CN108265238B - Zirconium-based metallic glass endogenetic composite material and tissue thinning method thereof - Google Patents
Zirconium-based metallic glass endogenetic composite material and tissue thinning method thereof Download PDFInfo
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Abstract
The invention discloses a zirconium-based metallic glass endogenetic composite material and a tissue thinning method thereof. The zirconium-based metal composite material comprises the following components in atomic percentage: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 15, c is more than or equal to 5 and less than or equal to 20, d is more than or equal to 2 and less than or equal to 12, e is more than or equal to 5 and less than or equal to 23, f is more than or equal to 5 and less than or equal to 15, g is more than or equal to 0.5 and less than or equal to. According to the invention, according to the principle of heterogeneous nucleation of precipitated phases, the heat of mixing of Sn element and BMG alloy element is firstly calculated, and the result shows that the Sn element is added into the Zr-Ti-Cu-Ni-Be-Nb alloy system, and only Zr is formed in the alloy5Sn3Nanoparticles of and Zr5Sn3Melting Point 1988 ℃, beta-Zr (Ti) melting Point 1856 ℃, Zr5Sn3Precipitating before beta-Zr (Ti), and calculating Zr5Sn3And Zr5Sn3Degree of mismatch of (2), finding Zr5Sn3Can be used as an effective heterogeneous nucleation core of the beta-Zr phase, so that the beta-Zr (Ti) phase precipitated firstly in the solidification process of the alloy is Zr5Sn3Separating out and growing up as a core; on the basis of ensuring the forming capability of the bulk metallic glass, Sn element is added to form a beta-Zr phase heterogeneous nucleation core, and the phase morphology is firstly separated out through heterogeneous nucleation refining to obtain a fine and uniform organizational structure.
Description
Technical Field
The invention belongs to the technology of metal-based composite materials, and particularly relates to a zirconium-based metal glass endogenetic composite material and a tissue refining method thereof.
Background
Bulk Metallic Glass (BMG) materials, while having high fracture strength and hardness and high elastic strain limit, suffer catastrophic brittle fracture without macroscopic plastic deformation at room temperature since the plastic deformation of single-phase metallic glass is achieved by highly localized shear deformation, the number of shear bands that can be actuated before fracture is quite limited. Therefore, the room temperature brittleness problem has developed into an important bottleneck for the application of BMG materials.
In order to improve the room temperature brittleness of the BMG material, the Johnson research group in 2000 USA firstly prepares a micrometer-sized beta-Zr (Ti) solid solution phase plasticized BMG composite material by adding Nb alloying elements into a Zr-Ti-Cu-Ni-Be alloy system, and the tensile plastic strain of the BMG composite material reaches 3%. Then, a large amount of researches realize fine homogenization on dendritic crystal beta-Zr (Ti) phase solid solution by adjusting the cooling rate, obtain a uniform and fine second phase structure and optimize the performance.
Although the as-cast endogenous solid solution plasticized BMG composite material adopts a method for increasing the solidification cooling rate to obtain a uniform and fine second phase structure, the method is easily limited by equipment conditions, and the cooling conditions often cannot meet the requirement for obtaining an ideal structure.
Disclosure of Invention
The invention aims to provide a zirconium-based metallic glass endogenetic composite material and a tissue thinning method thereof. The composite material is structurally characterized in that BMG is used as a matrix, and an as-cast beta-Zr (Ti) phase is used as a second phase. According to the principle of precipitation phase heterogeneous nucleation, firstly, the heat of mixing Sn element and BMG alloy element is calculated, and the Zr-Ti-Cu-Ni-Be-Nb alloy system is found to Be added with Sn element, only Zr is formed in the alloy5Sn3Nanoparticles of and Zr5Sn3Melting Point 1988 ℃, beta-Zr (Ti) melting Point 1856 ℃, Zr5Sn3Precipitating before beta-Zr (Ti), and calculating Zr5Sn3And Zr5Sn3Degree of mismatch of (2), finding Zr5Sn3Can be taken as beta-ZThe heterogeneous nucleation core of the r phase realizes the refinement of the second phase on the basis of not influencing the amorphous forming capability of the matrix, and the composite material with fine and uniform tissue is obtained.
The technical solution for realizing the purpose of the invention is as follows: the endogenetic composite material of a kind of zirconium base metallic glass, its alloy element atom percentage expression is: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 15, c is more than or equal to 5 and less than or equal to 20, d is more than or equal to 2 and less than or equal to 12, e is more than or equal to 5 and less than or equal to 23, f is more than or equal to 5 and less than or equal to 15, g is more than or equal to 0.5 and less than or equal to 2, and a + b + c + d + e + f + g = 100.
