CN109182876A - A kind of crystalline state high entropy alloy material containing beryllium and preparation method thereof - Google Patents
A kind of crystalline state high entropy alloy material containing beryllium and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to high-entropy alloy fields, more particularly, to a kind of crystalline state high entropy alloy material containing beryllium and preparation method thereof.It develops the CoCrFeNiBe high-entropy alloy with high specific strength, since beryllium atom size is small, differs larger with other constituent element atomic sizes by addition beryllium element, and it is poor to be conducive to raising alloy atom size；Furthermore the enthalpy of mixing of beryllium and other four kinds of elements has lesser negative value, therefore the high-entropy alloy can largely change the δ of this alloy, lesser degree changes Δ H by the content of micro adjustment beryllium elementmix, therefore relatively significantly change the institutional framework of high-entropy alloy and alloy is made to avoid falling in amorphous alloy region or intermetallic object area, to obtain solid solution phase high-entropy alloy.Additionally due to beryllium lightweight height is than strong performance, so that the hardness of this series high-entropy alloy and slightly also significantly being enhanced, density reduction, to increase the specific strength of alloy.
Description
Technical field
The invention belongs to high-entropy alloy fields, more particularly, to a kind of crystalline state high entropy alloy material containing beryllium and its preparation
Method.
Background technique
Conventional alloys use the design concept based on one or two kinds of elements, obtain single pivot or double pivot alloys.High entropy
Alloy breaks through this design concept, and the element for connecing near atomic ratio by five kinds or five kinds or more forms, therefore high-entropy alloy has
The higher entropy of mixing, biggish distortion of lattice, slow diffusion effect etc., simultaneously because the cocktail effect of high-entropy alloy, it can
The performance regulated and controled as needed changes the proportion of alloying element.
Typical case's high-entropy alloy series reported at present has CoCrFeNi, the high-entropy alloys such as CoCrFeNiAl, MoNbTaW；
There are also using TiZrHfBeCuNi as high entropy amorphous alloy of representative etc..Wherein CoCrFeNi high-entropy alloy is moulded with 60% stretching
Property, intensity only has 200-500MPa；CoCrFeNiAl high-entropy alloy is 1174MPa in the maximum tensile strength, is in Al content
In the case of 11%；It is 0.2% that the most excellent comprehensive mechanical property of CoFeNiVMo high-entropy alloy, which is Mo content, at this time tensile strength
For 686.9MPa；The compression strength of AlCoCuNiSiV can reach 1568MPa in compression test, and CoCrFeNiMnCu high entropy closes
The compression strength of gold is only 750MPa.Although high-entropy alloy has biggish improvement compared to intensity, the hardness etc. of common alloy,
But comprehensive mechanical property is still unable to reach current requirement of the high-grade, precision and advanced field to material property.
Beryllium is a kind of lightweight height than strong metal, the small (1.848g/cm of density-3), bulk modulus (130GPa), modulus of shearing
(132GPa) and Young's modulus (287GPa) will be big than common metal.The addition of beryllium can significantly improve the density, strong of alloy
The important mechanical properties such as degree, hardness and specific strength.Simultaneously as the VEC of beryllium is smaller, differ larger with most of metal, and VEC
(electron concentration) is the important parameter of determining solid solution phase, and as VEC < 6.87, alloy forms single FCC phase, as VEC >=8
Alloy forms single BCC phase, and as 6.87≤VEC < 8, alloy contains FCC and BCC phase simultaneously；Therefore it can pass through the addition tune of beryllium
The phase composition for controlling alloy, to further improve alloy property.
In crystalline state high-entropy alloy reported at present, the example using beryllium element there is no, this is because beryllium atom size phase
Smaller than common metal element, atomic size difference is larger, while larger with the negative heat of mixing value of most of metallic element, is easy to make
Alloy falls in the region of amorphous alloy, such as a kind of high entropy amorphous alloy material disclosed in patent CN103334065A
TiZrHfBeCuNi。
A kind of crystalline state containing beryllium that comprehensive mechanical property is excellent high entropy alloy material how is obtained, and obtains single solid solution phase
Or double solid solution phases, it is a problem to be solved.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of crystalline state high entropy alloy materials containing beryllium
And preparation method thereof, by addition beryllium element, the CoCrFeNiBe high-entropy alloy with high specific strength is developed, due to beryllium original
Sub- size is small, differs larger with other constituent element atomic sizes, and it is poor to be conducive to raising alloy atom size；Furthermore beryllium with other four kinds
The enthalpy of mixing of element has lesser negative value, therefore the high-entropy alloy can be by the content of micro adjustment beryllium element, can larger journey
Degree ground changes the δ of this alloy, and lesser degree changes Δ Hmix, therefore relatively significantly change the institutional framework of high-entropy alloy and make to close
Gold avoids falling in amorphous alloy region or intermetallic object area, to obtain solid solution phase high-entropy alloy.Additionally due to beryllium
Lightweight height is than strong performance, so that the hardness of this series high-entropy alloy and slightly also significantly enhanced, density reduction, from
And increase the specific strength of alloy.Thus the skill that the prior art lacks the excellent crystalline state high entropy alloy material of comprehensive mechanical property is solved
Art problem.
