CN115478234A - Be-free zirconium-based amorphous alloy with plasticity and preparation method thereof - Google Patents
Be-free zirconium-based amorphous alloy with plasticity 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 Be-free zirconium-based amorphous alloy with plasticity and a preparation method thereof, wherein the atomic percentage expression of the Be-free zirconium-based amorphous alloy is as follows: zr a Cu b Ni c Al d Nb e Fe f Hf g M r (ii) a Wherein a + b + c + d + e + f + g + r =100; m is a rare earth element; and 50 < a < 70; b is more than 10 and less than 20; c is more than 5 and less than 15; d is more than 5 and less than 15; e is more than 0 and less than 10; f is more than 0 and less than 10; g is more than 0 and less than 2; r is more than 0 and less than 0.5; the Be-free zirconium-based amorphous alloy with plasticity and the preparation method thereof take Zr and Cu as main elements, and the amorphous alloy has excellent mechanical properties on the basis of stable amorphous forming capability by compounding and regulating other elements; nb and Fe are added under the condition of abandoning toxic elements Be and noble metals Pd and Ag, the configuration entropy of the system is increased, the amorphous forming capability and stability of the zirconium-based amorphous alloy are improved, and the improvement on conductivity and plasticity is realizedPromoting effect is achieved.
Description
Technical Field
The invention belongs to the technical field of amorphous alloys, and particularly relates to a Be-free zirconium-based amorphous alloy with plasticity and a preparation method thereof.
Background
As a novel alloy material, the amorphous alloy has unique structural characteristics of long-range order and short-range order, so that the amorphous alloy has other properties superior to the alloy, such as high strength, high hardness, high corrosion resistance, self-sharpening property and the like, so that the amorphous alloy has wide application prospects in military, medical instruments, sports goods, electronic product parts, precision parts and the like.
The Zr-based amorphous alloy is an amorphous alloy with the amorphous alloy forming capability second to that of Pd-based amorphous alloy in an amorphous alloy system, but the Zr-based amorphous alloy usually contains toxic elements Be as the maximum amorphous forming capability, but does not contain toxic elements and precious metals, and the amorphous forming capability of the Zr-based amorphous alloy is not too high, and most of the amorphous alloys have elasticity and plasticity, so that the application and development of materials are limited to a certain extent.
Therefore, the development of the Be-free, cheap and plastic zirconium-based amorphous alloy without precious metals has a propulsion effect on the application and development of the amorphous alloy.
Disclosure of Invention
The invention provides a Be-free zirconium-based amorphous alloy with plasticity and a preparation method thereof, and aims to solve the problem of insufficient plasticity of the Be-free zirconium-based amorphous alloy.
In order to solve the technical problems, the invention provides a Be-free zirconium-based amorphous alloy with plasticity, which comprises the following atomic percent expressions: zr a Cu b Ni c Al d Nb e Fe f Hf g M r (ii) a Wherein a + b + c + d + e + f + g + r =100; m is a rare earth element; and 50 < a < 70; b is more than 10 and less than 20; c is more than 5 and less than 15; d is more than 5 and less than 15; e is more than 0 and less than 10; f is more than 0 and less than 10; g is more than 0 and less than 2; r is more than 0 and less than 0.5.
In another aspect, the invention further provides a preparation method of the Be-free zirconium-based amorphous alloy with plasticity, which comprises the following steps: s1, converting the components into mass ratios according to the atomic percentages as described in claim 1, and weighing and configuring the raw materials; s2, performing electric arc premelting on the refractory metal, hf and part of Zr to obtain a premelted material; s3, performing vacuum induction melting on the pre-melted material and the rest raw materials, maintaining the temperature at 1900-2000 ℃ for 5-10 min, ensuring that the pre-melted material is fully melted, cooling to 1200-1300 ℃ to be poured into an ingot, and taking out the ingot after complete cooling; and S4, die-casting the cast ingot in a copper mold to obtain the Be-free zirconium-based amorphous alloy with plasticity.
