CN108193147B - High-toughness zirconium-based amorphous alloy material and preparation method thereof - Google Patents
High-toughness zirconium-based amorphous alloy material and preparation method thereof Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 62
- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 47
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000004512 die casting Methods 0.000 claims description 6
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 9
- 238000007496 glass forming Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 15
- 238000013001 point bending Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- 238000010891 electric arc Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910001092 metal group alloy Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000005300 metallic glass Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
Abstract
The inventionRelates to the field of high-mechanical-property materials, in particular to a high-toughness ultrahigh-strength zirconium-based amorphous alloy and a preparation method thereof. The alloy comprises the following chemical components: (Zr)aHf1‑a)x(Cu1‑b‑c‑dNibAlcLd)yNbzM100‑x‑y‑z(ii) a According to the invention, on the basis of the components with excellent performance of the original Zr-based amorphous alloy, the specific elements capable of increasing the amorphous chaos degree are added, the glass forming capability and the mechanical property of the Zr-based amorphous alloy are improved, and the bending and breaking strain of the Zr-based amorphous alloy is improved on the premise of not reducing the breaking and bending strength of the original alloy material.
Description
Technical Field
The invention relates to a material with high mechanical property in the application fields of consumer electronics, precision devices (such as robots), medical instruments, aerospace, aviation and the like, in particular to a high-toughness ultrahigh-strength zirconium-based amorphous alloy and a preparation method thereof.
Background
Amorphous alloys are distinguished from common crystalline materials by their distinct structural differences. In general, materials exist in the form of crystals, while amorphous materials are characterized by long-range disorder (short-range order), metastable state (crystallization at a certain temperature), isotropic physical properties to some extent, lack of exact melting point, glass transition temperature point, and the like. Meanwhile, the Glass has a similar structure with common Glass, has the characteristics of solid, metal and Glass, and is also called Metallic Glass (Metallic Glass). The crystal grain structure is not existed, and the atoms are randomly and uniformly distributed directly, and are connected by metal bond. Because the crystal grain structure is not existed, the crystal grain boundary and other defects and the lattice period translational symmetry and other characteristics are not existed, so that the crystal alloy material has the excellent properties which are not possessed by the traditional crystalline alloy material, such as high mechanical strength, high hardness, low elastic modulus, high wear resistance, high corrosion resistance and excellent soft magnetic property. The amorphous alloy has an internal structure formed by the super-quenching solidification of a molten mother alloy, and atoms of the amorphous alloy are not arranged in a periodic manner in the solidification process, so that a long-range disordered amorphous state is formed. After the discovery of the amorphous alloy, research and exploration of researchers are attracted for decades, and at present, amorphous alloy systems such as Zr-based, Cu-based, Al-based, Fe-based, Pd-based, Ni-based, Ti-based, Mg-based, rare earth-based systems and the like are discovered. The research result of the Zr-based bulk amorphous alloy material is the most remarkable, and although the application of the Zr-based bulk amorphous alloy in industry is still limited by practical factors of various applications, such as high raw material cost, harsh process conditions, complex post-treatment processing and the like. The biggest limiting factor of the application is that the amorphous alloy has no plasticity, so that the feedback of the market application is always hesitant. Therefore, improving the toughness of the amorphous alloy is an urgent need for mass production of the material.
The mechanical strength of the existing metal alloy material is generally below 1000MPa, the mechanical strength of the zirconium-based bulk amorphous alloy material is above 1500MPa, and the mechanical strength of the zirconium-based bulk amorphous alloy material is much better than that of the traditional metal alloy material; however, the toughness of the currently reported zirconium-based bulk amorphous alloy materials is much lower than that of metal alloy materials, which causes the failure of reliability test of practical products in application. The improvement of the toughness of the Zr-based amorphous alloy is always an industry bottleneck problem, and until now, no obvious improvement is reported.
Disclosure of Invention
The invention aims to overcome the problems and provide a high-toughness zirconium-based amorphous alloy material. This application is through on the composition basis of original Zr base amorphous alloy excellent properties, adds the specific element that can increase amorphous chaos degree, improves its glass forming ability and mechanicalness: on the premise of not reducing the breaking bending strength of the original alloy, the bending breaking strain of the alloy is improved.
