CN114657480B - Zr-based amorphous alloy with high plastic phase separation and preparation method and application thereof - Google Patents

Zr-based amorphous alloy with high plastic phase separation and preparation method and application thereof Download PDF

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CN114657480B
CN114657480B CN202210311818.XA CN202210311818A CN114657480B CN 114657480 B CN114657480 B CN 114657480B CN 202210311818 A CN202210311818 A CN 202210311818A CN 114657480 B CN114657480 B CN 114657480B
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吴渊
张英杰
夏洋
王辉
刘雄军
蒋虽合
吕昭平
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University of Science and Technology Beijing USTB
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    • C22C45/00—Amorphous alloys
    • C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
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Abstract

The invention belongs to the field of bulk amorphous alloy, and relates to a high-plasticity phase separation Zr-based amorphous alloy, a preparation method and application thereof, wherein the amorphous alloy comprises component atomsThe percentage expression is: zr (Zr) a Cu b M c Al d Wherein a is more than or equal to 55 and less than or equal to 60,5, b is more than or equal to 35,5, c is more than or equal to 35,5 and d is more than or equal to 8, and a+b+c+d=100 is required to be satisfied; m is one or more of Ni, fe and Co (can be in any proportion); the block Zr-based amorphous alloy with the diameter not less than 2mm can be prepared by an arc melting and copper mold suction casting method. The beneficial effects of the invention are as follows: as the positive mixing enthalpy component is introduced into the Zr-based amorphous alloy, the structural non-uniformity of the as-cast structure of the alloy system can be increased by utilizing the mutual repulsive interaction between immiscible components, so that the room temperature plasticity of the alloy system is obviously improved, and the compression plasticity of the alloy system is not lower than 10%.

Description

Zr-based amorphous alloy with high plastic phase separation and preparation method and application thereof
Technical Field
The invention belongs to the field of bulk amorphous alloys, and particularly relates to a high-plasticity phase separation Zr-based amorphous alloy, and a preparation method and application thereof.
Technical Field
Unlike crystalline metals, which undergo plastic deformation by dislocation or twinning deformation mechanisms, room temperature plastic deformation of amorphous alloys is mainly performed by highly localized shearing, and after yielding of the material, plastic deformation is mainly concentrated in a limited number of shear bands with an initial thickness of only tens of nanometers, cannot withstand subsequent loading, and often exhibits catastrophic brittle fracture characteristics. Even though a few amorphous alloy systems exhibit some plastic deformation capability under compressive loading, shear softening occurs due to a sharp decrease in viscosity near the localized shear band, and the same work hardening capability as crystalline metallic materials, i.e., the property of work softening in true stress-strain curves, is not exhibited. Therefore, the phenomena of room-temperature brittleness and strain softening become the 'Acrylonitrile heel' of the amorphous alloy, and the excellent mechanical properties such as high strength, high fracture toughness and the like cannot be reflected in the actual service process, so that the engineering popularization and application of the amorphous alloy as a structural material are greatly limited.
The amorphous alloy effectively blocks the rapid expansion of a single shearing band in the deformation process by adjusting the intrinsic characteristics such as the elastic constant or the heterogeneous structure of a plurality of scales (nano-scale to micron-scale), so as to promote the initiation, proliferation and mutual intersection of the shearing bands, improve the number of the shearing bands in the amorphous alloy, reduce the localization degree of heterogeneous deformation, and be a main means for toughening and plasticizing the single-phase amorphous alloy at present. Research shows that by introducing components with positive mixing enthalpy, utilizing mutual repulsion among immiscible components with positive mixing enthalpy and combining component adjustment and cooling rate control, amorphous alloy with different scale structure non-uniformity can be obtained by solidification, and large room temperature plasticity is realized.