The preparation method has the beneficial effects that Zr and Cu are used as main elements, and other elements are compounded and regulated so that the amorphous alloy has excellent mechanical properties on the basis of stable amorphous forming capability; nb and Fe are added under the condition of abandoning toxic elements Be and noble metals Pd and Ag, so that the potential entropy of the system is increased, the amorphous forming capability and stability of the zirconium-based amorphous alloy are improved, and the promotion effect on the improvement of the conductivity and the plasticity is realized.
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 the 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 embodiments or the prior art descriptions 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 a stress-strain curve of a bar of example 1 of a Be-free zirconium-based amorphous alloy having plasticity according to the present invention;
FIG. 2 is a stress-strain curve of a bar of example 2 of a Be-free zirconium-based amorphous alloy having plasticity according to the present invention;
FIG. 3 is a stress-strain curve of a bar of example 3 of a Be-free zirconium-based amorphous alloy having plasticity according to the present invention;
fig. 4 is a stress-strain graph of the bar of example 4 of the Be-free zirconium-based amorphous alloy having plasticity according to the present invention;
fig. 5 is a stress-strain graph of the comparative example 1 bar material having plasticity of the Be-free zirconium-based amorphous alloy of 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a Be-free zirconium-based amorphous alloy with plasticity, which comprises the following atomic percentage expressions: zr a Cu b Ni c Al d Nb e Fe f Hf g M r (ii) a Wherein a + b + c + d + e + f + g + r =100; m is a rare earth element; and 50 < a < 70; b is more than 10 and less than 20; c is more than 5 and less than 15; d is more than 5 and less than 15; e is more than 0 and less than 10; f is more than 0 and less than 10; g is more than 0 and less than 2; r is more than 0 and less than 0.5.
In the embodiment, specifically, be has obvious amorphous forming capability, but because Be has toxicity, the invention abandons Be and selects other non-toxic elements for compounding so as to ensure that the amorphous alloy still keeps good amorphous forming capability.
In the embodiment, the noble metals such as Pd and Ag also have a positive influence on the amorphous forming ability, but due to cost factors, the invention selects conventional easily available metal elements to substitute for noble metals to be compounded in the amorphous alloy, and the selected conventional easily available metal elements are all low-cost industrial grade low-purity materials, so as to realize mass production.
In this embodiment, specifically, nb and Fe can jointly increase the potential entropy of the system in the system, thereby improving the amorphous forming ability of the zirconium-based amorphous alloy, improving the stability of the zirconium-based amorphous alloy, and simultaneously having a positive effect on the change of the electrical conductivity and the improvement of the plasticity.
In the present embodiment, it is preferable that: a + b + c + d + e + f + g + r =100; and 60 < a < 70; b is more than 12 and less than 17; c is more than 8 and less than 13; d is more than 8 and less than 12; 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 0 and less than 0.5.
In this embodiment, optionally, the M includes Y, dy, lu, ho, yb, ce, rh, os; the oxygen element is harmful to the amorphous forming capability of the amorphous alloy, but the oxygen element is doped into the amorphous alloy inevitably in the process from the raw material to the forming process, and the rare earth element such as Y and the like is added in the invention, so that the rare earth element preferentially reacts with the oxygen element in the smelting process to reduce the content of the oxygen element in the alloy components, thereby reducing the influence of the oxygen element and further improving the amorphous forming capability.
In this embodiment, specifically, the non-Be-based amorphous alloy having plasticity has an amorphous forming ability of not less than 4mm.
In this embodiment, specifically, the compressive strength of the Be-free zirconium-based amorphous alloy with plasticity is not lower than 1600MPa.
In the present embodiment, specifically, the vickers strength hv0.5 of the Be-free zirconium-based amorphous alloy having plasticity is not less than 520.
The invention also provides a preparation method of the Be-free zirconium-based amorphous alloy with plasticity, which comprises the following steps: s1, converting the components into mass ratios according to the atomic percentages as described in claim 1, and weighing and configuring the raw materials; s2, performing electric arc premelting on the refractory metal, hf and part of Zr to obtain a premelted material; s3, performing vacuum induction melting on the pre-melted material and the rest raw materials, maintaining the temperature at 1900-2000 ℃ for 5-10 min, ensuring that the pre-melted material is fully melted, cooling to 1200-1300 ℃ to be poured into an ingot, and taking out the ingot after complete cooling; and S4, die-casting the cast ingot in a copper mold to obtain the Be-free zirconium-based amorphous alloy with plasticity.