Another object of the present invention is to provide a method for preparing a high-toughness zirconium-based amorphous alloy material, which does not require an additional process, and does not require complicated treatment of the alloy material or surface treatment of the formed product.
The object of the invention can be achieved by the following measures:
a high-toughness zirconium-based amorphous alloy material comprises the following chemical components:
(ZraHf1-a)x(Cu1-b-c-dNibAlcLd)yNbzM100-x-y-z；
wherein:
l is an element of group IIIB or IVB,
m is an element of group VIII, group IB, group IIIA or group IVA,
45≤x≤65，10≤y≤45，0≤z≤10，
0.9885≤a≤0.9894，0.05≤b≤0.2，0.05≤c≤0.3，0≤d≤0.05。
in a preferred embodiment, a is 0.989 or 0.9889.
In a preferred embodiment, x is more than or equal to 50 and less than or equal to 60; more preferably, 51 ≦ x ≦ 59; more preferably, 53. ltoreq. x.ltoreq.57.
In a preferred embodiment, 20. ltoreq. y.ltoreq.45; more preferably, y is 30-45; more preferably, 38. ltoreq. y.ltoreq.42.
In a preferred embodiment, z is 1. ltoreq. z.ltoreq.10; more preferably, z is 2. ltoreq. z.ltoreq.5; more preferably, z is 3. ltoreq. z.ltoreq.4.
In a preferred embodiment, b is 0.10-0.20; more preferably, 0.10. ltoreq. b.ltoreq.0.15.
In a preferred embodiment, c is 0.10-0.35; more preferably, c is 0.20-0.35; more preferably, 0.22. ltoreq. c.ltoreq.0.34.
In a preferred embodiment, d is 0.001 ≦ 0.05; more preferably, d is 0.005. ltoreq. d.ltoreq.0.05; more preferably, d is 0.01. ltoreq. d.ltoreq.0.02.
On the basis of the original Zr-based amorphous alloy components, elements which can increase the specific types and contents of amorphous chaos are further added, so that the mechanical properties of the product are improved on the basis of not changing the original properties of the alloy.
In the present invention, L is an element of group IIIB or IVB. In a preferred embodiment, L is Y, Er or Gd element, preferably Y or Er. We find that in the alloy, the proper amount of the elements can react preferentially to oxygen in the air to absorb the impurity element oxygen in the preparation process, so that the oxidation resistance of the alloy material is enhanced; secondly, the addition of such trace elements leads to less impurities formed on the surface, so that the quality of the interior and the surface of the material is also more excellent. The inventors have further found that when L and M are different in composition, the appropriate content in the amorphous alloy is also different. For example, when L is Y, d is not more than 0.05 (i.e., 0.001. ltoreq. d.ltoreq.0.05); when L is Er, d is preferably below 0.015, otherwise, too high d can influence the bending strain and impact toughness of the material; however, when L is Gd element, d is preferably 0.008 or less, otherwise too high d may affect the three-point bending strength, bending strain and impact toughness of the material.
In the present invention, M is an element of group VIII, group IB, group IIIA or group IVA. In a preferred embodiment, M is Fe, Co or Sn, more preferably, M is Fe or Co, and most preferably, M is Fe. These elements provide atomic diameters of different sizes within the zirconium-based system, causing an increase in the degree of disorder of the alloy material.
In a more preferred embodiment, (Zr) of the present applicationaHf1-a)x(Cu1-b-c-dNibAlcLd)yNbz(Fe/Co/Sn)100-x-y-z(ii) a More preferred formulations are shown in table 1.
The invention provides a preparation method of a high-toughness zirconium-based amorphous alloy material, which comprises the following steps: after high-purity raw materials corresponding to elements of the alloy are weighed in proportion, a mother alloy material is prepared by adopting an arc melting method under the protection of inert gas, and then an amorphous alloy material is prepared by adopting a vacuum die casting machine.
The high-purity raw materials of the invention are metal or nonmetal materials with the purity of corresponding elements of more than 99.3 percent.
The invention provides a more specific preparation method of a high-toughness zirconium-based amorphous alloy material, which comprises the following steps:
1. the raw materials adopted in the embodiment are high-purity raw materials, wherein the purity of Zr is 99.4%, the purity of the rest elements is 99.9%, and the raw materials are accurately weighed according to the formula proportion;
2. preparing a round ingot-shaped master alloy material by an arc melting method under the protection of argon;
3. selecting a certain amount of master alloy material, and preparing a sample with the thickness of 2mm by using a vacuum die casting machine;
4. after the amount is detected by XRD, the samples are confirmed to be completely amorphous;
5. and respectively carrying out three-point bending and impact mechanical property tests on the completely amorphous sample.
