every 60min need to adjust direction of rotation it is primary;
B) dehydrated alcohol is added in the powder of dry grinding 45h and carries out wet-milling 5h;After ball milling terminates, ball grinder is taken out, it will
Vacuum oven is opened, and is then opened ball grinder cover, and reserve certain gap, is shut chamber door after putting it into drying box;
Temperature is adjusted to 50 DEG C after being vacuumized with vacuum machine, is taken out after drying for 24 hours;Powder after dry is put into
In ball mill, with the revolving speed ball milling 2h of 120r/min, taken out for use after the screening of high-entropy alloy composite powder is prepared;
C) composite material densifies: the FCC high entropy of BCC high-entropy alloy and 70wt% that the step 2) of 30wt% is obtained closes
Bronze body, which is placed in ball grinder, carries out powder mixing machine;Vacuum-sintering is carried out using discharge plasma sintering technique, sintering temperature is
1050 DEG C, sintering time 10min, when sintering, pressurizes 50Mpa, and vacuum degree < 8Pa obtains the high-entropy alloy composite material.
The high-entropy alloy composite wood of tough modeling face-centred cubic structure (FCC) of high hardware heart cubic phase (BCC) enhancing of the invention
Material designs and prepares the two-phase high-entropy alloy composite material of technique preparation by ingredient, closes by the high entropy that high-energy ball milling obtains
Gold is nanocrystalline or Ultra-fine Grained, generates metal phase enhancing and strengthens;Heating, pressurization densification process in, BCC high-entropy alloy phase with
FCC high-entropy alloy mutually while keeping respective crystal structure, realizes that the strong modeling of high-entropy alloy composite material combines, in addition, firmly
The BCC crystal grain of matter phase can generate extruding to FCC phase, and nanometer FCC deformation occurs feather organization prepares the double of high-strength and high ductility
Phase high-entropy alloy composite material.
Detailed description of the invention
Fig. 1 is composite sample of the Examples 1 and 2 after discharge plasma sintering;
Fig. 2 is the XRD analysis figure of BCC high-entropy alloy prepared by embodiment 1;
Fig. 3 is the XRD analysis figure of FCC high-entropy alloy prepared by embodiment 1;
Fig. 4 is the two-phase high-entropy alloy composite material of embodiment 2;
Fig. 5 is the TEM figure of composite material prepared by embodiment 2.
Specific embodiment
The present invention is further described below by embodiment and attached drawing.
Raw material selects: according to the form below 1 weighs purity as 99.99% Al, Fe, Cr, Co, Ni, Cu metal powder, and granularity≤
45μm。
Embodiment 1
(1) prepared by composite granule: by ready FeNiCoCrCuAl2.8(under be designated as molar ratio) with
Al0.3FeNiCo1.2CrCu powder carries out mechanical alloying in high energy ball mill, and dry grinding revolving speed is 400r/min, and dry grind 40h
Afterwards, two aspect high-entropy alloy FeNiCoCrCuAl of body-centered is prepared in wet-milling time 5h, wet-milling revolving speed 300r/min2.8Powder.
Specific step is as follows:
A) powder for waiting ball milling is put into two different stainless steel grinding jars, using stainless steel ball as abrasive body, according to
Ball powder quality not less than 10:1 compares ball milling.Before ball milling, 10min first is vacuumized with vacuum machine, is filled with 0.5MPa argon gas later
As protective gas;The revolving speed of ball mill be 400r/min, and every 60min need to adjust direction of rotation it is primary.
B) dehydrated alcohol is added in the powder of ball milling 45h and carries out wet-milling 5h.After ball milling terminates, ball grinder is taken out, it will
Vacuum oven is opened, and is then opened ball grinder cover, and reserve certain gap, is shut chamber door after putting it into drying box.
Temperature is adjusted to 50 DEG C after being vacuumized with vacuum machine, is taken out after drying for 24 hours.Powder after dry is put into
In ball mill, with the revolving speed ball milling 2h (dry grinding) of 150r/min, taken out for use after the screening of high-entropy alloy composite powder is prepared.
(2) composite material densifies: above-mentioned BCC high-entropy alloy powder (30wt%) is set with FCC alloy powder (70wt%)
Carry out powder mixing machine in ball grinder (by the mechanical mixture 4h of 150r/min);It is carried out using discharge plasma sintering technique true
Sky sintering, sintering temperature are 1050 DEG C, sintering time 10min, and when sintering pressurizes 50Mpa, and vacuum degree < 8Pa obtains the height
Entropy alloy composite materials, finally obtaining diameter as shown in Figure 1 is 20mm, and height is about the composite material of 5mm.