In this embodiment, specifically, the vacuum induction melting in step S3 includes: vacuum degree not greater than 10 -1 MPa; the protective gas comprises Ar and N 2 。
Example 1
The titanium-based amorphous alloy prepared by the embodiment comprises the following components: zr 62.4 Cu 15.4 Ni 9.9 Al 9.7 Nb 1 Fe 1 Hf 0.5 Y 0.1
The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) And (3) detecting the bar and the plate by XRD, wherein the bar is of an amorphous structure, and the plate is crystallized.
Example 2
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows:
Zr 62.1 Cu 15.1 Ni 9.7 Al 9.5 Nb 1 Fe 2 Hf 0.4 Y 0.1 Ho 0.1
the preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) The bar and the plate are detected by XRD, and are in amorphous structures.
Example 3
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows: zr 62.1 Cu 15.1 Ni 9.7 Al 9.5 Nb 2 Fe 1 Hf 0.4 Y 0.1 Ho 0.1 The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 cutting appropriate raw materials, carrying out vacuum induction copper die casting, and preparing the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) The bar and the plate are detected by XRD, and are in amorphous structures.
Example 4
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows: zr 61.4 Cu 15 Ni 9.6 Al 9.5 Nb 2 Fe 2 Hf 0.4 Y 0.1
The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 cutting appropriate raw materials, carrying out vacuum induction copper die casting, and preparing the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) And detecting the bar and the plate by XRD, wherein the bar and the plate are in amorphous structures.
Example 5
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows: zr 52.5 Cu 18.7 Ni 13.5 Al 13.1 Nb 1 Fe 1 Hf 0.1 Dy 0.1
The preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 cutting appropriate raw materials, carrying out vacuum induction copper die casting, and preparing the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) The bar and the plate are detected by XRD, and are in amorphous structures.
Example 6
The composition of the zirconium-based amorphous alloy prepared in the embodiment is as follows:
Zr 51.2 Cu 11.2 Ni 7.6 Al 14.2 Nb 6.8 Fe 6.8 Hf 1.8 Ho 0.2 Ce 0.2
the preparation method comprises the following steps:
(1) Weighing the components in proportion, firstly smelting Hf, nb and part of Zr by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after completely smelting.
(2) Adding pre-melted Zr-Hf-Nb 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 cutting appropriate raw materials, carrying out vacuum induction copper die casting, and preparing the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) The bar and the plate are detected by XRD, and are in amorphous structures.
Comparative example 1
The composition of the zirconium-based amorphous alloy prepared in this comparative example was: zr 63.8 Cu 15.5 Ni 10.1 Al 10 Hf 0.5 Y 0.1
The preparation method comprises the following steps:
(1) Weighing the components in proportion, smelting part of Zr and Hf by adopting an electric arc or high-temperature vacuum smelting furnace, and cooling and taking out after the Zr and the Hf are completely smelted.
(2) Adding pre-melted Zr-Hf 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 cutting appropriate raw materials, carrying out vacuum induction copper die casting, and preparing the alloy plate with the diameter of 3mm bar and 20 x 50 x 4mm by using the copper die.
(5) The bar and the plate are detected by XRD, and are in amorphous structures.
Hardness testing of the bars was performed using a vickers hardness tester and conductivity testing of the plate samples was performed using a digital eddy current metal conductivity meter, and the results of preferred examples 1 to 4 and comparative example 1 are shown in table 1 below.
TABLE 1
| Examples of the invention | Compressive strength/MPa | Hardness Hv0.5 | Conductivity% IACS |
| Example 1 | 1947 | 551 | 1.05 |
| Example 2 | 1960 | 562 | 1.06 |
| Example 3 | 1851 | 575 | 1.06 |
| Example 4 | 1837 | 571 | 1.07 |
| Comparative example 1 | 1982 | 557 | 1.04 |
The addition of a proper amount of Nb not only increases the disorder of the alloy atomic structure and improves the thermal stability of the material, but also a small amount of Nb is beneficial to improving the plasticity of the material. The addition of Fe element can reduce the free volume of the material and can cause the precipitation of nanocrystalline phase, so that the strength and the plasticity of the material are enhanced.