To achieve the above object, according to one aspect of the present invention, the crystalline state high entropy alloy material containing beryllium includes simple substance
Element beryllium, cobalt, chromium, iron and nickel, or the alloying element including simple substance element beryllium Yu cobalt ferrochrome nickel, component atoms percentage group
As (CoCrFeNi)1-xBex, 0 x≤0.225 <.
Preferably, which includes a kind of in body center cubic solid solution, face-centered cubic solid solution or intermetallic compound phase
Or it is a variety of.
Preferably, the specific strength of the alloy is not less than 2.2 × 105Nm/kg, density are not more than 8.205g/cm3, compress and bend
Intensity is taken not less than 167MPa, compressed rupture strength is not less than 1700MPa, and Vickers hardness is not less than 211HV.
Preferably, the crystalline state high entropy alloy material containing beryllium, component atoms percentage group become (CoCrFeNi)0.96Be0.4。
Preferably, the crystalline state high entropy alloy material containing beryllium, component atoms percentage group become (CoCrFeNi)0.915Be0.085。
Preferably, the crystalline state high entropy alloy material containing beryllium, component atoms percentage expression formula are
(CoCrFeNi)0.87Be0.13。
Preferably, the crystalline state high entropy alloy material containing beryllium, component atoms percentage expression formula are
(CoCrFeNi)0.82Be0.18。
Preferably, the crystalline state high entropy alloy material containing beryllium, component atoms percentage expression formula are
(CoCrFeNi)0.775Be0.225。
Other side according to the invention provides a kind of method for preparing crystalline state high entropy alloy material containing beryllium,
Method includes the following steps:
(1) use purity for 99.5% or more block Co, Cr, Fe, Ni and Be metal, it is former according to the ingredient of the alloy
Sub- percentage composition carries out ingredient, obtains metal mixture；
(2) vacuum arc melting furnace molten alloy is used, 3 × 10 are evacuated to furnace chamber-3Pa is hereinafter, be filled with high-purity argon
Gas；
(3) metal mixture described in melting using vacuum spray to cast or inhales casting technology, master alloy is injected copper to uniform state
In mould, the high-entropy alloy bar is obtained.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
(1) the present invention provides a kind of crystalline state high entropy alloy materials containing beryllium, small using beryllium atom size, with other constituent elements original
Sub- size difference is larger, and it is poor to be conducive to raising alloy atom size；The enthalpy of mixing of beryllium and tetra- kinds of elements of CoCrFeNi is utilized simultaneously
With lesser negative value, largely change the δ of this alloy, lesser degree changes Δ Hmix, to relatively significantly change high entropy
The institutional framework of alloy and alloy is made to avoid falling in amorphous alloy region or intermetallic object area, finally obtains solid solution phase
High-entropy alloy.
(2) content of the present invention by micro adjustment beryllium in the alloy, may be implemented it in body center cubic solid solution
(FCC), the transformation between the phases such as face-centered cubic solid solution (BCC) and intermetallic compound.
(3) present invention is obtained higher than strong crystalline state with high intensity, high rigidity, low-density and height by addition beryllium
The specific strength of entropy alloy, the alloy is not less than 2.2 × 105Nm/kg, density are not more than 8.205g/cm3, compression yield strength is not
Lower than 167MPa, compressed rupture strength is not less than 1700MPa, and Vickers hardness is not less than 211HV, and with the increase of beryllium content,
In addition to density decline, other performances are all significantly increased.
Detailed description of the invention
Fig. 1 is alloy phase selecting criterion schematic diagram.
Fig. 2 instantiates (CoCrFeNi)1-xBexThe XRD spectrum of high-entropy alloy.