Disclosure of Invention
The invention discloses a high-plasticity phase separation Zr-based amorphous alloy and a preparation method and application thereof, which are used for solving any one of the above and other potential problems in the prior art. In order to solve the problems, the technical scheme of the invention is as follows: the Zr-based amorphous alloy is characterized in that a Cu element in the Zr-based amorphous alloy is introduced into a non-miscible component with positive mixing enthalpy, and the structural non-uniformity of a Zr-based amorphous as-cast structure is increased by utilizing the mutual repulsive interaction between the non-miscible components, so that the room temperature plasticity of the amorphous alloy is improved;
the compression plasticity of the Zr-based amorphous alloy is not less than 10%, and the critical dimension is not less than 2mm.
Further, the amorphous alloy has the following atomic percent expression: zr (Zr) a Cu b M c Al d Wherein a is more than or equal to 55 and less than or equal to 60,5, b is more than or equal to 35,5, c is more than or equal to 35,5 and d is more than or equal to 8, and a+b+c+d=100 is required to be satisfied; m is one or more of Ni, fe and Co.
Further, when M is Ni, a=57, b=20, c=15, and d=8, the expression of the alloy is Zr 57 Cu 20 Ni 15 Al 8 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed bulk amorphous can reach 2mm, and the compression molding property can reach 20%。
Further, when M is Ni, a=60, b=20, c=15, and d=5, the expression of the alloy is Zr 60 Cu 20 Ni 15 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 20%.
Further, when M is Fe, a=60, b=20, c=15, and d=5, the expression of the alloy is Zr 60 Cu 20 Fe 15 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 2mm, and the compression molding performance can reach 10%.
Further, when M is Ni and Fe and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 10 Fe 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 15%.
Further, when M is Ni and Co and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 10 Co 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the amorphous block can reach 2mm, and the compression molding performance can reach 10%.
Further, when M is Ni, fe, and Co, and the atomic ratio is 1:1:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 5 Fe 5 Co 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 10%.
Another object of the present invention is to provide a method for preparing the above-mentioned high-plasticity phase separation Zr amorphous alloy, which specifically comprises the following steps:
step one: according to the designed expression components and proportion, selecting pure metal raw materials with purity more than 99.9 percent for standby; step two: smelting the metal raw material weighed in the first step uniformly in an arc furnace protected by Ti oxygen absorption and inert gas, and cooling to obtain a required master alloy cast ingot;
step three: melting the master alloy cast ingot prepared in the second step to obtain a master alloy melt, and sucking the master alloy melt into water-cooled copper dies with different apertures to obtain a pure amorphous block alloy;
the pore size is not greater than the critical size of the corresponding component.
The high-plasticity phase separation Zr-based amorphous alloy is applied to the fields of biological materials, mobile equipment, sports goods and medical appliances.
The beneficial effects of the invention are as follows: the series of block amorphous alloys provided by the invention have a large formation component range and wide preparation conditions;
the alloy system can prepare a block amorphous with the diameter of more than 2mm, and can improve the room temperature plasticity of the amorphous alloy while keeping the inherent attribute of the amorphous alloy;
the bulk amorphous with different scale non-uniformity can be obtained through the adjustment of the alloy components and the cooling speed, so that different mechanical properties can be regulated and obtained.
The main component of the block amorphous alloy provided by the invention is common pure metal element, has low price, is convenient to prepare, has no Ni or Be as part of components, and has wide application prospect.
