CN108504970B - Low-brittleness zirconium-based amorphous alloy and preparation method thereof - Google Patents
Low-brittleness zirconium-based amorphous alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-brittleness zirconium-based amorphous alloy, which comprises the following components(ZraTibCucNidBeeMfNg)1‑xOxWherein M is one or more of Ag, In and Sb, and N is one or more of Mo, Mn and Pr; a. b, c, d, e, f, g and x are atomic percent, wherein a is more than or equal to 39 and less than or equal to 44, b is more than or equal to 10 and less than or equal to 15, c is more than or equal to 10 and less than or equal to 14, d is more than or equal to 6 and less than or equal to 15, e is more than or equal to 18 and less than or equal to 23, f is more than or equal to 0 and less than or equal to 10, g is more than or. The zirconium-based amorphous alloy has high hardness, high tensile strength and formation size, and most importantly, has lower brittleness by improving the composition and the preparation method, and solves the problem of high brittleness of the zirconium-based amorphous alloy in the prior art.
Description
Technical Field
The invention belongs to the field of metal materials, and particularly relates to a low-brittleness zirconium-based amorphous alloy and a preparation method thereof.
Background
From the atomic model of the constituent substances, substances can be classified into ordered structures and disordered structures, wherein crystals are typically ordered structures, and gaseous, liquid and some solids belong to disordered structures. Amorphous alloy, which is called amorphous alloy for short, refers to a metal alloy without long-range order but with short-range order, and because of the characteristics of the metal alloy, amorphous alloy liquid is called glassy alloy or amorphous alloy. The amorphous alloy has long-range disorder but short-range order, which means that atoms do not have periodicity and translational symmetry in spatial arrangement, but have certain regularity in bonding with adjacent or next-adjacent atoms within a micro scale of 1-2 nm. Like crystalline alloys, amorphous alloys are multicomponent alloy systems, and have the characteristics of high strength, high elasticity, corrosion resistance, good hot formability and the like due to the special microstructure, so that the amorphous alloys have attracted much attention in recent years and are applied to many fields.
Amorphous alloys have very typical structural features: 1. long-range disorder, the atomic arrangement of which does not have long-range periodicity, and crystal grain boundaries, lattice defects, and the like cannot be seen by an electron microscope; 2. short-range order, the distance between adjacent atoms and the crystal is very small, and the coordination numbers are very close; 3. the uniformity is that the amorphous alloy has uniform and isotropic structure and uniform components, and has no heterogeneous phase, precipitate, segregation or other fluctuation of components like crystals; 4. and structural phase change, wherein when the temperature rises, obvious structural phase change can occur in a certain narrow temperature zone. In the past decades, many massive amorphous alloys of new elements have been discovered by researchers, and some of the practical components have been discovered and utilized, and based on these researches, modern amorphous alloy materials not only have greatly improved forming ability, but also have high hardness, yield strength, elastic strain limit and fatigue resistance, and relatively high fracture toughness and corrosion resistance. In general, the trend of amorphous alloy materials is to improve the forming ability and mechanical properties of amorphous alloys to meet wider application requirements. At present, the improvement of amorphous alloy materials is mostly based on the improvement of amorphous alloys with known component formulas, and different technical effects are obtained by the difference of component compositions, component proportions and preparation methods.
Zr-Ti-Cu-Ni is a common quaternary zirconium-based amorphous alloy and has good vitrification forming capability. In the quaternary system, four different atoms can form a compact microstructure, so that the amorphous alloy is more compact and stable in macroscopic state structure. In the prior art, Zr-Ti-Cu-Ni quaternary amorphous alloy is improved, for example, elements with small atomic volume or elements with larger atomic volume are added, so that a multi-element alloy system after being added has a more compact and stable structure due to the atomic composition with gradient size. However, the zirconium-based amorphous alloy containing the Zr-Ti-Cu-Ni four components in the prior art is sensitive to the purity of raw materials, and the prepared amorphous alloy has the problems of high brittleness, low forming capability and low strength.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a zirconium-based amorphous alloy which is improved aiming at a Zr-Ti-Cu-Ni quaternary amorphous alloy and a preparation method of the zirconium-based amorphous alloy.
