CN113073270A - Wide-temperature-area zero-expansion alloy with abnormal component fluctuation and preparation method thereof - Google Patents

Wide-temperature-area zero-expansion alloy with abnormal component fluctuation and preparation method thereof Download PDF

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CN113073270A
CN113073270A CN202110294895.4A CN202110294895A CN113073270A CN 113073270 A CN113073270 A CN 113073270A CN 202110294895 A CN202110294895 A CN 202110294895A CN 113073270 A CN113073270 A CN 113073270A
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alloy
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CN113073270B (en
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林鲲
张文斌
邢献然
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University of Science and Technology Beijing USTB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26—Methods of annealing
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
    • C21D1/773—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material under reduced pressure or vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C30/00—Alloys containing less than 50% by weight of each constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/04—Making ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60

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Abstract

The invention belongs to the field of phase change alloy preparation, and particularly relates to a wide-temperature-zone zero-expansion alloy with abnormal component fluctuation and a preparation method thereof. The atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation is Hf0.6Ti0.4Fe2+xWherein x is more than or equal to 0 and is more than or equal to 1. The zero-expansion alloy phase belongs to a hexagonal system,the Hf and Ti are distributed at 4f positions, the Fe is distributed at 2a and 6h positions, the excessive Fe occupies Hf/Ti positions, and the microstructure shows periodic alternation of Hf-rich and Ti-rich areas and macroscopically shows zero expansion in a wide temperature area. The invention has the beneficial effects that: the synthesis steps are simple and easy to realize, the continuous positive and negative thermal expansion coupling formed by periodic component fluctuation is more stable than that of a traditional two-phase composite structure, the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation shows zero-expansion characteristic in a temperature range of 100-500K, and the linear expansion coefficient alphal≤1.8×10‑6。