Drawings
FIG. 1 is an XRD pattern of a 2mm sample of a bulk amorphous alloy of Zr-Cu-Ni-Al system prepared in example 1 of the present invention;
FIG. 2 is an XRD pattern of a 3mm sample of a bulk amorphous alloy of Zr-Cu-Ni-Al system prepared in example 1 of the present invention;
FIG. 3 Zr prepared in example 1 of the present invention 60 Cu 20 Ni 15 Al 5 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
FIG. 4 Zr prepared in example 1 of the present invention 57 Cu 20 Ni 15 Al 8 XRD pattern of amorphous alloy 2mm sample;
FIG. 5 Zr prepared in example 1 of the present invention 57 Cu 20 Ni 15 Al 8 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
FIG. 6 Zr prepared in example 2 of the present invention 60 Cu 20 Fe 15 Al 5 XRD pattern of amorphous alloy 2mm sample;
FIG. 7 Zr prepared in example 2 of the present invention 60 Cu 20 Fe 15 Al 5 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
FIG. 8 Zr prepared in example 3 of the present invention 60 Cu 20 Ni 14 Fe 1 Al 5 XRD pattern of amorphous alloy 2mm sample;
FIG. 9 Zr prepared in example 3 according to the invention 60 Cu 20 Ni 14 Fe 1 Al 5 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
FIG. 10 Zr prepared in example 3 of the present invention 60 Cu 20 Ni 10 Fe 5 Al 5 XRD pattern of amorphous alloy 3mm sample;
FIG. 11 Zr prepared in example 3 of the present invention 60 Cu 20 Ni 10 Fe 5 Al 5 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
FIG. 12 Zr prepared in example 4 of the present invention 60 Cu 20 Ni 5 Fe 5 Co 5 Al 5 XRD pattern of amorphous alloy 3mm sample;
FIG. 13 Zr prepared in example 4 of the present invention 60 Cu 20 Ni 5 Fe 5 Co 5 Al 5 A compressive stress strain curve of a 2mm sample of the amorphous alloy;
Detailed Description
The technical scheme of the invention is further described below with reference to specific implementation examples. According to the high-plasticity phase separation Zr-based amorphous alloy, the structural non-uniformity of an as-cast structure of the Zr-based amorphous alloy is increased by introducing the immiscible components which are positively mixed with Cu element in the Zr-based amorphous alloy and utilizing the mutual repulsive interaction between the immiscible components, so that the room temperature plasticity of the amorphous alloy is improved;
the compression plasticity of the Zr-based amorphous alloy is not less than 10%, and the critical dimension is not less than 2mm.
The amorphous alloy comprises the following components in atomic percent: zr (Zr) a Cu b M c Al d Wherein a is more than or equal to 55 and less than or equal to 60,5, b is more than or equal to 35,5 and c is more than or equal to 5535,5 d is less than or equal to 8, and a+b+c+d=100 needs to be satisfied; m is one or more of Ni, fe and Co.
When M is Ni, a=57, b=20, c=15 and d=8, the alloy has the expression Zr 57 Cu 20 Ni 15 Al 8 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed bulk amorphous can reach 2mm, and the compression molding property can reach 20%.
When M is Ni, a=60, b=20, c=15 and d=5, the alloy has the expression Zr 60 Cu 20 Ni 15 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 20%.
When M is Fe, a=60, b=20, c=15 and d=5, the alloy has the expression Zr 60 Cu 20 Fe 15 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 2mm, and the compression molding performance can reach 10%.
When M is Ni and Fe and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 10 Fe 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 15%.
When M is Ni and Co and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 10 Co 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 2mm, and the compression molding performance can reach 10%.
When M is Ni, fe, and Co and the atomic ratio is 1:1:1, a=60, b=20, c=15, d=5, the expression of the alloy is Zr 60 Cu 20 Ni 5 Fe 5 Co 5 Al 5 The method comprises the steps of carrying out a first treatment on the surface of the The critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 10%.
The method for preparing the high-plasticity phase separation Zr amorphous alloy specifically comprises the following steps:
step one: according to the designed expression components and proportion, selecting pure metal raw materials with purity more than 99.9 percent for standby;
step two: smelting the metal raw material weighed in the first step uniformly in an arc furnace protected by Ti oxygen absorption and inert gas, and cooling to obtain a required master alloy cast ingot; step three: and (3) melting the master alloy cast ingot prepared in the step two to obtain a master alloy melt, and sucking the master alloy melt into water-cooled copper dies with different apertures to obtain the pure amorphous block alloy.
The pore size is not greater than the critical size of the corresponding component. The high-plasticity phase separation Zr-based amorphous alloy is applied to the fields of biological materials, mobile equipment, sports goods and medical appliances.
