CN110042295A - A kind of preparation method of nanometer of high-entropy alloy block materials - Google Patents
A kind of preparation method of nanometer of high-entropy alloy block materials Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B22F3/08—Compacting only by explosive forces
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- 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
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Abstract
The present invention relates to the preparation methods of a kind of nanometer of high-entropy alloy block materials, belong to technical field of high-entropy.The method is by the way that by five kinds, with the high purity metal powder of first-class atomic ratio or nearly atomic ratio, ball milling, the metal powder for then obtaining ball milling mixing are fitted into sample cell under protective gas atmosphere, single shaft compacting, obtained compacting powder；Explosion shock wave treatment is carried out to sample cell with explosive, the sample cell after shock treatment is heat-treated under inert gas protection, a kind of nanometer of high-entropy alloy block materials are finally obtained in sample cell.High-entropy alloy block materials hardness with higher, plasticity and the intensity that the method is prepared.The method is low in cost, simple process, time-consuming short, high-efficient, has important theory significance and practical value for the development and application of high-entropy alloy.
Description
Technical field
The present invention relates to the preparation methods of a kind of nanometer of high-entropy alloy block materials, belong to technical field of high-entropy.
Background technique
Nineteen ninety-five Ye Junwei etc. breaks through the traditional idea of design of material, proposes new alloy on amorphous alloy basis and sets
Meter theory, referred to as multi-principal high-entropy alloy (HEA).High-entropy alloy is by five kinds or five kinds or more element constituent elements according to equal atoms
Than or near atomic ratio alloying, the higher alloy of a kind of entropy of mixing of solid solution is formed, due to having high entropy thermodynamically
Distortion of lattice effect in effect, structure, sluggish diffusion effect kinetically, the cocktail effect in performance, are easy to get
The high solid solution phase of thermal stability and nanostructure even non crystalline structure.
High-entropy alloy has the conventional alloys institutes such as high intensity, high rigidity, high-wearing feature, high antioxidant, highly corrosion resistant
The excellent properties that cannot be provided simultaneously with, become most has one of 3 big hot spots of development potentiality in recent years, and there is very high science to grind
Study carefully value.This method involves great expense and limitation of the finally formed product with shape and size, the more than ten years in past, very much
Kind method successfully synthesizes high-entropy alloy, mainly includes vacuum melting method, powder metallurgic method, laser melting coating, electrochemical deposition method
Deng.Vacuum melting method is that most researchers prepare method used by high-entropy alloy, but fusion process is relatively complicated,
Certain limitation can be caused to the size and shape of institute's cast alloy, and be difficult to control the tissue and performance of high-entropy alloy
System.
Summary of the invention
At high cost, complex process and performance instability problem for existing high-entropy alloy block materials preparation method,
The present invention provides the preparation method of a kind of nanometer of high-entropy alloy block materials, the high-entropy alloy block materials plasticity being prepared and
Intensity is improved；The method is at low cost, high-efficient, and product property is stablized excellent, can be used for industrialized production.
To achieve the above object, technical scheme is as follows:
A kind of preparation method of nanometer of high-entropy alloy block materials, the method comprises the following steps:
Step 1: by five kinds with the high purity metal powder of first-class atomic ratio or nearly atomic ratio under protective gas atmosphere ball
60-70h, rotational speed of ball-mill 250-350rpm are ground, ratio of grinding media to material is 8-12:1 (mass ratio), the alloy powder after obtaining ball milling；It is former
Feed powder end select and dosage is this field conventional selection；
Step 2: the alloy powder that ball milling mixing is obtained is fitted into sample cell, single shaft compacting, obtaining consistency is 79-
90% compacting powder；
Step 3: carrying out explosion shock wave treatment, detonation velocity 2300-3500m/s to sample cell；
Step 4: under inert gas protection by the sample cell after shock treatment, it is heat-treated 10-12h at 400-600 DEG C,
It is cooled to room temperature, a kind of nanometer of high-entropy alloy block materials is obtained in sample cell；
Wherein, the purity of metal powder described in step 1 is 99.9% or more.
Preferably, the average grain diameter of metal powder described in step 1 is 5-60 μm.
Preferably, metal powder described in step 1 is Al powder, Co powder Cr powder, Fe powder and Ni powder.