The technical effect to be achieved by the invention is realized by the following scheme:
the composition of the low-brittleness zirconium-based amorphous alloy provided by the invention is (Zr)aTibCucNidBeeMfNg)1-xOxWherein M is one or more of Ag, In and Sb, and N is one or more of Mo, Mn and Pr; a. b, c, d, e, f, g and x are atomic percent, wherein a is more than or equal to 39 and less than or equal to 44, b is more than or equal to 10 and less than or equal to 15, c is more than or equal to 10 and less than or equal to 14, d is more than or equal to 6 and less than or equal to 15, e is more than or equal to 18 and less than or equal to 23, f is more than or equal to 0 and less than or equal to 10, g is more than or.
The Zr-based amorphous alloy is one of amorphous systems with new formula components, and in the development process of the prior art, the Zr-based amorphous alloy is developed from the earliest binary alloy and ternary alloy to the current five-element and six-element or more intermediate-component alloy. In terms of dynamics, the multi-component amorphous alloy system also relates to redistribution and displacement type diffusion of multiple elements in the precipitation of the multi-component alloy phase, so that the dynamics of the alloy is retarded, the atoms of the components are not easy to effectively diffuse, and the nucleation and growth processes of the alloy are inhibited, so that the multi-component alloy is easier to form various metastable phases and presents an amorphous state. To enhance the ability of amorphous alloys to form, many researchers have sought to form amorphous states and have overlooked other related properties. The inventor of the invention finds in long-term practice that the Zr-Ti-Cu-Ni four-component zirconium-based amorphous alloy as a main alloy component has a loose structure between atoms in an alloy system taking Zr as the most main component, and macroscopically causes the defect of the mechanical property of the quaternary alloy. Based on the above principle, the inventor of the present invention proposes to add other components matched with the four main elements of Zr, Ti, Cu and Ni into the zirconium-based alloy raw material, the number of the matched components is not more than 4-5, so as to avoid the whole forming of an excessive high-entropy system, thereby leading the whole alloy to be in a metastable state, on the other hand, the added adaptive components and the atomic radius among the main components are distributed in a certain rule, meanwhile, the atomic percentage of the component is matched with the atomic radius, and the added component and the main component have large negative mixing enthalpy, namely, the alloy is easy to form a highly disordered close-packed structure in a liquid state, has high liquid-solid interface energy, reduces the long-range diffusion capacity of atoms, thereby inhibiting the formation and growth of crystal nucleus and improving the amorphous forming capability and thermal stability of the amorphous alloy macroscopically.
In the invention, Zr, Ti, Cu and Ni are used as main alloy components, Be, M components and N components which are matched with each other are used as other alloy components, M is one or more of Ag, In and Sb, and N is one or more of Mo, Mn and Pr and has specific atomic percentage. Meanwhile, in the zirconium-based amorphous alloy of the invention, because of the components capable of inhibiting the formation and growth of crystal nuclei, in the smelting process, a product with lower oxygen content than that of the zirconium-based amorphous alloy in the prior art can be obtained by controlling the smelting process, and in the zirconium-based amorphous alloy of the invention, the oxygen content is very low, and the atomic percent of the alloy only accounts for less than 200 ppm.
Further, f is in the range of 1-10, and g is in the range of 0.2-1.
Furthermore, the ranges of a, b, c, d, e, f, g and x are 39-40, 10-12, 10-13, 6-10, 18-22, 5-10, 0.2-0.5 and 100-150 ppm.
Further, the volume fraction of the crystalline phase is 5-10% and the volume fraction of the amorphous phase is 90-95% based on the total volume of the zirconium-based amorphous alloy. The zirconium-based amorphous alloy has a high volume ratio of an amorphous phase due to the special composition proportion.