Example 1: preparation and performance of Zr-Cu-Ni-Al series block amorphous alloy
Design Zr 60 Cu a Ni b Al 5 Amorphous alloy composition, wherein a = 5,10,15,20,25,30; b=35-a. The obtained component is Zr 60 Cu 5 Ni 30 Al 5 、Zr 60 Cu 10 Ni 25 Al 5 、Zr 60 Cu 15 Ni 20 Al 5 、Zr 60 Cu 20 Ni 15 Al 5 、Zr 60 Cu 25 Ni 10 Al 5 And Zr (Zr) 60 Cu 30 Ni 5 Al 5 Is a metal alloy.
Zr as shown in FIG. 1 and FIG. 2 respectively 60 Cu 5 Ni 30 Al 5 、Zr 60 Cu 10 Ni 25 Al 5 、Zr 60 Cu 15 Ni 20 Al 5 、Zr 60 Cu 20 Ni 15 Al 5 、Zr 60 Cu 25 Ni 10 Al 5 And Zr (Zr) 60 Cu 30 Ni 5 Al 5 X-ray diffraction (XRD) patterns of 2mm and 3mm samples of the alloy show that all components can form a single amorphous sample with the diameter of 2mm, and most components can form a single amorphous sample with the diameter of 3 mm.
Zr 60 Cu 20 Ni 15 Al 5 The compressive stress strain curve of the alloy 2mm specimen is shown in figure 3. It can be seen that the alloy does not break catastrophically immediately after reaching the yield strength, but rather is subjected to a process ofThe plastic deformation of the block amorphous alloy is more than 20%, which shows that the block amorphous alloy has good plastic deformation capability.
Design Zr 57 Cu 20 Ni 15 Al 8 Amorphous alloy composition. As shown in fig. 4, an X-ray diffraction (XRD) pattern of a 2mm sample thereof indicates that the composition can form a single amorphous sample having a diameter of 2mm. The compressive stress strain curve of the alloy 2mm specimen is shown as 5, and the plastic deformation capacity of the alloy can reach 20%.
Example 2: preparation and performance of Zr-Cu-Fe-Al series block amorphous alloy
Design Zr 60 Cu 20 Fe 15 Al 5 Amorphous alloy composition. As shown in fig. 6, an X-ray diffraction (XRD) pattern of a 2mm sample thereof indicates that the composition can form a single amorphous sample having a diameter of 2mm. The compressive stress strain curve of the alloy 2mm specimen is shown as 7, and the plastic deformation capacity of the alloy can be seen to reach 10%.
Example 3: preparation and performance of Zr-Cu-Ni-Fe-Al series block amorphous alloy
Design Zr 60 Cu 20 Ni 14 Fe 1 Al 5 Amorphous alloy composition. As shown in fig. 8, an X-ray diffraction (XRD) pattern of a 2mm sample thereof indicates that the composition can form a single amorphous sample having a diameter of 2mm. The compressive stress strain curve of the alloy 2mm specimen is shown as 9, and the plastic deformation capacity of the alloy can be seen to reach 10%.
Design Zr 60 Cu 20 Ni 10 Fe 5 Al 5 Amorphous alloy composition. The X-ray diffraction (XRD) pattern of a 3mm sample thereof is shown in fig. 10, which shows that the composition can form a single amorphous sample having a diameter of 3 mm. The compressive stress strain curve of the alloy 2mm specimen is shown as 11, and the plastic deformation capacity of the alloy can reach 15%.
Example 4: preparation and performance of Zr-Cu-Ni-Fe-Co-Al series block amorphous alloy
Design Zr 60 Cu 20 Ni 5 Fe 5 Co 5 Al 5 Amorphous alloy composition. As shown in FIG. 12, an X-ray diffraction (XRD) pattern of a 3mm sample thereof is shownSpectrum, spectrum shows that the component can form a single amorphous sample with the diameter of 3 mm. The compressive stress strain curve of the 2mm sample of the alloy is shown as 13, and the plastic deformation capacity of the alloy can be seen to reach 10%.
