Preparation and application of high-strength low-expansion Laves phase intermetallic compound

By preparing high-strength, low-expanding Laves phase intermetallic compounds, the problem of dimensional instability of metal materials under temperature changes is solved, dimensional stability and high strength within a specific temperature range are achieved, and the application temperature range is broadened.

CN120443058AActive Publication Date: 2025-08-08UNIV OF SCI & TECH BEIJING
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Patent Information

Application Number
CN202510948657.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-10
Publication Date
2025-08-08
Estimated Expiration
2045-07-10

AI Technical Summary

Technical Problem

The dimensional instability problems caused by thermal expansion and contraction of existing metal materials under temperature changes affect the performance and reliability of precision equipment.

Method used

Fe2Bx, a high-strength low-expanded Laves phase intermetallic compound (Zr0.65Nb0.35) was prepared. By introducing B element, the low-expansion temperature zone is broadened and the thermal expansion behavior is optimized. The arc furnace smelting and annealing process are used to form the Fd-3m space group structure of the cubic crystal system.

Benefits of technology

It exhibits low expansion characteristics within the temperature range of 120~370K, with a linear expansion coefficient of -0.76×10-6 to 1.99×10-6, a compression strength of 650MPa to 1059MPa, and a stable material shape and dimensions, suitable for precision instruments and temperature-sensitive equipment.

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Abstract

The invention discloses preparation and application of a Laves phase intermetallic compound with high strength and low expansion. The chemical formula of the high-strength low-expansion Laves phase intermetallic compound is (Zr0. 65Nb0. 35) Fe2Bx, x is larger than or equal to 0.05 and smaller than or equal to 0.2, the crystal structure is a cubic system, the space group is Fd-3m, Zr and Nb occupy 8a (0, 0, 0) sites, and Fe occupies 16d (5 / 8, 5 / 8 and 5 / 8) sites. And the Curie temperature reaches 370K. The element B is introduced into the (Zr, Nb) Fe2 ternary metal, a low-expansion temperature zone is effectively widened, the thermal expansion behavior is regulated and controlled, and the obtained high-strength low-expansion Laves phase intermetallic compound has excellent thermal stability and high precision, has the remarkable characteristics that the shape and the size are not influenced by temperature change, and is suitable for large-scale production. The constant length / volume, namely low thermal expansion characteristic, in a specific temperature interval range is realized.
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Description

Technical Field

[0001] The present invention belongs to the technical field of new materials, and in particular relates to the preparation and application of a Laves phase intermetallic compound with high strength and low expansion. Background Art

[0002] Research on the thermal stability of precision device materials is extremely valuable. The thermal expansion and contraction of traditional metal materials can cause deformation of instrument components, leading to a series of problems in precision equipment (such as optoelectronic systems, aerospace components, and integrated circuits), such as dimensional mismatch, mechanical stress concentration, and even functional failure. Therefore, the development of functional materials that maintain dimensional stability despite temperature fluctuations has become a key technological need.

[0003] Low-expansion materials, through sophisticated crystal and magnetic structural design, are able to maintain stable lattice parameters across a wide temperature range. This unique property has attracted widespread attention in cutting-edge technologies requiring submicron dimensional accuracy, offering irreplaceable application prospects in aerospace, precision optical instruments, microelectronic packaging, and high-precision measurement tools. Metal-based low-expansion materials, with their superior overall performance (such as excellent mechanical strength, thermal conductivity, and processability), are considered the material category with the greatest potential for engineering applications. The most representative example is the Invar alloy system, with a century-long history of application. It has played a vital role in precision instruments, watches, and other fields, and continues to be optimized and developed. Summary of the Invention

[0004] The present invention discloses a preparation and application of a Laves phase intermetallic compound with high strength and low expansion, so as to solve any of the above and other potential problems in the prior art.

[0005] In order to solve the above technical problems, the technical solution of the present invention is: a Laves phase intermetallic compound with high strength and low expansion, the chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B x , wherein 0.05≤x≤0.2, and the high-strength, low-expansion Laves phase intermetallic compound has a cubic crystal system, a space group of Fd-3m, Zr and Nb occupy the 8a (0, 0, 0) site, and Fe occupies the 16d (5 / 8, 5 / 8, 5 / 8) site; exhibits ferromagnetism, and the Curie temperature reaches 370K.