Further, the zirconium-based amorphous alloy has the hardness of more than 500HV, the tensile strength of 2500-.
The invention also provides a method for preparing the low-brittleness zirconium-based amorphous alloy part, which comprises the following steps:
step one, proportionally mixing raw materials of a zirconium-based amorphous alloy according to a formula, wherein the purity of the raw materials is more than 99.9%;
step two, in vacuum condition or argon atmosphereSmelting the raw materials by electric arc smelting or other conventional smelting modes, and repeatedly smelting for 3-6 times; the vacuum degree in the smelting process is 10-3-10-1Pa, the pressure of argon atmosphere is 0.01-0.05MPa, and a master alloy ingot is obtained after cooling;
and step three, obtaining the zirconium-based amorphous alloy product by a conventional amorphous alloy preparation method.
Further, the Be element is divided into a plurality of equal parts in the form of intermediate alloy and is uniformly added in the smelting process.
Further, the Be element is added in the form of NiBeM intermediate alloy, TiBeM intermediate alloy and ZrBeM intermediate alloy, wherein the atomic percentages of Ni/Ti/Zr, Be and M are 1 (2.5-5): (0.6-0.8).
Further, the smelting mode in the step two is two-stage induction smelting, and the first-stage smelting conditions are as follows: the induction voltage is 11-12kV, the smelting time is 0.5-1min, and the second-stage smelting conditions are as follows: the induction voltage is 6-7kV, the smelting time is 0.5-1min, and the first-stage smelting mode and the second-stage smelting mode are alternately carried out until the alloy is evenly smelted.
Further, the smelting conditions in the first stage are as follows: the induction voltage is 11.5kV, the smelting time is 0.5min, and the second-stage smelting conditions are as follows: the induction voltage is 7kV, the smelting time is 0.5min, and the first-stage smelting and the second-stage smelting are alternately smelted for 3 times respectively.
In the present invention, the Be element as the element having the smallest atomic radius forms larger atoms and filler atoms between atoms in the zirconium-based amorphous alloy of the present invention to form a close-packed structure. In the prior art, the amount of Be added in many publications exceeds 10%, even 15% or more, but there are difficulties in the actual preparation process, and the difficulties are: in the prior art, the preparation process of the zirconium-based amorphous alloy comprises the steps of mixing raw material powder together, and then heating the mixture in the existing smelting mode to enable the raw materials to form uniform molten soup, so that uniform alloy is prepared. Be element is different from other elements in high temperature resistance point, so that burning loss is easy to occur in the processing process in the prior art, and the content of Be element often cannot reach the set percentage content. In the invention, the inventor utilizes Be element, Ni/Ti/Zr and M component to prepare the intermediate alloy under the condition of being lower than the smelting temperature at a specific atomic percentage, so that the intermediate alloy has higher smelting temperature tolerance than the single Be raw material, and simultaneously, two-section type induction smelting is preferably adopted in the preparation method, the smelting is carried out in a mode of alternating high induction voltage and low induction voltage, the purpose of uniformly smelting the alloy is achieved through the change of magnetic induction and the change of temperature in a certain range, and the burning loss of Be is reduced to the minimum.
The invention has the following advantages:
1. the zirconium-based amorphous alloy has high hardness, high tensile strength and formation size, and most importantly, has lower brittleness by improving the composition and the preparation method, and solves the problem of high brittleness of the zirconium-based amorphous alloy in the prior art.
2. The method for preparing the low-brittleness zirconium-based amorphous alloy is suitable for preparing the low-brittleness zirconium-based amorphous alloy, does not need to add any equipment, slightly improves the existing process, and is convenient, practical and suitable for batch production.