The enthalpy of mixing refers to the change in enthalpy, which is one basis reflecting whether a chemical reaction is endothermic and exothermic, and if the enthalpy changes positive, it indicates that the chemical reaction is endothermic, and if the enthalpy changes negative, it indicates that the chemical reaction is exothermic, the enthalpy is defined as h=u+pv, and the enthalpy of mixing is positive, i.e. (Δh) min >0)。
The Zr-based amorphous alloy with high plastic phase separation provided by the embodiment of the application and the preparation method and application thereof are described in detail. The above description of embodiments is only for aiding in understanding the method of the present application and its core ideas; meanwhile, as those skilled in the art will have modifications in the specific embodiments and application scope in accordance with the ideas of the present application, the present description should not be construed as limiting the present application in view of the above.
Certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will appreciate that a hardware manufacturer may refer to the same component by different names. The description and claims do not take the form of an element differentiated by name, but rather by functionality. As referred to throughout the specification and claims, the terms "comprising," including, "and" includes "are intended to be interpreted as" including/comprising, but not limited to. By "substantially" is meant that within an acceptable error range, a person skilled in the art is able to solve the technical problem within a certain error range, substantially achieving the technical effect. The description hereinafter sets forth the preferred embodiment for carrying out the present application, but is not intended to limit the scope of the present application in general, for the purpose of illustrating the general principles of the present application. The scope of the present application is defined by the appended claims.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a product or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such product or system. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a commodity or system comprising such elements.
It should be understood that the term "and/or" as used herein is merely one relationship describing the association of the associated objects, meaning that there may be three relationships, e.g., a and/or B, may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
While the foregoing description illustrates and describes the preferred embodiments of the present application, it is to be understood that this application is not limited to the forms disclosed herein, but is not to be construed as an exclusive use of other embodiments, and is capable of many other combinations, modifications and environments, and adaptations within the scope of the teachings described herein, through the foregoing teachings or through the knowledge or skills of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the present invention are intended to be within the scope of the appended claims.

Claims (3)

1. The Zr-based amorphous alloy is characterized in that the Zr-based amorphous alloy is introduced into a difficult-to-mix component with positive mixing enthalpy with Cu element in the Zr-based amorphous alloy, and the structural non-uniformity of an as-cast structure of the Zr-based amorphous alloy is increased by utilizing the mutual repulsive interaction between the difficult-to-mix component, so that the room temperature plasticity of the amorphous alloy is improved;
the compression plasticity of the Zr-based amorphous alloy is not less than 10%, and the critical dimension is not less than 2mm;
the amorphous alloy comprises the following components in atomic percent: zrCuMAl, wherein a= 60,5 is equal to or less than b is equal to or less than 35,5 is equal to or less than 35, d=5, and a+b+c+d=100 is required to be satisfied; m is one or more of Ni, fe and Co;
when M is Fe, a=60, b=20, c=15 and d=5, the expression of the alloy is zrcufenal; the critical dimension of the formed block amorphous can reach 2mm, and the compression molding performance can reach 10%;
when M is Ni and Fe, and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is zrccunifeal; the critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 15%;
when M is Ni and Co and the atomic ratio is 2:1, a=60, b=20, c=15, d=5, the expression of the alloy is zrccunicoal; the critical dimension of the formed block amorphous can reach 2mm, and the compression molding performance can reach 10%;
when M is Ni, fe and Co and the atomic ratio is 1:1:1, a=60, b=20, c=15, d=5, the expression of the alloy is zrccunifecoal; the critical dimension of the formed block amorphous can reach 3mm, and the compression molding performance can reach 10%.
2. A method for preparing the high plasticity phase separation Zr amorphous alloy as claimed in claim 1, wherein said method specifically comprises the steps of:
step one: according to the designed expression components and proportion, selecting pure metal raw materials with purity more than 99.9 percent for standby;
step two: smelting the metal raw material weighed in the first step uniformly in an arc furnace protected by Ti oxygen absorption and inert gas, and cooling to obtain a required master alloy cast ingot;
step three: melting the master alloy cast ingot prepared in the second step to obtain a master alloy melt, and sucking the master alloy melt into water-cooled copper dies with different apertures to obtain a pure amorphous block alloy; the pore size is not greater than the critical size of the corresponding component.
3. A method for preparing a high plasticity phase separation Zr-based amorphous alloy for biological materials, mobile equipment, sports goods and medical appliances according to claim 1.
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