The details for each of the above steps are as follows:
in step 1, the equipment used was an analytical balance with an accuracy of 0.0001 g.
In the step 2, a plurality of methods for preparing the amorphous master alloy are provided, and the amorphous master alloy is prepared by using an electric arc furnace copper mold smelting method. The electric arc furnace mainly consists of the following modules: cavity, vacuum apparatus, circuit system, circulating water system and mould. The cavity is used for providing an environment for melting the alloy; the vacuum equipment comprises a mechanical pump, a molecular pump, a vacuum pipeline and various vacuum gauges; the circuit system is used for striking arc and controlling the solenoid valve and various devices; the circulating water is used for cooling the copper mold, the copper crucible and the molecular pump; the mold was used to suction cast various amorphous samples. FIG. 4 shows the principle of the electric arc furnace, in which the upper half is a copper crucible and the lower half is a mold, and the alloy is formed by using the high temperature generated by the tungsten arc discharge.
In step 3, the vacuum die casting machine can adopt equipment developed by the cooperation of AAC and other research units. The equipment is used for forming national standard three-point bending and impact toughness sample shapes, and the die is designed, simulated and manufactured in an AAC interior.
In step 4, XRD test is completed in an AAC analysis center, and the size specification of a specific test sample is in accordance with the AAC unified sample preparation standard.
In the step 5, the three-point bending and impact mechanical property tests of the sample are finished in the AAC, and the size specification of the specific test sample is in accordance with the AAC unified sampling standard.
The invention has the beneficial effects that:
aiming at that the three-point bending fracture elongation of the Zr-based amorphous alloy after the toughness is improved is about 1.5 to 2 percent and the impact toughness is not more than 100J/cm2The technical patent aims at improving the toughness of the Zr-based amorphous alloy to achieve the three-point bending fracture elongation rate of 3.6 percent and the impact toughness of more than 180J/cm2。
This application is throughOn the basis of components with excellent performance of the Zr-based amorphous alloy, specific elements capable of increasing amorphous chaos are added, glass forming capacity and mechanical property of the Zr-based amorphous alloy are improved, bending fracture strain of the Zr-based amorphous alloy is improved on the premise that fracture bending strength of an original alloy material is not reduced, mechanical strength of the Zr-based bulk amorphous alloy material can reach more than 2000MPa, and performance of the Zr-based bulk amorphous alloy in a reliability test can be effectively improved. Limited experimental data show that on the basis of original Zr-based amorphous alloy with the breaking bending strength of 2107.47MPa and the bending breaking strain of 2.56%, by adopting the synthesis of the chemical composition, the bending breaking strain can reach more than 3.6% on the premise of not reducing the breaking bending strength of the original Zr-based amorphous alloy, and the impact toughness is more than 180J/cm2(ii) a The method provided by the invention does not need additional working procedures, does not need to carry out complex treatment on alloy raw materials, and does not need to carry out surface treatment on the formed product.
Drawings
FIG. 1 shows the results of three-point bending mechanical property test of example 1;
FIG. 2 is the results of three-point bending mechanical property test of example 2;
FIG. 3 shows the results of the three-point bending mechanical property test of example 4;
fig. 4 is a schematic view of the principle of use of an electric arc furnace.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the embodiments. However, it will be appreciated by those of ordinary skill in the art that numerous technical details are set forth in order to provide a better understanding of the present invention in its various embodiments. However, the technical solutions claimed in the claims of the present invention can be implemented without these technical details and with various changes and modifications based on the following embodiments.
Examples 1 to 9
The chemical composition of each Zr-based amorphous alloy is detailed in table 1.
The molar ratio of each element of the Zr-based amorphous alloy of each example is detailed in table 2.
