CN114836700B - Large-size zirconium-based amorphous alloy with high strength and high hardness and preparation method thereof - Google Patents
Large-size zirconium-based amorphous alloy with high strength and high hardness and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of amorphous alloy, and particularly relates to a high-strength and high-hardness amorphous alloyThe large-size zirconium-based amorphous alloy and the preparation method thereof have the atomic percentage expression as follows: zr a Cu b Ni c Al d Ti e Fe f Hf g M r (ii) a Wherein M is one or more of Y, dy, lu, ho, yb, ce, rh and Os; a is more than 45 and less than 55; b is more than 20 and less than 30; c is more than 5 and less than 10; d is more than 5 and less than 10; e is more than 0 and less than 5; f is more than 0 and less than 5; g is more than 0 and less than 2; r is more than or equal to 0 and less than 0.5; according to the large-size zirconium-based amorphous alloy with high strength and high hardness and the preparation method thereof, the components with high strength and high hardness are obtained by selecting conventional elements and compounding with rare earth elements which are easy to obtain; the oxygen element is harmful to the forming capability of the amorphous alloy, the oxygen element of the amorphous alloy is reduced by adding a small amount of rare earth elements, the amorphous forming capability of the amorphous alloy is improved, and the application field of the product is enlarged by adding the toxic element Be instead of the toxic element Be.
Description
Technical Field
The invention belongs to the technical field of amorphous alloys, and particularly relates to a large-size zirconium-based amorphous alloy with high strength and high hardness and a preparation method thereof.
Background
The amorphous alloy has unique long-range disorder and short-range order structure, so that the amorphous alloy has more excellent mechanical property compared with the alloy, and the amorphous alloy with excellent physical and chemical properties has wider application prospect compared with the alloy. Z r-based bulk amorphous alloy material is mainly applied to the fields of military supplies, space engineering materials, precision machining, sports and leisure supplies, electronic product shells, medical appliances and the like.
Although the Zr-based amorphous alloy has excellent amorphous forming ability, strength and hardness, and the amorphous forming ability of the amorphous alloy can be improved through the blending of the components, the strength of most Zr-based amorphous alloys is below 2000MPa, or the amorphous alloy with high strength, excellent forming ability and low cost is less, so that the industrial application of the amorphous alloy is hindered. For example, the amorphous alloy of the ZrCuNiAl system has the amorphous forming capability exceeding cm, and the system does not contain a toxic element Be, but the strength of the system is below 1900MPa, although the amorphous alloy of the ZrCuAgAlCo system not only has the amorphous forming capability exceeding cm, but also has higher strength, the breaking strength of the amorphous alloy reaches 2200MPa, but the amorphous alloy contains noble metals, so that the raw material acquisition is limited.
The development of the amorphous alloy which has high strength and high hardness and the raw material of which does not contain noble metal has a promoting effect on the application and development of the amorphous alloy.
Disclosure of Invention
The invention provides a large-size zirconium-based amorphous alloy with high strength and high hardness and a preparation method thereof, and aims to solve the technical problem that an amorphous alloy without precious metals cannot have both high strength and high hardness.
In order to solve the technical problems, the invention provides a large-size zirconium-based amorphous alloy with high strength and high hardness, and the atomic percentage expression of the large-size zirconium-based amorphous alloy is as follows: zr a Cu b Ni c Al d Ti e Fe f Hf g M r (ii) a Wherein M is one or more of Y, dy, lu, ho, yb, ce, rh and Os; a is more than 45 and less than 55; b is more than 20 and less than 30; c is more than 5 and less than 10; d is more than 5 and less than 10; e is more than 0 and less than 5; f is more than 0 and less than 5; g is more than 0 and less than 2; r is more than or equal to 0 and less than 0.5.
In another aspect, the present invention further provides a method for preparing a large-size zirconium-based amorphous alloy with both high strength and high hardness, comprising the following steps: step S1, preparing the components of each metal raw material according to the atomic ratio as described in claim 1; s2, performing electric arc premelting on all Hf and a proper amount of Zr to obtain a premelted ingot; s3, performing vacuum induction melting on the pre-melted ingot and the residual metal raw materials, and pouring to obtain a melted ingot; and S4, carrying out die casting on the smelted cast ingot to obtain the large-size zirconium-based amorphous alloy with high strength and high hardness.