3. The low-brittleness zirconium-based amorphous alloy has strong antibacterial effect.
4. The low-brittleness zirconium-based amorphous alloy overcomes the defects of the zirconium-based amorphous alloy in the prior art, and is suitable for being applied to the fields of smart phones, watch assemblies, medical implants, implanted teeth, magnet cores, sports equipment, aerospace devices and the like.
Detailed Description
The present invention will be described in detail with reference to examples.
Examples
The formula of the zirconium-based amorphous alloy is prepared according to the components in the following table, and the number behind the element symbol is the atomic percent of each element.
The preparation method of the alloy comprises the following steps:
step one, proportionally mixing raw materials of the zirconium-based amorphous alloy according to a formula, wherein the purity of the raw materials is more than 99.9%.
In examples 1 to 10, the Be element was added in the form of a NiBeM master alloy, wherein the atomic percentages of Ni, Be and M were 1: 3: 0.6, and the rest of the raw materials are added in the form of powder. (the atomic percentages of Ni and Be not including the M component are unchanged).
In examples 11-18, the Be element was added as a TiBeM master alloy, where the atomic percentages of Ti, Be, and M were 1: 4.5: 0.6, and the rest of the raw materials are added in the form of powder. (the atomic percentages of Ti and Be not including the M component are unchanged).
In examples 19 to 27, the Be element was added as a ZrBeM master alloy, wherein the atomic percentages of Zr, Be and M were 1: 5: 0.6, and the rest of the raw materials are added in the form of powder. (the atomic percentages of Zr and Be not including the M component were unchanged).
The components except the Be intermediate alloy are uniformly mixed, the mixture is divided into a plurality of equal parts, and the equal parts of the Be intermediate alloy are divided into a plurality of equal parts to Be sequentially and uniformly added in the smelting process.
Step two, under the vacuum degree of 10-3Raw materials are subjected to induction melting under the Pa condition, the melting mode is two-section type induction melting, and the first-section melting condition is as follows: the induction voltage is 11.5kV, the smelting time is 0.5min, and the second-stage smelting conditions are as follows: the induction voltage is 7kV, the smelting time is 0.5min, the first stage smelting and the second stage smelting are alternately smelted for 3 times respectively at 10 DEG C2-103And cooling at the speed of K/s to obtain a master alloy ingot.
And step three, preparing the zirconium-based amorphous alloy into a sheet by a die-casting process, and then adding the sheet to prepare a required test sample by machining according to the test requirement.
The maximum forming capacity of the zirconium-based amorphous alloy prepared in the embodiment is more than 20mm, the glass transition temperature is in the range of 460-480 ℃, the initial melting temperature is in the range of 860-880 ℃, the processing process is not difficult, and the conventional equipment is adopted. According to metallographic tests, the volume fraction of the crystalline phase in examples 1-27 accounts for 5-10%, the volume fraction of the amorphous phase accounts for 90-95%, and particularly in examples 1-13, the volume fraction of the crystalline phase in the zirconium-based amorphous alloy is less than 8%.
As a comparative example, the following are specified in comparison with the examples of the present invention:
the preparation method of the comparative example is a preparation method of the conventional amorphous alloy: after mixing alloy raw materials, smelting the alloy uniformly in a smelting device by using an induction smelting process, cooling to obtain a master alloy ingot, then preparing the master alloy ingot into a sheet by using a die casting process, and preparing a required test sample by using machining according to the test requirement.
The toughness of the alloy (so as to represent the brittleness) is tested by using a metal pendulum tester according to GB/T229-2007 metallic material Charpy pendulum impact test method, and a standard sample made of the amorphous alloy is tested at the room temperature of 25 ℃. The length of a standard impact sample is 55cm, the cross section is a square section of 10 multiplied by 10cm, the V-shaped notch is formed, the blade of a pendulum bob is 2mm, the absorption power KV2 of the test sample is higher, and the higher the KV2 value is, the better the impact toughness of the test sample is. KV2 units are joules. And (3) performing hardness test on the prepared zirconium-based amorphous alloy by using a Vickers hardness tester according to the Vickers hardness test method of GB/T7997-2014 hard alloy. Part 1 of the tensile test of metallic materials according to GB/T228.1-2010, using a universal tester: room temperature test method the tensile strength of the test specimens was tested.