A method for preparing the zirconium-based metallic glass endogenetic composite material comprises the following steps:
the first step is as follows: selecting a block metal glass alloy system, and adjusting the alloy components according to the precipitation phase heterogeneous nucleation principle: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 15, c is more than or equal to 5 and less than or equal to 20, d is more than or equal to 2 and less than or equal to 12, e is more than or equal to 5 and less than or equal to 23, f is more than or equal to 5 and less than or equal to 15, g is more than or equal to 0.5 and less than or equal to 2, and a + b + c + d + e + f + g =5Sn3The core is separated out and grows up to obtain fine and uniform tissues;
the second step is that: smelting the alloy components obtained in the first step into a master alloy by adopting an electric arc smelting method;
the third step: re-melting the mother alloy, and suction-casting the mother alloy into a section by a copper mold;
the fourth step: and then the section is melted to a molten state by induction melting, and a rapid sequential solidification process is adopted after heat preservation, so that the uniform and fine as-cast beta-Zr (Ti) -phase composite material on the bulk metallic glass substrate is prepared.
The purity of the alloy component in the first step is more than 99.5%.
The draw rate of the rapid sequential solidification process described in the fourth step is 5 mm/s.
Compared with the prior art, the invention has the following remarkable advantages:
(1) only trace Sn element needs to be added to form Zr while ensuring the amorphous forming capability of the existing Bulk Metallic Glass (BMG)5Sn3Nanoparticles of Zr5Sn3As a heterogeneous nucleation core, the beta-Zr (Ti) phase is promoted to be uniformly precipitated, and a fine and uniform second phase structure is obtained.
(2) The traditional method refines the precipitated phase structure by changing the cooling rate, needs high cooling rate, namely large drawing rate, and therefore has high requirement on equipment and is easy to consume the equipment. The method is simple and convenient, can realize the refinement of the tissue at a lower drawing speed, and is energy-saving and efficient.
Drawings
FIG. 1 is a flow chart of the method for refining the structure of the bulk metallic glass composite material.
FIG. 2 is Zr56.2Ti13.8Nb5.0Cu6.9Ni5.6Be12.5(S1) microstructure of the composite material (a is a microstructure picture, b is an XRD picture).
FIG. 3 shows (Zr) in example 156.2Ti13.8Nb5.0Cu6.9Ni5.6Be12.5）99Sn1（S1+Sn1) The microstructure of the composite material (a is a microstructure picture, and b is an XRD picture).
FIG. 4 shows (S1 + Sn) in example 11) And room temperature compression profile of S1 composite.
Detailed Description
The present invention is described in further detail below with reference to the attached drawings.
The flow chart of the method for thinning the structure of the bulk metal glass composite material is shown in figure 1:
(1) designing alloy components:
selecting a Zr-Ti-Cu-Ni-Be-Nb alloy system with good Glass Forming Ability (GFA), and designing alloy components according to the precipitation phase heterogeneous nucleation principle. Specifically, bulk metallic glass (Zr) is selectedaTibCucNidBeeNbf）SngBy adjusting the relative proportion of alloy elements Zr, Ti, Cu, Ni, Be, Nb and Sn, Zr is formed on the premise of ensuring the amorphous forming capability5Sn3The particles promote heterogeneous nucleation of beta-Zr (Ti) phase so as to obtain a uniformly refined tissue structure.
(2) Smelting a master alloy:
converting the mass percent according to the atomic percent of different alloy elements obtained by the component design in the step (1), and preparing the required alloy by adopting high-purity metal components. Under the protection of high-purity Ar gas, residual oxygen in the cavity is removed by smelting Ti or Zr pure metal, and a water-cooled copper crucible non-consumable arc smelting device is adopted to smelt the master alloy. And carrying out electromagnetic stirring while smelting the master alloy for multiple times to obtain a uniformly mixed master alloy button ingot.
(3) Material molding:
and after remelting the master alloy, performing suction casting or blow casting on the master alloy to form a required section, wherein the shape and the size of the section can be designed according to requirements.
(4) Rapid sequential solidification
And (3) putting the section formed by the copper mold into a treated graphite crucible, vacuumizing, introducing high-purity argon, performing induction heating to melt the alloy, and soaking the alloy into the Ga-In-Sn liquid alloy with extremely strong cooling capacity at the same drawing speed after heat preservation.
(5) And (3) tissue structure characterization:
and (3) performing microstructure characterization on the prepared composite material by using an X-ray diffractometer (XRD), a Differential Scanning Calorimeter (DSC), an Optical Microscope (OM), an electron scanning microscope (SEM) and the like, and further performing mechanical property characterization on the composite material to determine the refining effect after Sn is added.
The invention is further illustrated by the following examples and figures.