The large-size zirconium-based amorphous alloy with high strength and high hardness and the preparation method thereof have the beneficial effects that the components with high strength and high hardness are obtained by selecting conventional elements and easily-obtained rare earth elements for compounding; the oxygen element is harmful to the forming capability of the amorphous alloy, the oxygen element of the amorphous alloy is reduced by adding a small amount of rare earth elements, the amorphous forming capability of the amorphous alloy is improved, and the application field of the product is enlarged by adding the toxic element Be instead of adding the toxic element Be.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an XRD pattern of a 5mm sample of example 1 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
fig. 2 is an XRD pattern of a 5mm sample of example 2 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
FIG. 3 is an XRD pattern of a 5mm sample of example 3 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
FIG. 4 is an XRD pattern of a 3mm sample of comparative example 1 of a large-sized zirconium-based amorphous alloy of the present invention having both high strength and high hardness;
FIG. 5 is a stress-strain diagram of a 3mm sample of example 1 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
FIG. 6 is a stress-strain diagram of a 3mm sample of example 2 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
FIG. 7 is a stress-strain diagram of a 3mm sample of example 3 of a large-sized zirconium-based amorphous alloy having both high strength and high hardness according to the present invention;
FIG. 8 is a stress-strain diagram of a 3mm sample of comparative example 1 of a large-size zirconium-based amorphous alloy having both high strength and high hardness according to the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to obtain the Zr-based bulk amorphous alloy with strong amorphous forming capability, high strength and high hardness, the invention provides the Zr-based bulk amorphous alloy which has multiple elements and is easy to obtain.
The invention provides a large-size zirconium-based amorphous alloy with high strength and high hardness, which has the atomic percentage expression as follows: zr a Cu b Ni c Al d Ti e Fe f Hf g M r (ii) a Wherein M is one or more of Y, dy, lu, ho, yb, ce, rh and Os; a is more than 45 and less than 55; b is more than 20 and less than 30; c is more than 5 and less than 10; d is more than 5 and less than 10; e is more than 0 and less than 5; f is more than 0 and less than 5; g is more than 0 and less than 2; r is more than or equal to 0 and less than 0.5.
Specifically, the invention takes zirconium as a main element, does not contain a toxic element Be which can remarkably improve the amorphous forming ability, improves the amorphous forming ability of the zirconium-based amorphous alloy, ensures the mechanical property of the zirconium-based amorphous alloy while improving the amorphous forming ability of the zirconium-based amorphous alloy through compounding of other elements, shows that Be, te, cd, hg and Pb belong to highly toxic elements during intravenous injection according to the medical classification of element toxicity (acute toxicity), co, mg, mn, nb, ni, zn and the like belong to toxic toxicity during intravenous injection, and the biological action of the element toxicity depends on the physicochemical properties of the element and the concentration of the element at the action part of an organism, so the invention abandons the highly toxic element Be, enlarges the suitable intake range, improves the tolerance of the organism and reduces the poisoning risk.
Specifically, when Ti is combined with two or more of Cu, ni, co, zn and Mn, the compressive strength and hardness of the obtained zirconium-based amorphous alloy can Be greatly improved, meanwhile, ti and Be are often added together in the prior art to play a synergistic effect of oxidation resistance and the like in the amorphous alloy forming process, but Be is a toxic element.
Specifically, oxygen is an element harmful to the forming capacity of the amorphous alloy, the doping of the oxygen is inevitably caused in the process from raw materials to forming, trace rare earth is preferentially combined with oxygen in the material smelting process, so that the oxygen content of the material is reduced, and the trace rare earth can generate chemical reaction in the smelting process to play a role in purifying partial impurities, so that heterogeneous nucleation of the material is reduced, namely the amorphous forming capacity of the material is improved.
In this embodiment, specifically, the critical dimension of the large-size zirconium-based amorphous alloy is not less than Φ 5mm.
In this embodiment, specifically, the compressive strength of the large-size zirconium-based amorphous alloy is not less than 2300MPa.
In this embodiment, specifically, the hardness of the large-size zirconium-based amorphous alloy is not less than 550Hv.
The invention also provides a preparation method of the large-size zirconium-based amorphous alloy with high strength and high hardness, which comprises the following steps: step S1, preparing the components of each metal raw material according to the atomic ratio as described in claim 1; s2, performing electric arc premelting on all Hf and a proper amount of Zr to obtain a premelted ingot; s3, performing vacuum induction melting on the pre-melted ingot and the residual metal raw materials, and pouring to obtain a melted ingot; and S4, carrying out die casting on the smelted cast ingot to obtain the large-size zirconium-based amorphous alloy with high strength and high hardness.
In this embodiment, specifically, the step S2 pre-smelting pre-smelts the refractory materials, so as to facilitate uniform smelting of each component in the subsequent flow.