Fig. 3 instantiates (CoCrFeNi)1-xBexThe SEM image of high-entropy alloy.
Fig. 4 instantiates (CoCrFeNi)1-xBexThe room temperature compressive stress strain curve of high-entropy alloy.
Fig. 5 instantiates (CoCrFeNi)1-xBexThe compression yield strength change trend curve of high-entropy alloy.
Fig. 6 instantiates (CoCrFeNi)1-xBexThe compressed rupture strength change trend curve of high-entropy alloy.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
In general, alloying component is calculated by enthalpy of mixing (Δ Hmix) and atomic size poor (δ) determine, formula are as follows:
N: the constituent element number of alloy；
ci: the atomic fraction of i-th kind of element；
ri: the atomic radius of i-th kind of element；
Alloy average atom radius；
The parameter of i-th kind of element and the interaction of jth kind element.
As shown in Figure 1, only solid solution is formed in the region of S label；S ' is the region of mark, and alloy is still with solid solution
Based on, and for some multi-principal high-entropy alloys, then there is micro ordered solid solution that can be precipitated out；B1And B2It is the two of label
A region is amorphous alloy；And the region that C is label is intermetallic compound.
However, due to beryllium atom size compared to common metal element it is smaller, atomic size difference is larger, at the same with most of gold
The negative heat of mixing value for belonging to element is larger, is easy the region for making alloy fall in amorphous alloy according to above-mentioned conventional criterion thinking.
Unexpectedly, present invention discover that alloy is made in beryllium and other four kinds of element-specifics Co, Cr, Fe, Ni, match in certain
Than can avoid forming amorphous alloy, obtaining the high-entropy alloy of complete crystalline state under composition.The present invention is by the way that especially selection can be with beryllium
Element compounds to form alloy, and the metallic element small with the negative heat of mixing value of beryllium combines, and sufficiently combines beryllium element atomic size small
Characteristic so that alloy successfully falls into the region of crystal alloy.Be Elements Atom size is small, and hardness is high, and density is small, plays regulation
The effect of alloy microstructure and mechanical property.By finely tuning beryllium content, which can be realized from body center cubic solid solution
(FCC), the transformation between the phases such as face-centered cubic solid solution (BCC) and intermetallic compound.In addition, since beryllium lightweight height is than strong
Performance, so that the hardness of this series high-entropy alloy and slightly also significantly being enhanced, density reduction, to increase alloy
Specific strength.
The invention proposes high-entropy alloy containing beryllium and preparation method thereof, (CoCrFeNi)1-xBexFor alloy of the invention at
Point, it is made of simple substance element beryllium, cobalt, chromium, iron and nickel, or be made of simple substance element beryllium and the alloying element of cobalt ferrochrome nickel.
It can be containing on a small quantity by bring impurity in raw metal in practical alloy material.Preparation method be using vacuum arc melting,
When vacuum degree reaches 3 × 10-3After Pa, it is filled with high-purity argon gas；It by purity is 99.5% or more, such as 99.99% by electric arc
Pure metal melting is uniform, obtains master alloy ingot；Using vacuum spray to cast or casting machine is inhaled, alloy is injected in copper mold, high entropy is obtained
Alloy bar material or sheet material.Because of addition beryllium element, the high-entropy alloy of acquisition has high than excellent mechanicals such as strong, high rigidity the present invention
Performance, while structure easy-regulating.
The following are embodiments:
1, the preparation of multi-principal high-entropy alloy
(1) raw material preparation
Raw material used in the present invention is not less than 99.5% pure Co, Cr, Fe, Ni for purity, and Be metal passes through atom hundred
Divide than being matched after calculating mass percent, the ingredient of distributing precision 0.001g, each alloy are shown in Table 1.
Table 1 (CoCrFeNi)1-xBexHigh-entropy alloy component list (at.%)
(2) melting and casting
The present invention uses vacuum arc melting method molten alloy.Raw material is placed in water jacketed copper crucible, furnace chamber is taken out true
Sky is to 3 × 10-3After Pa, high-purity argon gas is filled with to half of atmospheric pressure.It first uses the pure titanium of electric arc melting about 1 minute, to remove furnace chamber
The oxygen of middle remnants.Molten alloy opens electromagnetic agitation assisted melting, so that alloy melting is more equal to fully liquid state later
Even, this process is repeated 6 times, by alloy turn-over before repeating every time.After melting, using copper mold spray to cast or the method cast is inhaled, it will
Alloy injects in copper mold, bar needed for obtaining.