Example 1
(1) Selection of raw materials
The purity of each metal component selected by the master alloy ingot prepared by the invention is shown in table 1, and the alloy components are
（Zr56.2Ti13.8Nb5.0Cu6.9Ni5.6Be12.5）99Sn1(abbreviation: S1+ Sn1) (atomic percent).
TABLE 1 purity (%) -of selected metal components for preparing master alloy ingots
| Alloy element | Zr | Ti | Cu | Ni | Be | Nb | Sn |
| Purity/%) | 99.95 | 99.95 | 99.99 | 99.99 | 99.5 | 99.9 | 99.99 |
(2) Preparation of master alloy ingot
Under the conditions of Ti gas suction and high-purity argon protection, a non-consumable arc melting furnace is used for melting a mother alloy buckle ingot, and the specific procedures are as follows:
a. mechanically polishing the surface of a metal raw material to remove oxide skin on the surface, and preparing the material according to a designed component proportion; the prepared materials are put into a water-cooled copper crucible in a smelting furnace according to the weight of about 80g per ingot, and the furnace is covered by a furnace cover and vacuumized to 2 multiplied by 10-3Pa; filling a certain amount of high-purity argon (99.99%) with pressure, wherein the pressure range of the argon is 0.4-0.6 MPa;
b. before a master alloy ingot is melted, melting the Ti ingot for air suction for 2-3 times;
c. smelting a master alloy ingot for multiple times: the method comprises the steps of firstly smelting Zr, Ti, Cu, Ni, Be, Nb and Sn alloy elements for 2-3 times by adopting a non-consumable tungsten electrode, and applying an electromagnetic stirring effect to obtain a mother alloy button ingot which is uniformly mixed. The current adopted during smelting is 500-650A, and the voltage adopted during electromagnetic stirring is 1-3V.
(3) Shaping of materials
And placing the mother alloy ingot in a forming system in which a water-cooled copper crucible and a water-cooled copper mold are tightly combined. The system is pumped to 4-5 × 10-4Pa; after the remelting by electric arc heating, the rod-shaped sample with the required diameter is prepared by injecting the rod-shaped sample into a water-cooling copper mold by self gravity under the protective atmosphere of 0.6MPa of inert gas (99.999 percent of high-purity argon).
(4) Rapid sequential solidification
And (3) putting the section formed by the copper die into a treated graphite crucible, vacuumizing, filling high-purity argon, performing induction heating until the alloy is molten, preserving the heat for ten minutes, and immersing the section into the Ga-In-Sn liquid alloy with extremely strong cooling capacity at a drawing speed of 5 mm/s.
(5) Structural and performance characterization
FIG. 3(a) is S1+ Sn prepared using the above process conditions (6 mm diameter, 5mm/S draw rate)1The microstructure of the alloy. It was found that fine dendritic phases were uniformly distributed on the amorphous matrix, and the phase β -zr (ti) structure was found by XRD analysis (fig. 3 (b)).
Comparing fig. 2 and fig. 3, it can be found that under the same process conditions, after 1% of Sn is added to the S1 alloy, the β -zr (ti) phase is finely and uniformly distributed on the metallic glass substrate, and the tissue refinement of the zirconium-based metallic glass endogenous composite material is realized.
FIG. 4 shows (S1 + Sn)1) And S1 composite material stress-strain curve, the experimental conditions are that the sample is Ø 3 multiplied by 6mm columnar sample, the experimental temperature is room temperature (25 ℃), the compressive strain rate is 2 multiplied by 10-4s-1. The mechanical property test result shows that:
prepared (S1 + Sn)1) The breaking strength of the composite material reaches 1830MPa, the compression plasticity reaches 12%, the breaking strength of the S1 composite material reaches 1590MPa, and the compression plasticity reaches 15%. Compared with the Sn, the material has better performance.
Example 2
In the same manner as in example 1, the alloy composition was: (Zr)60Ti14.67Nb5.33Cu5.56Ni4.44Be10）99Sn1. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 5mm/s, in comparison with Zr60Ti14.67Nb5.33Cu5.56Ni4.44Be10The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Example 3
In the same manner as in example 1, the alloy composition was: (Zr)63Ti15Nb7.5Cu5.5Ni4Be5）99Sn1. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 5mm/s, in comparison with Zr63Ti15Nb7.5Cu5.5Ni4Be5The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Example 4
In the same manner as in example 1, the alloy composition was: (Zr)70Ti5Nb10.5Cu5Ni2Be7.5）99Sn1. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 10mm/s, in comparison with Zr70Ti5Nb10.5Cu5Ni2Be7.5The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Example 5
In the same manner as in example 1, the alloy composition was: (Zr)52.2Ti13.8Nb5.0Cu6.9Ni7.6Be14.5）99.25Sn0.75. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 5mm/s, in comparison with Zr52.2Ti13.8Nb5.0Cu6.9Ni7.6Be14.5The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Example 6
In the same manner as in example 1, the alloy composition was: (Zr)43Ti15Nb7.5Cu12.5Ni12Be10）99.5Sn0.5. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 10mm/s, in comparison with Zr43Ti15Nb7.5Cu12.5Ni12Be10The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Example 7
In the same manner as in example 1, the alloy composition was: (Zr)41Ti11.5Nb10Cu5.5Ni9Be23）99.5Sn0.5. A bar-shaped as-cast beta-Zr/bulk metallic glass composite sample with a diameter of 6mm was prepared at a draw rate of 10mm/s, in comparison with Zr41Ti11.5Nb10Cu5.5Ni9Be23The structure of the alloy and the composite material is obviously, uniformly and finely divided.