In this embodiment, specifically, the vacuum degree of the vacuum induction melting in the step S3 is not higher than 20MPa, the lower the vacuum degree is, the better the vacuum degree is, and the product obtained when the vacuum degree is 20MPa can meet the performance requirement; wherein the inert gas for purging in vacuum environment comprises Ar and N 2 。
In this embodiment, specifically, in the step S3, the melting temperature is 1900-2000 ℃, and the melting time is 5-10min, so that the material is sufficiently and uniformly melted.
In this embodiment, specifically, in step S3, the casting temperature is 1200 ℃ to 1300 ℃, the casting is performed when the temperature is cooled to 1200 ℃ to 1300 ℃ after the melting is completed, and the casting is taken out for subsequent pressing after the cooling is completed.
In this embodiment, specifically, the die-casting mold for die-casting the smelting ingot in step S4 is a water-cooled copper mold, and the size and the shape of the die-casting mold can be adjusted according to requirements.
Example 1
The titanium-based amorphous alloy prepared by the embodiment comprises the following components: zr 50 Cu 24.8 Ni 9.8 Al 8.8 Ti 5 Fe 1 Hf 0.6
The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting part of Zr and Hf by adopting electric arc, and cooling and taking out after the Zr and Hf are completely smelted.
(2) Adding the pre-melted Zr-Hf pre-melted ingot and the rest raw materials into a crucible, putting the crucible into a vacuum melting furnace, vacuumizing to below 20Pa, washing gas twice, and turning on an induction melting power supply to heat to 1900-2000 ℃ for melting;
(3) And (3) cooling after the metal is completely melted, and when the temperature is reduced to 1200-1300 ℃, casting and cooling to room temperature in a mold with a regular shape.
(4) And (3) intercepting proper raw materials, carrying out vacuum induction copper die casting, and preparing alloy bars with the diameters of 3mm and 5mm by adopting a copper die.
Example 2
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows: zr 49.5 Cu 24.3 Ni 9.7 Al 8.6 Ti 4.6 Fe 2 Hf 1 Y 0.2 Ho 0.1 The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting part of Zr and Hf by adopting electric arc, and cooling and taking out after the Zr and Hf are completely molten.
(2) Adding the pre-melted Zr-Hf pre-melted ingot and the rest raw materials into a crucible, putting the crucible into a vacuum melting furnace, vacuumizing to below 20Pa, washing gas twice, and turning on an induction melting power supply to heat to 1900-2000 ℃ for melting;
(3) And (3) cooling after the metal is completely melted, and when the temperature is reduced to 1200-1300 ℃, casting and cooling to room temperature in a mold with a regular shape.
(4) And (3) intercepting proper raw materials, carrying out vacuum induction copper die casting, and preparing alloy bars with the diameters of 3mm and 5mm by adopting a copper die.
Example 3
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows: zr 49 Cu 24 Ni 9.6 Al 8.6 Ti 5 Fe 3 Hf 0.6 Ho 0.1 Ru 0.1 The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting part of Zr and Hf by adopting electric arc, and cooling and taking out after the Zr and Hf are completely molten.
(2) Adding the pre-melted Zr-Hf pre-melted ingot and the rest raw materials into a crucible, putting the crucible into a vacuum melting furnace, vacuumizing to below 20Pa, washing gas twice, and turning on an induction melting power supply to heat to 1900-2000 ℃ for melting;
(3) And (3) cooling after the metal is completely melted, and when the temperature is reduced to 1200-1300 ℃, casting and cooling to room temperature in a mold with a regular shape.
(4) And (3) intercepting proper raw materials, carrying out vacuum induction copper die casting, and preparing alloy bars with the diameters of 3mm and 5mm by adopting a copper die.
Comparative example 1
The composition of the zirconium-based amorphous alloy prepared in this comparative example was: zr 55 Cu 30 Ni 5 Al 10
The preparation method comprises the following steps:
(1) Weighing the components in proportion, adding the raw materials into a crucible, putting the crucible into a vacuum smelting furnace, vacuumizing to below 20Pa, washing gas twice, and turning on an induction smelting power supply to heat to 1900-2000 ℃ for smelting;
(2) And (3) cooling after the metal is completely melted, and when the temperature is reduced to 1200-1300 ℃, casting and cooling to room temperature in a mold with a regular shape.
(3) And (3) intercepting proper raw materials, carrying out vacuum induction copper die casting, and preparing an alloy bar with the diameter of 3mm by using a copper die.
The experimental data for examples 1-3 and comparative example 1 are shown in table 1.