[0006] Furthermore, the linear expansion coefficient (α l ) is not higher than 1.99×10 -6, the compression strength is not higher than 1059MPa.

[0007] Furthermore, the chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.05 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (α l ) is -0.76×10 -6 , the compressive strength is 650MPa.

[0008] Furthermore, the chemical formula of the high-strength zero-expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.1 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (α l ) is 0.20×10 -6 , the compressive strength is 805 MPa.

[0009] Furthermore, the chemical formula of the high-strength zero-expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.15 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (α l ) is 0.91×10 -6 , the compressive strength is 1059MPa.

[0010] Furthermore, the chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.2 , which exhibits low expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (α l ) is 1.99×10 -6 , the compressive strength is 960MPa.

[0011] Another object of the present invention is to provide a method for preparing the above-mentioned high-strength, low-expansion Laves phase intermetallic compound, which specifically comprises the following steps: S1) According to the high strength and low expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B x Prepare the corresponding raw materials; S2) mixing the raw materials prepared in S1); S3) uniformly melting the raw materials mixed in S2) by an electric arc furnace; S4) annealing the uniformly melted sample under a protective atmosphere; S5) After annealing, a high-strength and low-expansion Laves phase intermetallic compound is obtained.

[0012] Furthermore, the Zr and Nb in S1) 、 The purity of Fe metal raw materials is >99.9%.

[0013] Furthermore, the specific annealing process in S4) is: annealing at a temperature not lower than 1200° C. for at least 24 hours; the protective atmosphere is an inert gas.

[0014] The high-strength, low-expansion Laves-phase intermetallic compound described above has important applications in precision instrumentation, including standard metrology tools (e.g., gauge blocks and standard rulers), temperature measurement devices (e.g., thermometers), spatial positioning instruments (e.g., distance meters and gravimeter components), precision timing equipment (e.g., clock balances), microwave resonant devices, and optical instrument components. Furthermore, its excellent temperature-regulating properties make it a functional component of thermobimetallic materials, playing a key role in temperature-sensitive devices.

[0015] The technical effect of the present invention is as follows: Due to the adoption of the above technical solution, the present invention provides a high-strength and low-expansion Laves phase intermetallic compound and a preparation method thereof, which exhibits low expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (αl) is -0.76×10 -6 , 0.20×10 -6 , 0.91×10 -6 , and 1.99×10 -6 , where (Zr 0.65 Nb 0.35 )Fe2B 0.1 and (Zr 0.65 Nb 0.35 )Fe2B 0.15 They exhibit high compressive strength at room temperature, which are 805MPa and 1059MPa respectively, and therefore have potential application prospects.

[0016] On the one hand, the present invention provides a method for preparing a high-strength, low-expansion Laves phase intermetallic compound. The preparation method introduces the B element into the (Zr, Nb)Fe2 ternary metal, effectively widens its low-expansion temperature range, regulates its thermal expansion behavior, and optimizes its mechanical properties.

[0017] On the other hand, the high-strength, low-expansion Laves phase intermetallic compound prepared by the present invention has excellent thermal stability and high precision. Its notable feature is that its shape and size are not affected by temperature changes, and it achieves constant length / volume within a specific temperature range, that is, low thermal expansion characteristics.

[0018] The high-strength, low-expansion Laves-phase intermetallic compound provided by the present invention boasts high strength and maintains stable shape and size despite temperature fluctuations. Compared to intermetallic compounds, this material has a wider operating temperature range and improved mechanical behavior, facilitating its processing and application. Furthermore, compared to other solid materials, this material exhibits superior electrical properties, opening up the possibility of practical engineering applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0020] Figure 1 The X-ray diffraction pattern of the Nb and B-doped ZrFe2-type Laves phase intermetallic compound powder at 300K of the present invention; Figure 2 This is a crystal structure diagram of the Nb and B-doped ZrFe2-type Laves phase intermetallic compound of the present invention; Figure 3 The linear expansion diagram of the Nb and B doped ZrFe2 type Laves phase intermetallic compound of the present invention; Figure 4 This is the stress-strain curve of the Nb and B-doped ZrFe2-type Laves phase intermetallic compound described in the present invention. DETAILED DESCRIPTION

[0021] In order to better understand the technical solution of the present invention, the embodiments of the present invention are described in detail below with reference to the accompanying drawings.