The addition of Nb and Fe can not only improve the compressive strength and hardness of the material, but also change the electrical conductivity of the material, and in the case of the change of one element, the electrical conductivity of Nb or Fe is changed along with the change of the other element, and the increase of the total amount of the two elements can also lead to the increase of the electrical conductivity. The simultaneous addition of Nb and Fe leads to more complicated nano structure in the material, and although the hardness and the plasticity of the material are improved, the strength of the material is not changed greatly.
In conclusion, the Be-free zirconium-based amorphous alloy with plasticity and the preparation method thereof have the advantages that Zr and Cu are used as main elements, and other elements are compounded and regulated so that the amorphous alloy has excellent mechanical properties on the basis of stable amorphous forming capability; nb and Fe are added under the condition of abandoning toxic elements Be and noble metals Pd and Ag, so that the potential entropy of the system is increased, the amorphous forming capability and stability of the zirconium-based amorphous alloy are improved, and the promotion effect on the improvement of the conductivity and the plasticity is realized.
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 (8)
1. A Be-free zirconium-based amorphous alloy with plasticity is characterized in that the atomic percent expression is as follows:
Zr a Cu b Ni c Al d Nb e Fe f Hf g M r (ii) a Wherein
a+b+c+d+e+f+g+r＝100；
M is a rare earth element; and
50＜a＜70；
10＜b＜20；
5＜c＜15；
5＜d＜15；
0＜e＜10；
0＜f＜10；
0＜g＜2；
0＜r＜0.5。
2. the plastic Be-free zirconium-based amorphous alloy according to claim 1, wherein:
a + b + c + d + e + f + g + r =100; and
60＜a＜70；
12＜b＜17；
8＜c＜13；
8＜d＜12；
0＜e＜5；
0＜f＜5；
0＜g＜2；
0＜r＜0.5。
3. the plastic Be-free zirconium-based amorphous alloy according to claim 1, wherein the amorphous alloy is a zirconium-based amorphous alloy,
the M comprises Y, dy, lu, ho, yb, ce, rh and Os.
4. The plastic Be-free zirconium-based amorphous alloy according to claim 1, wherein the amorphous alloy is a zirconium-based amorphous alloy,
the amorphous forming ability of the Be-free zirconium-based amorphous alloy with plasticity is not less than 4mm.
5. The plastic Be-free zirconium-based amorphous alloy according to claim 1, wherein the amorphous alloy is a zirconium-based amorphous alloy,
the compressive strength of the Be-free zirconium-based amorphous alloy with plasticity is not lower than 1600MPa.
6. The Be-free zirconium-based amorphous alloy with plasticity according to claim 1, wherein,
the Be-free zirconium-based amorphous alloy with plasticity has the Vickers strength Hv0.5 of not less than 520.
7. A preparation method of a Be-free zirconium-based amorphous alloy with plasticity is characterized by comprising the following steps:
s1, converting the components into mass ratios according to the atomic percentages as described in claim 1, and weighing and configuring the raw materials;
s2, performing electric arc premelting on the refractory metal, hf and part of Zr to obtain a premelted material;
s3, performing vacuum induction melting on the pre-melted material and the rest raw materials, maintaining the temperature at 1900-2000 ℃ for 5-10 min, ensuring that the pre-melted material is fully melted, cooling to 1200-1300 ℃ to be poured into an ingot, and taking out the ingot after complete cooling;
and S4, die-casting the cast ingot in a copper mold to obtain the Be-free zirconium-based amorphous alloy with plasticity.
8. The method according to claim 7,
the vacuum induction melting in the step S3 comprises the following steps:
vacuum degree not greater than 10 -1 MPa；
The protective gas comprises Ar and N 2 。
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| CN114032478A (en) * | 2021-11-11 | 2022-02-11 | 盘星新型合金材料(常州)有限公司 | Zr-based amorphous alloy with plasticity and preparation method thereof |
| CN114214575A (en) * | 2021-12-18 | 2022-03-22 | 东莞宜安新材料研究院有限公司 | Zirconium-based amorphous alloy material and preparation method thereof |
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Application publication date: 20221216 |