2, the institutional framework and performance of alloy
(1) XRD and crystal species analysis
The small pieces with a thickness of 1mm are cut from alloy bar material using diamond custting machine, sanding and polishing processing is carried out to it.
Crystal species analysis is carried out to sample using X-ray diffractometer, scanning angle range is 20 ° to 90 °, and sweep speed is 8 °/min.
Fig. 2 is (CoCrFeNi)1-xBexThe XRD test result of high-entropy alloy.
The results show that (CoCrFeNi)0.96Be0.04For single-phase body-centered cubic (FCC), with the increase of beryllium content, the center of area is vertical
Side (BCC) occurs when identical, after skin content reaches 18%, while intermetallic compound occurs, it is seen that the addition of beryllium is to height
The structure of entropy alloy has apparent regulating and controlling effect.
(2) microstructure observation
Fig. 3 is (CoCrFeNi)1-xBexSEM image wherein (a) (b) represents the high-entropy alloy of x=0.04 (c) be x
=0.085 high-entropy alloy, (d) high-entropy alloy for being x=0.13, (e) high-entropy alloy for being x=0.18, (f) is x=0.225
High-entropy alloy.When Be constituent content is 0.04, (CoCrFeNi)0.96Be0.04High-entropy alloy is homogeneous structure, in conjunction with front
XRD analysis and the calculated results, it should be FCC homogeneous structure, therefore, the crystal grain in SEM spectrum is not apparent；
When Be constituent content is 0.085, (CoCrFeNi)0.915Be0.085High-entropy alloy has Second Phase Precipitation, with Be
The crystal grain of the increase of constituent content, the second phase of precipitation is gradually grown up, is increased, and the second alternate crystal grain is interconnected to form
Apparent big crystal grain；
When Be constituent content is 0.18, there are three types of crystal grain in figure (e), thus judge (CoCrFeNi)0.82Be0.18High entropy
Third phase has been precipitated in alloy, analyzes in conjunction with calculated result, this cenotype may be intermetallic compound, the analysis phase with XRD spectrum
Unanimously.With the increase of Be constituent content, content of the third phase in high-entropy alloy is gradually increased, and along with the length of crystal grain
Greatly；
When Be constituent content is 0.225, (CoCrFeNi)0.775Be0.225Crystal grain in high-entropy alloy still there are three types of,
It can be seen that nascent FCC phase crystal grain still has, only its content is greatly reduced compared with preceding, and the third phase being newly precipitated
Crystal grain still have.
This result is consistent with above-mentioned XRD result.
(3) quasistatic compression is tested
It is cut from high-entropy alloy stick obtainedCompression sample, both ends polishing is parallel, in Zwick ten thousand
Room temperature compression experiment can be carried out on electronic material testing machine, compression speed is 1 × 10-3s-1, every kind of ingredient is repeated 3 times the above reality
It tests.Fig. 4 is (CoCrFeNi)1-xBexThe load-deformation curve of high-entropy alloy room temperature compression experiment, Fig. 5 and Fig. 6 are respectively
(CoCrFeNi)1-xBexThe variation tendency of high-entropy alloy room temperature compression yield strength and breaking strength.As it can be seen that with beryllium content
Increase, (CoCrFeNi)1-xBexThe yield strength and breaking strength of high-entropy alloy all increase considerably.When only adding 4% beryllium
When, the yield strength of alloy improves one times compared with the yield strength of CoCrFeNi alloy, and high-entropy alloy still has at this time
Very good temperature-room type plasticity (50%).
(4) high-entropy alloy Density Detection and specific strength calculate
(CoCrFeNi) is measured using drainage1-xBexThe density of high-entropy alloy；High entropy is measured using Vickers to close
The hardness of gold；According to compression test as a result, calculating the specific strength of alloy using the ratio of breaking strength and density, each property is appealed
Energy numerical value is as shown in table 2.It can be seen that the hardness and specific strength of high-entropy alloy all increase considerably, density with the increase of beryllium content
It is sequentially reduced.
Table 2 (CoCrFeNi)1-xBexDensity, hardness and the specific strength of high-entropy alloy
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of crystalline state high entropy alloy material containing beryllium, which is characterized in that the crystalline state high entropy alloy material containing beryllium includes simple substance member
Plain beryllium, cobalt, chromium, iron and nickel, or the alloying element including simple substance element beryllium Yu cobalt ferrochrome nickel, component atoms percentage composition
For (CoCrFeNi)1-xBex, 0 x≤0.225 <.