Preferably, the mole dosage of metal powder described in step 1 is equal.
Preferably, protective gas described in step 1 is nitrogen or inert gas.
Preferably, explosion shock wave treatment is carried out to sample cell using explosive in step 3.
Preferably, the explosive is nitromethane liquid, 8701 explosives or B explosive.
Preferably, the sample cell is stainless steel material, wall thickness 2-3mm.
Preferably, the bottom of the sample cell is equipped with momentum block, for unloading shock wave, prevents back wave from damaging sample.
Preferably, the momentum block is piece of stainless steel.
Beneficial effect
The present invention provides the preparation method of a kind of nanometer of high-entropy alloy block materials, first choice makes raw metal using ball milling
Then powder continuous crushing, deformation and cold welding utilize explosive so that powder is sufficiently mixed and is formed certain microstructure
Detonation TRANSIENT HIGH TEMPERATURE high pressure makes compacting powder instantaneously be consolidated, and eliminates alloy finally by heat treatment and produces in impact process
Raw residual stress, so that high-entropy alloy hardness, plasticity and intensity improve.The high-entropy alloy being prepared is consolidated by simple structure
Solution phase composition, alloy structure is uniform, and particle size is nanoscale, and hardness is up to 880HV, and compression strength is up to 1600MPa,
Breaking strain is up to 0.43；The method is low in cost, simple process, time-consuming short, high-efficient, for high-entropy alloy block materials
Development and application have important theory significance and practical value.
Detailed description of the invention
Fig. 1 used schematic device when being explosion shock wave treatment in the method for the invention；
Wherein: 1- plastics upper top cover, 2-PVC are managed, steel plug on 3- stainless steel, 4- stainless steel sample pipe, steel under 5- stainless steel
Plug, 6- plastic feet, 7- momentum block.
Fig. 2 is X-ray diffraction (XRD) figure for the final product that embodiment 1 is prepared.
Fig. 3 is energy dispersion X-ray spectrum (EDX) figure for the final product that embodiment 1 is prepared.
Fig. 4 is that figure is swept in the face electron backscatter diffraction (EBSD) for the final product that embodiment 1 is prepared.
Fig. 5 is the compressive stress strain curve figure for the final product that embodiment 1 is prepared.
Fig. 6 is the XRD diagram for the final product that embodiment 2 is prepared.
Fig. 7 is the EDX figure for the final product that embodiment is prepared.
Fig. 8 is the EBSD figure for the final product that embodiment 2 is prepared.
Fig. 9 is the compressive stress strain curve figure for the final product that embodiment 2 is prepared.
Figure 10 is the XRD diagram for the final product that embodiment 3 is prepared.
Figure 11 is the compressive stress strain curve figure for the final product that embodiment 3 is prepared.
Specific embodiment
Further description is made to the contents of the present invention combined with specific embodiments below.
In following embodiment:
(1) EDX, EBSD are tested: using the field emission scanning electron microscope of model Hitachi S-4800, test-strips
Part is 5kV acceleration voltage；
(2) XRD is tested: using the X-ray diffractometer of model Rigaku D/MAX-2500, test condition is CuKa spoke
It penetrates, λ=0.15406nm, 40kV operating voltage and 200mA operating current；
(3) hardness test: using the micro Vickers of model FM-700, test condition is pressure 2.4N, protects lotus
Time 15s.
(4) compressive stress strain curve: INSTROM (5985) type hydraulic servo Material Testing Machine is used.
(5) used device when explosion shock wave treatment in the method for the invention, as shown in Figure 1, comprising: pushed up on plastics
Lid 1, polyvinyl chloride (PVC) pipe 2, steel plug 5, plastic feet 6 and momentum block 7 under steel plug 3, sample cell 4, stainless steel on stainless steel.