TABLE 1 chemical composition of elements of examples
TABLE 2 molar ratios of the elements of the examples
The alloy preparation method comprises the following steps:
example 1 preparation of the alloy
1. Formulation according to chemical composition (Zr)0.9889Hf0.011)55(Cu1-b-c-d Ni0.1Al0.22Y0.01)40Nb3.5Fe1.5The following table is converted into atomic molar ratios. Each formulation required 240g of master alloy to be prepared, one master alloy at 60g, and a total of 4 master alloys to be prepared. The weighed amounts (total weight: 60g, 4 parts) were calculated as atomic mass. Wherein the purity of zirconium is 99.4%, which is industrial grade sponge zirconium, and the purity of the rest elements is 99.9%. The Hf element can also be sponge zirconium with a certain Hf content, and the weight needs to be converted according to the atomic percentage.
2. Under the protection of argon, a round ingot-shaped master alloy material is prepared by an electric arc melting method, and the whole process aims to melt various elements into an alloy material. In order to ensure the uniformity of the smelted mother alloy round ingot, the mother alloy round ingot needs to be turned over for 3-4 times in the process of smelting the mother alloy round ingot by electric arc, and the temperature of electric arc smelting heating is at the melting point of the mother alloyAbove, vacuum degree of 10-1Pa to 10-2Pa。
3. The prepared 240g of round ingot master alloy material is put into a vacuum die casting machine, and a uniform die casting process is adopted to form 12 strip-shaped samples for testing the mechanical properties of three-point bending and impacting, wherein the size is 2mm x 10mm x 50 mm.
4. The prepared sample is subjected to three-point bending and impact mechanical property test, and the specific data are shown in Table 3
TABLE 3 three-point bending and impact mechanical Property test data
Three-point bending test: the same sample is tested for 5, and in the figure, the stable value data in 5 selected universal testing machines is selected to eliminate the abnormity.
The preparation process of the alloy of other embodiments is the same as that of embodiment 1.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples for carrying out the invention, and that various changes in form and details may be made therein without departing from the spirit and scope of the invention in practice.
Claims (7)
1. A high-toughness zirconium-based amorphous alloy material is characterized in that the alloy comprises the following chemical components:
（ZraHf1-a)x(Cu1-b-c-dNibAlcLd)yNbzM100-x-y-z；
wherein:
53≤x≤65，10≤y≤45，0≤z≤10，
0.9885≤a≤0.9894，0.05≤b≤0.2，0.05≤c≤0.3；
wherein, the L is Er or Gd element;
when L is Er, d is more than or equal to 0.001 and less than or equal to 0.015; when L is Gd, d is more than or equal to 0.001 and less than or equal to 0.008;
and M is Co or Sn element.
2. The high-toughness zirconium-based amorphous alloy material according to claim 1, wherein a =0.989 or 0.9889.
3. The high-toughness Zr-based amorphous alloy material according to claim 1, wherein x is 53-60, y is 20-45, and z is 1-10.
4. The high-toughness Zr-based amorphous alloy material according to claim 3, wherein x is 53-59, y is 30-45, and z is 2-5.
5. The high-toughness Zr-based amorphous alloy material according to claim 1, wherein b is 0.10. ltoreq. b.ltoreq.0.20, and c is 0.10. ltoreq. c.ltoreq.0.3.
6. The high-toughness Zr-based amorphous alloy material according to claim 5, wherein b is 0.10-0.15 and c is 0.20-0.3.
7. A method for preparing high-toughness Zr-based amorphous alloy material according to claim 1, wherein high-purity raw materials corresponding to each element of the alloy are weighed in proportion, and then a mother alloy material is prepared by arc melting under the protection of inert gas, and then a vacuum die casting machine is used to prepare the amorphous alloy material.
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| CN111822673B (en) * | 2020-07-14 | 2022-05-31 | 西安工业大学 | Forming device and preparation method of amorphous alloy near-net-shape casting |
| CN113981335B (en) * | 2021-10-29 | 2022-09-23 | 盘星新型合金材料(常州)有限公司 | Microelement modified Be-free block amorphous alloy and preparation method and application thereof |
| CN115522143A (en) * | 2022-09-19 | 2022-12-27 | 盘星新型合金材料(常州)有限公司 | Large-size zirconium-based amorphous alloy containing tin, niobium and iron simultaneously and preparation method thereof |
| CN115449723A (en) * | 2022-09-21 | 2022-12-09 | 盘星新型合金材料(常州)有限公司 | Large-size zirconium-based amorphous alloy containing Sn and Fe at same time and preparation method thereof |
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