(3) structure and performance characterization test above-mentioned sample using equipment such as XRD, TEM.XRD analysis shows two
Kind high-entropy alloy is single BCC and FCC crystallographic structure (Fig. 2 and Fig. 3).In conjunction with Fig. 4 and Fig. 5, hard BCC phase and FCC phase
It is nanocrystalline, and BCC squeezes FCC solid solution crystal grain in alloy compaction process, causes the appearance of deformation twin.It is described multiple
Compression yield strength, breaking strength, plastic strain and the hardness of condensation material respectively reach 1530 ± 10MPa, 2060 ± 10MPa,
27.50% and 515HV.
The preparation of 2 composite granule of embodiment: upper table 1 is pressed by ready Al2FeNiCoCrCu (under be designated as molar ratio) preparation
BCC high-entropy alloy powder out, specific steps reference implementation example 1.
The alloy substrate of composite material selects Al0.4FeCrCo1.5NiTi0.3Alloy, composite material preparation process reference implementation
Example 1.Composite material pictorial diagram and TEM are shown in Fig. 4 and Fig. 5.Tem analysis shows that hard BCC phase with FCC phase is nanocrystalline, and
BCC squeezes FCC solid solution crystal grain in alloy compaction process, causes the appearance (Fig. 5) of deformation twin.
Two-phase high-entropy alloy composite material of the invention, using BCC high-entropy alloy particle as reinforced phase.It is according to height first
The design principle of entropy alloy designs the hard BCC high-entropy alloy system of high-strength height;Proportion alloy is carried out according to design ingredient, is used
Mechanic Alloying Technology, vacuum sphere grind the high-entropy alloy powder taken with body-centered cubic structure and face-centred cubic structure;It will system
The two kinds of high-entropy alloy powders got ready carry out sufficient mechanical mixture;Using at the technique of base hot extrusion again, preparing high-strength in advance
The high-entropy alloy composite material of high-ductility.The above is only a preferred embodiment of the present invention, it should be pointed out that: this technology is led
For the those of ordinary skill in domain, without departing from the principle of the present invention, several improvement and equivalent form can also be made
Replacement, these are improved and the obtained technical solution of equivalent replacement also should belong to protection scope of the present invention.
Claims (7)
1. the high-entropy alloy composite material that a kind of high hardware heart cubic phase enhances tough modeling face-centred cubic structure, which is characterized in that with
Plasticity FCC high-entropy alloy is matrix, and high rigidity BCC high-entropy alloy is reinforced phase, and double structure is by nanocrystalline or Ultra-fine Grained
Composition.
2. the high-entropy alloy that a kind of high hardware heart cubic phase according to claim 1 enhances tough modeling face-centred cubic structure is compound
Material, which is characterized in that the high-entropy alloy be the body center cubic solid solution (BCC) that is generated according to atomic ratio of each alloy compositions and
Face-centred cubic structure solid solution (FCC) alloy system;In high-entropy alloy, used raw material Al, Fe, Cr, Co, Ni, Cu's
Metal powder purity > 99.9%, granularity≤45 μm.
3. the high-entropy alloy that a kind of high hardware heart cubic phase according to claim 1 enhances tough modeling face-centred cubic structure is compound
Material, which is characterized in that high rigidity BCC high-entropy alloy ingredient is AlxFeCrCoNiCu, wherein each element content is molar ratio,
Aluminium content 0.7<x>3;Plasticity FCC high-entropy alloy system is AlvFeCrCoyNizCu, aluminium content 0 < v < 0.7, cobalt element and nickel member
The sum of cellulose content are as follows: 2 < z+y < 5.
4. the high-entropy alloy that a kind of high hardware heart cubic phase according to claim 1 enhances tough modeling face-centred cubic structure is compound
Material, which is characterized in that the matrix and reinforced phase is the alloyed powder obtained after vacuum high-energy ball milling.
5. the high-entropy alloy that a kind of high hardware heart cubic phase according to claim 1 enhances tough modeling face-centred cubic structure is compound
Material, which is characterized in that in composite material, the mass content of BCC high-entropy alloy is 10-40wt%, the quality of FCC high-entropy alloy
Content is 60-90wt%.