Wherein 6 center of plastic feet is equipped with circular trough, momentum block 7 is placed in circular trough, the momentum block 7 is piece of stainless steel, for unloading
Fall shock wave, prevent back wave from damaging sample, sample cell 4 is placed on momentum block 7, and sample cell 4 is provided with compacting powder, plastics
6 circumferential direction of pedestal is equipped with pvc pipe 2, and plastics upper top cover 1 is equipped with above pvc pipe 2, and 1 center of plastics upper top cover is equipped with circular hole, circular hole
Priming detonator is put at center, and detonator is located at plastics upper top cover upper center；Pvc pipe 2 and plastic feet 6 pass through glass glue bond one
It rises, explosive is poured into pvc pipe 2 and is filled, is filled and led up, cover plastics upper top cover 1, detonator is inserted into priming top center, and detonate thunder
Pipe carries out explosion shock wave treatment.
Embodiment 1
A kind of preparation method of nanometer of high-entropy alloy block materials, the method comprises the following steps:
Step 1: using high purity metal powder Al, Co, Cr, Fe and Ni as raw material powder:
Al powder: average grain diameter: 25 μm, atomic ratio: 20%, quality: 10.79g, purity: >=99.9%；
Co powder: average grain diameter: 5 μm, atomic ratio: 20%, quality: 23.57g, purity: >=99.9%；
Cr powder: average grain diameter: 25 μm, atomic ratio: 20%, quality: 20.79g, purity: >=99.9%；
Fe powder: average grain diameter: 25 μm, atomic ratio: 20%, quality: 22.33g, purity: >=99.9%；
Ni powder: average grain diameter: 20 μm, atomic ratio: 20%, quality: 23.47g, purity: >=99.9%.
It will be ground 60 hours in the raw material powder in a planetary ball mill argon atmospher of 300rpm.It the use of diameter dimension is 5-
For the stainless steel ball of 20mm as abrasive media, the mass ratio of ball and powder is 10:1.It overheats in order to prevent, the every fortune of process of lapping
10 minutes out of service after row 1 hour, the mixed-powder after obtaining ball milling.
Step 2: mixed-powder is pressed into stainless steel by the way of single shaft compacting (suppressing along an axial force distribution)
Just base, first base consistency (consistency=powder material compacted density/powder density itself) are pressed into the sample cell 4 of matter is
73%.
Step 3: be packed into pvc pipe 2 nitromethane liquid explosives detonation impact sample cell 4 generate TRANSIENT HIGH TEMPERATURE high pressure into
The shock wave synthesis of row high-entropy alloy, detonation velocity 2600m/s recycle sample cell 4.
Step 4: under argon gas protection, it is small that sample cell 4 after impact is heat-treated to 12 in 600 degrees Celsius of vacuum furnace
When, it is cooled to room temperature to it, removes sample cell 4 with wire cutting, obtain a kind of AlCoCrFeNi nanometers of high-entropy alloy block materials.
It is 7.1g/cm with the density that drainage measures final product3, which is the theoretical density of AlCoCrFeNi, final product
Average hardness is 550.7HV, and hardness highest point is up to 770HV, higher than the AlCoCrFeNi's that arc-plasma is sintered preparation
Hardness (518HV).
The XRD result of final product as shown in Fig. 2, final product by two kinds of phase compositions of BCC and FCC, this and the fortune reported at present
High-entropy alloy with the ingredient of electric arc furnaces preparation is consistent.Crystallite dimension is calculated by Scherrer formula, obtains the average crystalline substance of alloy
Particle size is 19nm.
The EDX result of final product as shown in figure 3, by the EDS maps result of each element in final product it is found that Al in final product,
Co, Cr, Fe and Ni Elemental redistribution are highly uniform.
As shown in figure 4, can be seen that from crystallite dimension statistical chart, the crystal grain less than 200nm accounts for about the EBSD result of final product
80%, the crystal grain accounting less than 1 μm is 100%.
Final product is 10-3s-1Strain rate under compressive stress strain curve result it is as shown in Figure 5, the results showed that,
Final product compression strength is up to 1620MPa, breaking strain 0.4, these performance indicators are above at present using arc melting method
The AlCoCrFeNi high-entropy alloy of preparation.
Embodiment 2
A kind of preparation method of nanometer of high-entropy alloy block materials, the method comprises the following steps:
Step 1: using high purity metal powder Al, Co, Cr, Fe and Ni as raw material powder:
Al powder: average grain diameter: 25 μm, atomic ratio: 15.79%, purity: >=99.9%；
Co powder: average grain diameter: 5 μm, atomic ratio: 21.05%, purity: >=99.9%；
Cr powder: average grain diameter: 25 μm, atomic ratio: 21.05%, purity: >=99.9%；
Fe powder: average grain diameter: 25 μm, atomic ratio: 21.05%, purity: >=99.9%；
Ni powder: average grain diameter: 20 μm, atomic ratio: 21.05%, purity: >=99.9%.