2. crystalline state high entropy alloy material containing beryllium as described in claim 1, which is characterized in that the alloy is dissolved comprising body-centered cubic
It is one or more in body, face-centered cubic solid solution or intermetallic compound phase.
3. crystalline state high entropy alloy material containing beryllium as described in claim 1, which is characterized in that the specific strength of the alloy is not less than
2.2×105Nm/kg, density are not more than 8.205g/cm3, for compression yield strength not less than 167MPa, compressed rupture strength is not low
In 1700MPa, Vickers hardness is not less than 211HV.
4. crystalline state high entropy alloy material containing beryllium as described in claim 1, component atoms percentage group becomes
(CoCrFeNi)0.96Be0.4。
5. crystalline state high entropy alloy material containing beryllium as described in claim 1, component atoms percentage group becomes
(CoCrFeNi)0.915Be0.085。
6. crystalline state high entropy alloy material containing beryllium as described in claim 1, component atoms percentage expression formula are
(CoCrFeNi)0.87Be0.13。
7. crystalline state high entropy alloy material containing beryllium as described in claim 1, component atoms percentage expression formula are
(CoCrFeNi)0.82Be0.18。
8. crystalline state high entropy alloy material containing beryllium as described in claim 1, component atoms percentage expression formula are
(CoCrFeNi)0.775Be0.225。
9. a kind of method for preparing any crystalline state high-entropy alloy containing beryllium in claim 1 to claim 8, this method
The following steps are included:
(1) use purity for 99.5% or more block Co, Cr, Fe, Ni and Be metal, according to the component atoms of the alloy
Percentage composition carries out ingredient, obtains metal mixture；
(2) vacuum arc melting furnace molten alloy is used, 3 × 10 are evacuated to furnace chamber-3Pa is hereinafter, be filled with high-purity argon gas；
(3) metal mixture described in melting using vacuum spray to cast or inhales casting technology, master alloy is injected copper mold to uniform state
In, obtain the high-entropy alloy bar.
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| CN110899712A (en) * | 2019-12-18 | 2020-03-24 | 长沙新材料产业研究院有限公司 | Aluminum-iron-containing high-entropy alloy suitable for additive manufacturing and modification method thereof |
| CN111254316A (en) * | 2020-04-01 | 2020-06-09 | 山东理工大学 | (MoNbZrTi) high-entropy alloy reinforced Ni-based alloy and preparation method thereof |
| CN115821145A (en) * | 2022-11-18 | 2023-03-21 | 华中科技大学 | High-strength high-plasticity multiphase high-entropy alloy material and preparation method thereof |
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| CN102776430A (en) * | 2012-08-20 | 2012-11-14 | 太原理工大学 | AlCoCrFeNiTix high-entropy alloy material and method for preparing same |
| CN105506613A (en) * | 2016-02-02 | 2016-04-20 | 济南大学 | Preparation method for high-entropy alloy coating |
| CN106756647A (en) * | 2016-12-12 | 2017-05-31 | 北京科技大学 | A kind of high-ductility zirconium-based bulk amorphous alloy without nickel and preparation method thereof without beryllium |
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| CN102766797A (en) * | 2011-05-04 | 2012-11-07 | 中国科学院金属研究所 | Multi-principal-element alloy |
| CN102776430A (en) * | 2012-08-20 | 2012-11-14 | 太原理工大学 | AlCoCrFeNiTix high-entropy alloy material and method for preparing same |
| CN105506613A (en) * | 2016-02-02 | 2016-04-20 | 济南大学 | Preparation method for high-entropy alloy coating |
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| CN110899712A (en) * | 2019-12-18 | 2020-03-24 | 长沙新材料产业研究院有限公司 | Aluminum-iron-containing high-entropy alloy suitable for additive manufacturing and modification method thereof |
| CN111254316A (en) * | 2020-04-01 | 2020-06-09 | 山东理工大学 | (MoNbZrTi) high-entropy alloy reinforced Ni-based alloy and preparation method thereof |
| CN115821145A (en) * | 2022-11-18 | 2023-03-21 | 华中科技大学 | High-strength high-plasticity multiphase high-entropy alloy material and preparation method thereof |
| CN115821145B (en) * | 2022-11-18 | 2023-11-28 | 华中科技大学 | High-strength high-plasticity multiphase high-entropy alloy material and preparation method thereof |
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