[0022] It should be understood that the embodiments described are only a portion of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] The terms used in the embodiments of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The singular forms "a", "an", "the" and "the" used in the embodiments of the present invention and the appended claims are also intended to include plural forms unless the context clearly indicates otherwise.

[0024] like Figure 1 and Figure 2As shown, the present invention provides a Laves phase intermetallic compound with high strength and low expansion, and the chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B x , wherein 0.05≤x≤0.2, and the crystal structure of the high-strength, low-expansion Laves phase intermetallic compound is cubic, the space group is Fd-3m, Zr and Nb occupy the 8a (0, 0, 0) site, and Fe occupies the 16d (5 / 8, 5 / 8, 5 / 8) site.

[0025] The high-strength low-expansion Laves phase intermetallic compound is ferromagnetic and has a Curie temperature of approximately 370K. The chemical formula of the high-strength low-expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.05、(Zr0.65 Nb 0.35 )Fe2B 0.1 、(Zr 0.65Nb0.35 )Fe2B 0.15 and (Zr 0.65 Nb 0.35 )Fe2B 0.2 , which exhibit low expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient (α l ) were -0.76×10 -6 , 0.20×10-6, 0.91×10 -6 , and 1.99×10 -6 The (Zr 0.65 Nb 0.35 )Fe2B 0.1 、(Zr 0.65 Nb 0.35 )Fe2B 0.15 The compressive strengths are 805 MPa and 1059 MPa respectively. Figure 4 shown.

[0026] The preparation method comprises the following steps: S1) According to the high strength and low expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B x Prepare the corresponding raw materials S2) mixing the raw materials prepared in S1); S3) The mixed raw materials are melted uniformly in an electric arc furnace. The specific process is as follows: first, the furnace body is vacuumed (vacuum degree <2.5×10 -3Pa), repeated melting at least twice under this vacuum condition or inert gas protection, each time for at least 1 minute, and auxiliary electromagnetic stirring with a current of 1A can be used to homogenize the alloy; S4) annealing the uniformly melted sample at 1200°C for at least 24 hours under a protective atmosphere; S5) After annealing, a high-strength and low-expansion Laves phase intermetallic compound is obtained.

[0027] The protective atmosphere is an inert atmosphere.

[0028] Example 1: The composition of the present invention is (Zr 0.65 Nb 0.35 )Fe2B 0.05 , and zero-expansion intermetallic compound blocks were synthesized by electric arc furnace melting method, and the reaction equations are as follows: 0.65Zr+ 0.35Nb+ 2Fe+ 0.05B =(Zr 0.65 Nb 0.35 )Fe2B 0.05 The specific operation is as follows: Weigh the raw materials of Zr, Nb, Fe and B with a molar ratio of 0.65:0.35:2:0.05 and place them in an electric arc furnace. Evacuate the furnace (vacuum degree <2.5×10 -3 Pa), and then repeatedly melted twice under inert gas protection, each time for 1 minute, and assisted by electromagnetic stirring with a current of 1A to homogenize the alloy. The obtained sample was annealed at 1200℃ for 24 hours under vacuum or inert atmosphere. X-ray diffraction results showed that the obtained product was (Zr 0.65 Nb 0.35 )Fe2B 0.05 Pure phase.

[0029] The high strength zero expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B 0.05 , measure linear expansion, which shows zero expansion characteristics in the temperature range of 120~370K, the linear expansion coefficient (α l ) is -0.76×10 -6 ,like Figure 3 shown.

[0030] The Laves phase intermetallic compound prepared in the method of the present invention can broaden the low expansion temperature range and improve the mechanical behavior of the matrix phase by doping with the B element, thereby achieving high strength and low expansion performance.

[0031] Example 2: The composition of the present invention is (Zr 0.65 Nb 0.35 )Fe2B 0.1 , and zero-expansion intermetallic compound blocks were synthesized by electric arc furnace melting method, and the reaction equations are as follows: 0.65Zr+ 0.35Nb+ 2Fe+ 0.1B =(Zr 0.65 Nb 0.35 )Fe2B 0.1 The specific operation is as follows: Weigh the raw materials of Zr, Nb, Fe and B with a molar ratio of 0.65:0.35:2:0.1 and place them in an electric arc furnace. Evacuate the furnace (vacuum degree <2.5×10 -3 Pa), repeated melting 3 times under vacuum conditions or inert gas protection, each time for 1.5 minutes, and electromagnetic stirring with a current of 1A can be used to homogenize the alloy. The obtained sample was annealed at 1300℃ for 26 hours under inert atmosphere. X-ray diffraction results show that the obtained product is (Zr 0.65 Nb 0.35 )Fe2B 0.1 Pure phase.