It will be ground 70 hours in the raw material powder in a planetary ball mill argon atmospher of 300rpm.It the use of diameter dimension is 5-
For the stainless steel ball of 20mm as abrasive media, the mass ratio of ball and powder is 12:1.It overheats in order to prevent, the every fortune of process of lapping
10 minutes out of service after row 1 hour, the mixed-powder after obtaining ball milling.
Step 2: will be pressed into just base in sample cell 4 that mixed-powder is pressed into stainless steel material by the way of uniaxial compacting,
First base consistency is 73%.
Step 3: be packed into pvc pipe 2 nitromethane liquid explosives detonation impact sample cell 4 generate TRANSIENT HIGH TEMPERATURE high pressure into
The shock wave synthesis of row high-entropy alloy, detonation velocity 3200m/s recycle sample cell 4.
Step 4: being cooled to room temperature to it, sample cell 4 is removed with wire cutting, obtains a kind of AlCoCrFeNi nanometers high entropy
Alloy block material.
It is 5.87g/cm with the density that drainage measures final product3, final product average hardness is 526.7 ± 43HV, highest
Hardness is 880HV, higher than the hardness (518HV) of the AlCoCrFeNi of arc-plasma sintering preparation.
The XRD result of final product is as shown in fig. 6, final product is calculated by two kinds of phase compositions of BCC and FCC by Scherrer formula
Crystallite dimension, the average grain size for obtaining alloy is 23nm.
The EDX result of final product as shown in fig. 7, by the EDS maps result of each element in final product it is found that Al in final product,
Co, Cr, Fe and Ni Elemental redistribution are highly uniform.
As shown in figure 8, can be seen that from crystallite dimension statistical chart, the crystal grain less than 200nm accounts for about the EBSD result of final product
80%, the crystal grain accounting less than 1 μm is 100%.
Final product is 10-3s-1Strain rate under compressive stress strain curve it is as shown in Figure 9, the results showed that, eventually produce
Object compression strength is up to 1502MPa, breaking strain 0.42, these performance indicators are above to be prepared using arc melting method at present
AlCoCrFeNi high-entropy alloy.
Embodiment 3
A kind of preparation method of nanometer of high-entropy alloy block materials, the method comprises the following steps:
Step 1: using high purity metal powder Al, Co, Cr, Fe and Ni as raw material powder:
Al powder: average grain diameter: 25 μm, atomic ratio: 27.27%, purity: >=99.9%；
Co powder: average grain diameter: 5 μm, atomic ratio: 18.18%, purity: >=99.9%；
Cr powder: average grain diameter: 25 μm, atomic ratio: 18.18%, purity: >=99.9%；
Fe powder: average grain diameter: 25 μm, atomic ratio: 18.18%, purity: >=99.9%；
Ni powder: average grain diameter: 20 μm, atomic ratio: 18.18%, purity: >=99.9%.
It will be ground 70 hours in the raw material powder in a planetary ball mill argon atmospher of 300rpm.It the use of diameter dimension is 5-
For the stainless steel ball of 20mm as abrasive media, the mass ratio of ball and powder is 8:1.It overheats in order to prevent, the every fortune of process of lapping
10 minutes out of service after row 1 hour, the mixed-powder after obtaining ball milling.
Step 2: will be pressed into just base in sample cell 4 that mixed-powder is pressed into stainless steel material by the way of uniaxial compacting,
First base consistency is 73%.
Step 3: it is packed into nitromethane liquid explosives detonation impact stainless steel sample pipe 4 in pvc pipe 2 and generates TRANSIENT HIGH TEMPERATURE
High pressure carries out the shock wave synthesis of high-entropy alloy, and detonation velocity 3200m/s recycles sample cell 4.
Step 4: being cooled to room temperature to it, removes sample cell 4 with wire cutting, obtains a kind of AlCoCrFeNi nanometers high entropy
Alloy block material.