Description

Wide-temperature-area zero-expansion alloy with abnormal component fluctuation and preparation method thereof
Technical Field
The invention belongs to the field of phase change alloy preparation, and particularly relates to a wide-temperature-zone zero-expansion alloy with abnormal component fluctuation and a preparation method thereof.
Background
Most substances show the property of expansion and contraction with temperature, however, the dimensional change and the thermal stress caused by thermal expansion greatly shorten the service life and the application range of the material. In many precision instruments, such as aerospace (the difference between the negative and positive surface temperature of the surface material of an aircraft in space is large, and the surface material has large thermal stress), electronic equipment (the main reason for the failure of a multilayer ceramic capacitor is that the heat generated by a Si chip causes the thermal expansion mismatch between the capacitor and the surrounding materials). Therefore, the development of a novel zero expansion (ZTE) material (a material which does not change the size of the material per se along with the temperature change) is important for practical application, and has great scientific significance for disclosing the intrinsic mechanism. Approaches to achieving zero expansion of materials generally fall into two broad categories: (1) adjusting the Coefficient of Thermal Expansion (CTE) of the material from positive to zero or negative by chemical modification, such as changing the chemical composition, such as invar (Fe-36 Ni); (2) by mixing negative thermal expansion material with positive thermal expansion material to form composite material, such as two-phase alloy (Er-Fe-V-Mo) and cladding material (La (Fe, Si)13) -Cu. The invention designs a wide-temperature-zone zero-expansion alloy (100-420K) between single-phase and composite materials, which has periodic composition fluctuation and as-cast Hf0.6Ti0.4Fe2.5There is a periodic compositional gradient in the short range, expressed as a periodic alternation of positive-negative thermal expansion, but the long range shows a single phase structure exhibiting zero expansion in a wide temperature range. Unlike conventional composite or dual phase zero expansion materials formed by solid phase sintering of metal/ceramic matrices, Hf0.6Ti0.4Fe2.5The long-range zero expansion of the intermetallic compound is realized by the continuous change of the micro positive and negative thermal expansion, which brings smaller thermal stress to prolong the service life of the material. Novel mechanism for periodic concentration gradient to regulate thermal expansionImplying the development of zero expansion alloys and providing guidance for designing other zero expansion intermetallics.
Disclosure of Invention
The invention discloses a preparation method of a wide-temperature-zone zero-expansion alloy with abnormal component fluctuation, which aims to solve any of the technical problems and other potential problems in the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows: the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation has the atomic percentage expression of Hf0.6Ti0.4Fe2+xWherein x is 0-1.
Further, the zero expansion alloy phase belongs to the hexagonal system, wherein Hf and Ti are distributed in 4f sites, Fe is distributed in 2a and 6h sites, and excess Fe occupies Hf/Ti sites.
Further, the microstructure of the zero expansion alloy shows periodic alternation of Hf-rich and Ti-rich areas, and macroscopically shows zero expansion in a wide temperature area.
Further, the-Hf rich region exhibits positive expansion and the Ti rich region exhibits negative expansion, with the periodic compositional gradient being accompanied by continuous positive and negative thermal expansion coupling.
Further, the atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal composition fluctuation is Hf0.6Ti0.4Fe2.5Exhibits zero expansion characteristic and linear expansion coefficient alpha within the temperature range of 100-420KlIs 0.5X 10-6。
Another object of the present invention is to provide a method for preparing a wide-temperature-zone zero-expansion alloy having abnormal composition fluctuation, the method comprising the steps of:
s1) preparing high-purity raw materials of Hf, Ti and Fe;
s2) weighing the three raw materials in the S1) according to the stoichiometric ratio and mixing;
s3) smelting the mixed raw materials in inert gas for multiple times through an electric arc furnace until the mixed raw materials are uniform;
s4) polishing and brightening the uniformly smelted sample, then placing the sample in a protective atmosphere for storage, and then annealing, and after the annealing is finished, obtaining the wide-temperature-area zero-expansion alloy with abnormal component fluctuation.
Further, the purity of the raw material in the S1) is required to be more than or equal to 99.95%.
Further, the protective atmosphere in S4) is vacuum or inert gas, and the inert gas is argon.
Further, the annealing temperature in the S4) is 800-1200 ℃, and the annealing time is 3-10 d.
Furthermore, the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation shows zero-expansion characteristic and linear expansion coefficient alpha within the temperature range of 100-500Kl≤1.8×10-6。
Compared with the prior art, the high-performance zero-expansion intermetallic compound can keep approximate consistency of shape and size in a wide temperature zone including room temperature;
compared with the existing thermal expansion regulation mechanism, the invention discovers a new method for regulating thermal expansion, and based on the microstructure, the invention discovers that macroscopic zero expansion regulation can be realized through periodic thermal expansion continuous fluctuation. Has certain guiding significance to the discovery of novel thermal expansion materials and the development of novel thermal expansion regulation mechanisms.
Drawings
FIG. 1 shows a zero expansion intermetallic compound Hf according to the present invention0.6Ti0.4Fe2+xWhen x is 0.5, Hf0.6Ti0.4Fe2.5X-ray diffraction contrast of the powder (line 1) with the corresponding single-phase structure (line 2) at room temperature;
FIG. 2 shows a wide temperature range zero expansion component Hf0.6Ti0.4Fe2.5Micro-structure Electron Probe Microscopy (EPMA);
FIG. 3 shows an intermetallic compound Hf according to the present invention0.6Ti0.4Fe2.5Linear expansion diagram of (a).
Detailed Description
The technical solution of the present invention is further described with reference to the following specific embodiments.
The invention provides a high-performance zero-expansion intermetallic compound which can keep approximate consistency of shape and size in a wide temperature zone (100-500K) including room temperature, has no texture and has excellent isotropic zero-expansion performance; compared with the existing thermal expansion regulation mechanism, the invention discovers a new method for regulating thermal expansion, and based on the microstructure, the invention discovers that macroscopic zero expansion regulation can be realized through periodic thermal expansion continuous fluctuation. Has certain guiding significance to the discovery of novel thermal expansion materials and the development of novel thermal expansion regulation mechanisms.