Claims (12)
1. The zirconium-based metallic glass endogenetic composite material is characterized in that the expression of the atomic percent of the alloy elements is as follows: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, and a is more than or equal to 5b is less than or equal to 15, c is less than or equal to 5 and less than or equal to 20, d is less than or equal to 2 and less than or equal to 12, e is less than or equal to 5 and less than or equal to 23, f is less than or equal to 5 and less than or equal to 15, g is less than or equal to 0.5 and less than or equal to 2, and a + b + c + d + e + f + g =100, wherein the metal glass composite material prepared from the alloy components is uniformly and dispersedly distributed with fine beta-Zr phase of a tough second phase:
the first step is as follows: selecting a block metal glass alloy system, and adjusting the alloy components according to the precipitation phase heterogeneous nucleation principle: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 15, c is more than or equal to 5 and less than or equal to 20, d is more than or equal to 2 and less than or equal to 12, e is more than or equal to 5 and less than or equal to 23, f is more than or equal to 5 and less than or equal to 15, g is more than or equal to 0.5 and less than or equal to 2, and a + b + c + d + e + f5Sn3The core is separated out and grows up to obtain fine and uniform tissues;
the second step is that: smelting the alloy components obtained in the first step into a master alloy by adopting an electric arc smelting method;
the third step: re-melting the mother alloy, and suction-casting the mother alloy into a section by a copper mold;
the fourth step: and then, induction melting the section to a molten state, and carrying out heat preservation and then adopting a rapid sequential solidification process to obtain the composite material.
2. The composite material of claim 1, wherein in the first step, the alloy constituents are each greater than 99.5% pure.
3. The composite material of claim 1, wherein in the second step, the master alloy is melted under an inert atmosphere.
4. The composite material of claim 1, wherein in the second step, the master alloy is melted under an inert atmosphere of 0.4 to 0.6 MPa.
5. The composite material of claim 1, wherein in the second step, electromagnetic stirring is adopted during smelting, the stirring voltage is 1-3V, and the current during smelting is 500-650A.
6. The composite of claim 1, wherein in the fourth step, the rapid sequential solidification process draws at a rate of 5 mm/s.
7. The preparation method of the zirconium-based metallic glass endogenetic composite material is characterized by comprising the following steps:
the first step is as follows: selecting a block metal glass alloy system, and adjusting the alloy components according to the precipitation phase heterogeneous nucleation principle: (Zr)aTibCucNidBeeNbf）SngWherein a is more than or equal to 35 and less than or equal to 70, b is more than or equal to 5 and less than or equal to 15, c is more than or equal to 5 and less than or equal to 20, d is more than or equal to 2 and less than or equal to 12, e is more than or equal to 5 and less than or equal to 23, f is more than or equal to 5 and less than or equal to 15, g is more than or equal to 0.5 and less than or equal to 2, and a + b + c + d + e + f5Sn3The core is separated out and grows up to obtain fine and uniform tissues;
the second step is that: smelting the alloy components obtained in the first step into a master alloy by adopting an electric arc smelting method;
the third step: re-melting the mother alloy, and suction-casting the mother alloy into a section by a copper mold;
the fourth step: and then, induction melting the section to a molten state, and carrying out heat preservation and then adopting a rapid sequential solidification process to obtain the composite material.
8. The method of claim 7, wherein in the first step, the alloy constituents are each greater than 99.5% pure.
9. The method of claim 7, wherein in the second step, the master alloy is melted under an inert atmosphere.
10. The method of claim 7, wherein in the second step, the master alloy is melted under an inert atmosphere of 0.4 to 0.6 MPa.
11. The method as claimed in claim 7, wherein in the second step, electromagnetic stirring is adopted during smelting, the stirring voltage is 1-3V, and the current during smelting is 500-650A.
12. The method of claim 7, wherein in the fourth step, the rapid sequential solidification process is operated at a draw rate of 5 mm/s.
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