6. the high-entropy alloy that a kind of high hardware heart cubic phase according to claim 1 enhances tough modeling face-centred cubic structure is compound
The preparation method of material, which comprises the following steps:
1) raw material selects: Al, Fe, Cr, Co, Ni, Cu metal powder purity > 99.9%, granularity≤45 μm;According to claim 3
Two kinds of alloy systems are weighed;
2) metal powder of load weighted two kinds of alloy systems is placed in and is respectively placed in stainless-steel vacuum grinding jar, filled after vacuumizing
Enter high purity argon protection gas, carry out mechanical alloying in high energy ball mill, dry grind 300 ~ 500r/min of revolving speed, and the dry grinding time is
40 ~ 50h, 2 ~ 5h of wet-milling time, wet-milling revolving speed are 100 ~ 300r/min;First dry grind, rear wet-milling;After wet-milling, vacuum tank is opened, very
After the dry 24 ~ 36h of sky, through 50 ~ 100r/min, 1 ~ 2h of dry grinding, two kinds of high-entropy alloy powders are prepared;
3) prepared by composite material powder: weighing, passes through by the mass ratio of design in two kinds of high-entropy alloy powders that step 2 obtains
The mechanical mixture 3-5h of 150 ~ 200r/min, preparation high rigidity BCC enhance plasticity FCC phase two-phase high-entropy alloy composite wood feed powder
Body;In composite material powder, the mass content of BCC high-entropy alloy powder is 10-40wt%, and the quality of FCC high-entropy alloy powder contains
Amount is 60-90wt%;
4) discharge plasma sintering shapes: above-mentioned high-entropy alloy composite powder being placed in graphite jig, using plasma discharging
Sintering technology carries out vacuum-sintering, and sintering temperature is 1000-1100 DEG C, sintering time 10min, and when sintering pressurizes 30-
50Mpa, vacuum degree < 8Pa obtain the high-entropy alloy composite material.
7. a kind of high rigidity BCC according to claim 1 enhances plasticity FCC phase two-phase high-entropy alloy composite material, special
Sign is, the microstructure of composite material by hard nanometer or Ultra-fine Grained BCC solid solution phase and partial deformation nanometer FCC twin
Tissue collectively constitutes.
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Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109972066A (en) * | 2019-05-05 | 2019-07-05 | 西北工业大学 | The method for improving AlCoCrCuFeNi high-entropy alloy power magnetic property using magnetic field |
CN110042295A (en) * | 2019-04-25 | 2019-07-23 | 北京理工大学 | A kind of preparation method of nanometer of high-entropy alloy block materials |
CN110373596A (en) * | 2019-07-08 | 2019-10-25 | 南京工程学院 | A kind of soft magnetism high entropy alloy material of island magnetocrystalline structure and preparation method thereof |
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CN111151753A (en) * | 2020-01-16 | 2020-05-15 | 中南大学 | Method for manufacturing shear deformation type phase change crack resistance by laser additive manufacturing |
CN111187964A (en) * | 2020-02-10 | 2020-05-22 | 东北大学 | High-strength-plasticity antibacterial high-entropy alloy and preparation method thereof |
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CN112143924A (en) * | 2020-09-25 | 2020-12-29 | 西安稀有金属材料研究院有限公司 | Preparation method of multi-scale high-strength high-entropy alloy material for corrosive environment |
CN112746214A (en) * | 2020-12-29 | 2021-05-04 | 中南大学 | Two-phase high-entropy alloy and preparation method thereof |
CN113234982A (en) * | 2021-04-21 | 2021-08-10 | 四川大学 | Preparation method of PDC drill bit matrix material |
CN113385689A (en) * | 2021-06-03 | 2021-09-14 | 广东工业大学 | High-entropy alloy and preparation method and application thereof |
CN113751722A (en) * | 2021-08-17 | 2021-12-07 | 温州大学 | Method for preparing FCC phase high-entropy alloy with high strength and high toughness |
CN114507801A (en) * | 2020-11-16 | 2022-05-17 | 中国科学院上海硅酸盐研究所 | Low-density and high-hardness high-entropy alloy material and preparation method thereof |
CN114855055A (en) * | 2022-05-31 | 2022-08-05 | 广东工业大学 | Low-crack-sensitivity high-entropy alloy powder material and preparation method and application thereof |
CN115354204A (en) * | 2022-08-26 | 2022-11-18 | 武汉纺织大学 | Grain bimodal distribution synergistic oxide dispersion strengthening and toughening high-entropy alloy and preparation thereof |
CN116287909A (en) * | 2023-01-30 | 2023-06-23 | 华东交通大学 | High-specific yield strength high-wear-resistance multistage heterogeneous aluminum alloy and preparation method thereof |
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CN113385689A (en) * | 2021-06-03 | 2021-09-14 | 广东工业大学 | High-entropy alloy and preparation method and application thereof |
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CN116287909A (en) * | 2023-01-30 | 2023-06-23 | 华东交通大学 | High-specific yield strength high-wear-resistance multistage heterogeneous aluminum alloy and preparation method thereof |
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