[0032] The high strength zero expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B 0.1 , measure linear expansion, which shows zero expansion characteristics in the temperature range of 120~370K, the linear expansion coefficient (α l ) is 0.20×10 -6 ,like Figure 3 As shown, the compressive strength is 805MPa. Figure 4 shown.

[0033] The Laves phase intermetallic compound prepared in the method of the present invention can broaden the low expansion temperature range and improve the mechanical behavior of the matrix phase by doping with the B element, thereby achieving high-strength zero-expansion performance.

[0034] Example 3: The composition of the present invention is (Zr 0.65 Nb 0.35 )Fe2B 0.15 The zero-expansion intermetallic compound blocks were synthesized by electric arc furnace melting method, and the reaction equation is as follows: 0.65Zr+ 0.35Nb+ 2Fe+ 0.15B =(Zr 0.65 Nb 0.35 )Fe2B 0.15 The specific operation is as follows: Weigh 10 g of Zr, Nb, Fe, and B raw materials with a molar ratio of 0.65:0.35:2:0.15. Place the raw materials in an electric arc furnace and evacuate the furnace to a vacuum degree of <2.5×10 -3 Pa), and repeatedly melted under this vacuum condition for 4 times, each time for 2 minutes, and assisted by electromagnetic stirring with a current of 1A to homogenize the alloy. The obtained sample was annealed at 1210℃ for 30 hours under vacuum or inert atmosphere. X-ray diffraction results show that the main phase of the obtained product is (Zr 0.65 Nb 0.35 )Fe2B 0.15 .

[0035] The high strength zero expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B 0.15 Measuring linear expansion, it shows zero expansion characteristics in the temperature range of 120~370K, the linear expansion coefficient (α l ) is 0.91×10 -6 ,like Figure 3 As shown, the compressive strength is 1059 MPa. Figure 4 shown.

[0036] The Laves phase intermetallic compound prepared in the method of the present invention can broaden the low expansion temperature range and improve the mechanical behavior of the matrix phase by doping with the B element, thereby achieving strength zero expansion performance.

[0037] Example 4: The composition of the present invention is (Zr 0.65 Nb 0.35 )Fe2B 0.2 The low expansion intermetallic compound blocks were synthesized by electric arc furnace melting method, and the reaction equation is as follows: 0.65Zr+ 0.35Nb+ 2Fe+ 0.2B =(Zr 0.65 Nb 0.35 )Fe2B 0.2 The specific operation is as follows: Weigh 10 g of Zr, Nb, Fe, and B raw materials with a molar ratio of 0.65:0.35:2:0.2. Place the raw materials in an electric arc furnace and evacuate the furnace to a vacuum degree of <2.5×10 -3Pa), and then repeatedly melted under inert gas protection under this vacuum condition for 5 times, each time for 3 minutes, and assisted by electromagnetic stirring with a current of 1A to homogenize the alloy. The obtained sample was annealed at 1220℃ for 28 hours under vacuum or inert atmosphere. X-ray diffraction results show that the main phase of the obtained product is (Zr 0.65 Nb 0.35 )Fe2B 0.2 .

[0038] The linear expansion of the high-strength zero-expansion Laves phase intermetallic compounds obtained in Examples 1-4 was measured. The results showed that the low expansion characteristics were observed in the temperature range of 120-370 K. The linear expansion coefficient (α l ) is not higher than 1.99×10 -6 ,like Figure 3 shown.

[0039] The Laves phase intermetallic compound prepared in the method of the present invention can broaden the low expansion temperature range and improve the mechanical behavior of the matrix phase by doping with the B element, thereby achieving high strength and low expansion performance.

[0040] The above details the preparation and application of a high-strength, low-expansion Laves-phase intermetallic compound provided in the examples of this application. The above examples are intended only to facilitate understanding of the methods and core concepts of this application. Furthermore, those skilled in the art will appreciate variations in the specific implementation and scope of application based on the principles of this application. Therefore, this description should not be construed as limiting this application.