It is 7.3g/cm with the density that drainage measures final product3, final product average hardness is 480HV, and maximum hardness is
580HV。
The results are shown in Figure 10 by the XRD of final product, and final product is calculated by two kinds of phase compositions of BCC and FCC by Scherrer formula
Crystallite dimension, the average grain size for obtaining alloy is 26nm.
Final product is 10-3s-1Strain rate under compressive stress strain curve it is as shown in figure 11, the results showed that, eventually produce
The compression strength of object is up to 1450MPa, breaking strain 0.43, these performance indicators are above at present using electric arc melting legal system
Standby AlCoCrFeNi alloy.
In conclusion using the high-entropy alloy block materials even tissue of technology disclosed by the invention preparation and with excellent
Room-temperature mechanical property, also indicate that high-entropy alloy technology of preparing high reliablity disclosed by the invention, present invention firstly discloses adopt
With the method for explosive sintering method synthesis nanometer high-entropy alloy block materials.It is described simple and easy, high reliablity and cost is relatively low,
With industrial applications prospect.
The above is merely preferred embodiments of the present invention, it is not intended to limit the scope of the present invention.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.
Claims (10)
1. the preparation method of a kind of nanometer of high-entropy alloy block materials, it is characterised in that: the method comprises the following steps:
Step 1: by five kinds with the high purity metal powder of first-class atomic ratio or nearly atomic ratio under protective gas atmosphere ball milling
60-70h, rotational speed of ball-mill 250-350rpm, ratio of grinding media to material 8-12:1, the alloy powder after obtaining ball milling；
Step 2: the alloy powder that ball milling mixing is obtained is fitted into sample cell, single shaft compacting, obtaining consistency is 79-90%
Compacting powder；
Step 3: carrying out explosion shock wave treatment, detonation velocity 2300-3500m/s to sample cell；
Step 4: under inert gas protection by the sample cell after shock treatment, 10-12h is heat-treated at 400-600 DEG C, it is cooling
To room temperature, a kind of nanometer of high-entropy alloy block materials are obtained in sample cell；
Wherein, the purity of metal powder described in step 1 is 99.9% or more.
2. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: in step 1
The average grain diameter of the metal powder is 5-60 μm.
3. the preparation method of a kind of nanometer of high-entropy alloy block materials as claimed in claim 1 or 2, it is characterised in that: step
Metal powder described in one is Al powder, Co powder, Cr powder, Fe powder and Ni powder.
4. the preparation method of a kind of nanometer of high-entropy alloy block materials as claimed in claim 1 or 2, it is characterised in that: step
The mole dosage of metal powder described in one is equal.
5. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: in step 1
The protective gas is nitrogen or inert gas.
6. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: in step 3
Explosion shock wave treatment is carried out to sample cell using explosive.
7. the preparation method of a kind of nanometer of high-entropy alloy block materials as claimed in claim 6, it is characterised in that: the explosive
For nitromethane liquid, 8701 explosives or B explosive.
8. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: the sample
Pipe is stainless steel material, wall thickness 2-3mm.
9. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: the sample
The bottom of pipe is equipped with momentum block.
10. the preparation method of a kind of nanometer of high-entropy alloy block materials as described in claim 1, it is characterised in that: described dynamic
Gauge block is piece of stainless steel.
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| CN110438385A (en) * | 2019-09-05 | 2019-11-12 | 青海大学 | A kind of Al-Co-Cr-Ni quaternary high-entropy alloy system and preparation method thereof |
| CN112921228A (en) * | 2021-01-21 | 2021-06-08 | 北京理工大学 | Preparation method of aluminum-nickel-loaded 3D skeleton high-entropy alloy composite energetic fragment |
| CN112961016A (en) * | 2020-12-18 | 2021-06-15 | 北京理工大学 | Preparation method of explosive-loaded 3D skeleton high-entropy alloy composite energetic fragment |
| CN113828779A (en) * | 2021-09-27 | 2021-12-24 | 吉林大学 | Laser repairing method for surface defects of high-entropy alloy prepared by powder metallurgy method |
| CN115213406A (en) * | 2022-06-24 | 2022-10-21 | 中北大学 | Method for preparing refractory high-entropy alloy by explosive loading |
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