TABLE 1 mechanical property table of phi 3mm sample of each example
| Compressive strength/MPa | Hardness Hv | |
| Example 1 | 2303 | 560 |
| Example 2 | 2380 | 570 |
| Example 3 | 2501 | 600 |
| Comparative example 1 | 1815 | 509 |
As can be seen from the data in Table 1 and the accompanying drawings of FIGS. 1-4, when the compound rare earth element is not contained in the comparative example 1, the XRD pattern thereof has a large number of needle-like peaks, and the amorphous forming ability is affected because the oxygen content is much greater than that of the examples, while the products of the examples 1-3 all show stable amorphous forming ability.
According to the above amorphous forming ability review, it can be seen from the accompanying fig. 5-8 that examples 1-3 are amorphous alloys, which exhibit distinct yield and fracture points in the range of 2300-2500MPa, while comparative example 1, which is inferior in amorphous forming ability, does not exhibit the stress-strain curve thereof.
In conclusion, the large-size zirconium-based amorphous alloy with high strength and high hardness and the preparation method thereof have the advantages that the components with high strength and high hardness are obtained by selecting conventional elements and compounding with rare earth elements which are easy to obtain; the oxygen element is harmful to the forming capability of the amorphous alloy, the oxygen element of the amorphous alloy is reduced by adding a small amount of rare earth elements, the amorphous forming capability of the amorphous alloy is improved, and the application field of the product is enlarged by adding the toxic element Be instead of the toxic element Be.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (6)
1. A large-size zirconium-based amorphous alloy is characterized in that,
Zr 50 Cu 24.8 Ni 9.8 Al 8.8 Ti 5 Fe 1 Hf 0.6 ；
Zr 49.5 Cu 24.3 Ni 9.7 Al 8.6 Ti 4.6 Fe 2 Hf 1 Y 0.2 Ho 0.1 ；
Zr 49 Cu 24 Ni 9.6 Al 8.6 Ti 5 Fe 3 Hf 0.6 Ho 0.1 Ru 0.1 ；
the critical dimension of the large-size zirconium-based amorphous alloy is not less than phi 5mm;
the compressive strength of the large-size zirconium-based amorphous alloy is not less than 2300MPa;
the hardness of the large-size zirconium-based amorphous alloy is not less than 550Hv.
2. A preparation method of a large-size zirconium-based amorphous alloy is characterized by comprising the following steps:
step S1, preparing the components of each metal raw material according to the atomic ratio as described in claim 1;
s2, performing electric arc premelting on all Hf and a proper amount of Zr to obtain a premelted ingot;
s3, performing vacuum induction melting on the pre-melted ingot and the residual metal raw materials, and pouring to obtain a melted ingot;
and S4, carrying out die casting on the smelted cast ingot to obtain the large-size zirconium-based amorphous alloy with high strength and high hardness.
3. The method according to claim 2,
the vacuum degree of the vacuum induction melting in the step S3 is not higher than 20MPa; wherein
The inert gas for washing gas in vacuum environment comprises Ar and N 2 。
4. The method according to claim 2,
in the step S3, the smelting temperature is 1900-2000 ℃, and the smelting time is 5-10min.
5. The method according to claim 2,
the pouring temperature in the step S3 is 1200-1300 ℃.
6. The method according to claim 2,
and the die-casting die for die-casting the smelting ingot in the step S4 is a water-cooling copper die.
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| CN115478234A (en) * | 2022-09-16 | 2022-12-16 | 盘星新型合金材料(常州)有限公司 | Be-free zirconium-based amorphous alloy with plasticity and preparation method thereof |
| CN115637395A (en) * | 2022-09-19 | 2023-01-24 | 盘星新型合金材料(常州)有限公司 | High-hardness large-size zirconium-based amorphous alloy with plastic deformation and preparation method thereof |
| CN115584446A (en) * | 2022-10-26 | 2023-01-10 | 盘星新型合金材料(常州)有限公司 | Large-size Zr-based amorphous alloy containing Nb and Si simultaneously and preparation method thereof |
| CN115584445A (en) * | 2022-10-26 | 2023-01-10 | 盘星新型合金材料(常州)有限公司 | Centimeter-level zirconium-based amorphous alloy with plasticity and preparation method thereof |
| CN116804258B (en) * | 2023-08-23 | 2023-10-27 | 南京工业大学 | Bulk zirconium-based amorphous alloy with high strength and high hardness and preparation method thereof |
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| EP2881488B1 (en) * | 2013-12-06 | 2017-04-19 | The Swatch Group Research and Development Ltd. | Bulk amorphous alloy made of beryllium-free zirconium |
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