Examples the test results are as follows:
comparative example test results are as follows:
the test results show that the zirconium-based amorphous alloy has the advantages of excellent impact toughness, high hardness, high strength, good elastic limit and obvious mechanical property advantage compared with a comparative example. In conclusion, the zirconium-based amorphous alloy in the embodiment of the invention has the advantages of strong impact resistance, small brittleness, high vitrification forming capability and good application prospect.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the embodiments of the present invention and not for limiting the same, and although the embodiments of the present invention are described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the embodiments of the present invention, and these modifications or equivalent substitutions cannot make the modified technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. A low-brittleness zirconium-based amorphous alloy is characterized in that:
the composition of the zirconium-based amorphous alloy is (Zr)aTibCucNidBeeMfNg)1-xOxWherein M is one or more of Ag, In and Sb, and N is one or more of Mo, Mn and Pr;
a. b, c, d, e, f, g and x are atomic percent, wherein a is more than or equal to 39 and less than or equal to 40, b is more than or equal to 10 and less than or equal to 12, c is more than or equal to 10 and less than or equal to 13, d is more than or equal to 6 and less than or equal to 10, e is more than or equal to 18 and less than or equal to 22, f is more than or equal to 5 and less than or equal to 10, g is more than or equal to 0.;
the zirconium-based amorphous alloy has the hardness of more than 500HV, the tensile strength of 2500-.
2. The low-brittleness zirconium-based amorphous alloy according to claim 1, wherein: based on the total volume of the zirconium-based amorphous alloy, the volume fraction of the crystalline phase is 5-10%, and the volume fraction of the amorphous phase is 90-95%.
3. A method for preparing a low-brittleness zirconium-based amorphous alloy according to any one of claims 1-2, comprising the steps of:
step one, proportionally mixing raw materials of a zirconium-based amorphous alloy according to a formula, wherein the purity of the raw materials is more than 99.9%;
smelting the raw materials by arc smelting or other conventional smelting modes under a vacuum condition or in an argon atmosphere, and repeatedly smelting for 3-6 times; the vacuum degree in the smelting process is 10-3-10-1Pa, the pressure of argon atmosphere is 0.01-0.05MPa, and a master alloy ingot is obtained after cooling;
and step three, obtaining the zirconium-based amorphous alloy product by a conventional amorphous alloy preparation method.
4. A method of producing a low-brittleness zirconium-based amorphous alloy according to claim 3, wherein: be element is divided into a plurality of equal parts in the form of intermediate alloy and is evenly added in the smelting process.
5. The method according to claim 4, wherein: the Be element is added in the form of NiBeM intermediate alloy, TiBeM intermediate alloy and ZrBeM intermediate alloy, wherein the atomic percentages of Ni/Ti/Zr, Be and M are 1 (2.5-5): (0.6-0.8).
6. A method of producing a low-brittleness zirconium-based amorphous alloy according to claim 3, wherein: the smelting mode in the second step is two-section induction smelting, and the first-section smelting conditions are as follows: the induction voltage is 11-12kV, the smelting time is 0.5-1min, and the second-stage smelting conditions are as follows: the induction voltage is 6-7kV, the smelting time is 0.5-1min, and the first-stage smelting mode and the second-stage smelting mode are alternately carried out until the alloy is evenly smelted.
7. The method of producing a low-brittleness zirconium-based amorphous alloy according to claim 6, wherein: the smelting conditions of the first stage are as follows: the induction voltage is 11.5kV, the smelting time is 0.5min, and the second-stage smelting conditions are as follows: the induction voltage is 7kV, the smelting time is 0.5min, and the first-stage smelting and the second-stage smelting are alternately smelted for 3 times respectively.
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