[0041] For example, certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that hardware manufacturers may use different nouns to refer to the same component. This specification and claims do not use differences in names as a way to distinguish components, but use differences in the functions of components as the criteria for distinction. For example, "including" and "comprising" mentioned throughout the specification and claims are open-ended terms, so they should be interpreted as "including / including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problems within a certain error range and basically achieve the technical effects. The subsequent description in the specification is a preferred embodiment of the present application, but the description is for the purpose of illustrating the general principles of the present application, and is not used to limit the scope of the present application. The scope of protection of the present application shall be as defined in the attached claims.

[0042] It should also be noted that the terms "include," "comprises," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a product or system comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such product or system. In the absence of further limitations, an element defined by the phrase "comprises a..." does not exclude the presence of other identical elements in the product or system comprising the element.

[0043] It should be understood that the term "and / or" as used herein is merely a description of the relationship between associated objects, indicating that three possible relationships exist. For example, "A and / or B" can represent: A exists alone, A and B exist simultaneously, or B exists alone. Furthermore, the character " / " in this document generally indicates that the associated objects are in an "or" relationship.

[0044] The above description shows and describes several preferred embodiments of the present application. However, as previously mentioned, it should be understood that the present application is not limited to the form disclosed herein and should not be construed as excluding other embodiments. Instead, the present application can be used in various other combinations, modifications, and environments and can be modified within the scope of the application concept described herein through the above teachings or technology or knowledge in the relevant field. Modifications and variations made by those skilled in the art that do not depart from the spirit and scope of the present application should be protected by the claims appended hereto.

Claims

1. A Laves phase intermetallic compound with high strength and low expansion, characterized in that: The chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B x , where 0.05≤x≤0.2, and the high-strength, low-expansion Laves phase intermetallic compound has a cubic crystal structure, a space group of Fd-3m, Zr and Nb occupy the 8a (0, 0, 0) site, and Fe occupies the 16d (5 / 8, 5 / 8, 5 / 8) site; the Curie temperature reaches 370K.

2. The high-strength, low-expansion Laves phase intermetallic compound according to claim 1, characterized in that: The linear expansion coefficient α of the high-strength and low-expansion Laves phase intermetallic compound l No more than 1.99×10 -6 , the compression strength is not higher than 1059MPa.

3. The high-strength, low-expansion Laves phase intermetallic compound according to claim 1, characterized in that: The chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.05 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient α l -0.76×10 -6 , the compressive strength is 650MPa.

4. The high-strength, low-expansion Laves phase intermetallic compound according to claim 1, characterized in that: The chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.1 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient α l 0.20×10 -6 , the compressive strength is 805 MPa.

5. The high-strength, low-expansion Laves phase intermetallic compound according to claim 1, characterized in that: The chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.15 , it exhibits zero expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient α l 0.91×10 -6 , the compressive strength is 1059MPa.

6. The high-strength, low-expansion Laves phase intermetallic compound according to claim 1, characterized in that: The chemical formula of the high strength and low expansion Laves phase intermetallic compound is (Zr 0.65 Nb 0.35 )Fe2B 0.2 , which exhibits low expansion characteristics in the temperature range of 120~370K, and the linear expansion coefficient α l 1.99×10 -6 , the compressive strength is 960MPa.

7. A method for preparing the high-strength, low-expansion Laves phase intermetallic compound according to any one of claims 1 to 6, characterized in that: The method specifically comprises the following steps: S1) According to the high strength and low expansion Laves phase intermetallic compound (Zr 0.65 Nb 0.35 )Fe2B x Prepare the corresponding raw materials; S2) mixing the raw materials prepared in S1); S3) uniformly melting the raw materials mixed in S2) by an electric arc furnace; S4) annealing the uniformly melted sample under a protective atmosphere; S5) After annealing, a high-strength and low-expansion Laves phase intermetallic compound is obtained.

8. The method according to claim 7, characterized in that The Zr in S1) 、 Nb 、 The purity of Fe metal raw materials is >99.9%.

9. The method according to claim 7, characterized in that The specific annealing process in S4) is: annealing at a temperature not lower than 1200° C. for at least 24 hours; the protective atmosphere is an inert gas.

10. Use of the high-strength, low-expansion Laves phase intermetallic compound according to any one of claims 1 to 6 in the field of precision instruments and temperature-sensitive equipment.

Citation Information

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