The invention relates to a wide-temperature-zone zero-expansion alloy with abnormal component fluctuation, wherein the atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation is Hf0.6Ti0.4Fe2+xWherein x is 0-1.
The zero expansion alloy phase belongs to a hexagonal system, wherein Hf and Ti are distributed in the 4f position of the hexagonal system, Fe is distributed in the 2a and 6h positions of the hexagonal system, and excessive Fe occupies the Hf/Ti position.
2a(0,0,0,)4f(1/3,1/3,1/3).
The microstructure of the zero expansion alloy shows periodic alternation of Hf-rich and Ti-rich areas and macroscopically shows zero expansion of a wide temperature area.
the-Hf rich region exhibits positive expansion and the Ti rich region exhibits negative expansion, with the periodic compositional gradient being accompanied by continuous positive and negative thermal expansion coupling.
The atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation is Hf0.6Ti0.4Fe2.5。
A method for preparing a wide-temperature-zone zero-expansion alloy with abnormal composition fluctuation, which comprises the following steps:
s1) preparing high-purity raw materials of Hf, Ti and Fe;
s2) weighing the three raw materials in the S1) according to the stoichiometric ratio and mixing;
s3) smelting the mixed raw materials in inert gas for multiple times through an electric arc furnace until the mixed raw materials are uniform;
s4) polishing and brightening the uniformly smelted sample, then placing the sample in a protective atmosphere for storage, and then annealing, and after the annealing is finished, obtaining the wide-temperature-area zero-expansion alloy with abnormal component fluctuation.
The purity of the raw material in the S1) is required to be more than or equal to 99.95 percent.
The protective atmosphere in the S4) is vacuum or inert gas, and the inert gas is argon.
The annealing temperature in the S4) is 800-1200 ℃, and the annealing time is 3-7 d.
The wide-temperature-zone zero-expansion alloy with abnormal component fluctuation shows zero-expansion characteristic and linear expansion coefficient alpha within the temperature range of 100-500Kl≤1.8×10-6。
Example 1:
preparation of the Standard stoichiometric composition of the invention is Hf0.6Ti0.4Fe2The intermetallic compound is synthesized by an electric arc furnace smelting method, and the reaction equation is as follows:
0.6×Hf+0.4×Fe+2.0×Fe＝Hf0.6Ti0.4Fe2
the specific operation is carried out according to the following steps:
5g of Hf, Ti and Fe raw materials with the molar ratio of 0.6:0.4:2.0 are weighed. Placing the raw material in an electric arc furnace, vacuumizing the furnace body (vacuum degree)<2.0×10-3Pa), filling inert gas into the furnace body after vacuumizing, and repeatedly smelting for 3-5 times under the protective gas atmosphere, wherein each time is 1-2min until the mixture is uniform. The sample is annealed at 800 ℃ for 7 days under vacuum or inert atmosphere. The X-ray diffraction result shows that the obtained product is macroscopically a single phase with a C14 structure and has no other impurity phases.
Example 2
Preparation of the non-stoichiometric composition of Hf in the present invention0.6Ti0.4Fe2.5The isotropic zero-expansion intermetallic compound block is synthesized by adopting an electric arc furnace smelting method, and the reaction equation is as follows:
0.6×Hf+0.4×Fe+2.5×Fe＝Hf0.6Ti0.4Fe2.5
the specific operation is carried out according to the following steps:
weighing Hf, Ti and Ti in a molar ratio of 0.6:0.4:2.5 respectively,5g of Fe raw material. Placing the raw material in an electric arc furnace, vacuumizing the furnace body (vacuum degree)<2.0×10-3Pa), filling inert gas into the furnace body after vacuumizing, and repeatedly smelting for 3-5 times under the protective gas atmosphere, wherein each time is 1-2min until the mixture is uniform. The sample is annealed at 1000 ℃ for 6 days under vacuum or inert atmosphere. The X-ray diffraction result shows that the obtained product is macroscopically a single phase with a C14 structure and has no other impurity phases.
For the non-stoichiometric zero expansion material Hf obtained in example 20.6Ti0.4Fe2.5Measuring linear expansion, and showing zero expansion characteristic and linear expansion coefficient (alpha) in a wide temperature range of 100-420Kl) Is 0.5X 10-6In addition, to the non-stoichiometric ratio Hf0.6Ti0.4Fe2.9The linear expansion is measured to show low thermal expansion in the temperature range of 100-500k, and the mechanical property is greatly improved.
FIG. 1 shows a zero expansion intermetallic compound Hf according to the present invention0.6Ti0.4Fe2+xWhen x is 0.6, Hf0.6Ti0.4Fe2.5The powder and a corresponding single-phase structure have an X-ray diffraction contrast pattern at room temperature, and different from the diffraction pattern of a traditional C14 single-phase structure material, the intermetallic compound of the invention shows a wider diffraction peak, which shows that the structure is extremely non-uniform;
FIG. 2 shows a wide temperature range zero expansion component Hf0.6Ti0.4Fe2.5Micro-structural Electron Probe Microscopy (EPMA) of (2), EPMA analysis found as xrd analysis, zero expansion intermetallic compound Hf0.6Ti0.4Fe2.5The microstructure of (a) is extremely uneven, showing a continuous distribution of Hf-rich and Ti-rich regions, whereas Fe is uniformly distributed over the entire range;
FIG. 3 shows an intermetallic compound Hf according to the present invention0.6Ti0.4Fe2.5The zero expansion temperature range is 100-420K.
Example 3:
preparation of the non-stoichiometric composition of Hf in the present invention0.6Ti0.4Fe2.2Isotropic zero expansionThe intermetallic compound block is synthesized by adopting an electric arc furnace smelting method, and the reaction equation is as follows:
0.6×Hf+0.4×Fe+2.2×Fe＝Hf0.6Ti0.4Fe2.2
the specific operation is carried out according to the following steps:
5g of Hf, Ti and Fe raw materials with the molar ratio of 0.6:0.4:2.2 are weighed. Placing the raw material in an electric arc furnace, vacuumizing the furnace body (vacuum degree)<2.0×10-3Pa), filling inert gas into the furnace body after vacuumizing, and repeatedly smelting for 3-5 times under the protective gas atmosphere, wherein each time is 1-2min until the mixture is uniform. The resulting sample was annealed at 1200 ℃ for 3 days under vacuum or inert atmosphere. The X-ray diffraction result shows that the obtained product is macroscopically a single phase with a C14 structure and has no other impurity phases.
The details of the wide temperature zone zero-expansion alloy with abnormal component fluctuation and the preparation method thereof provided by the embodiments of the present application are described above. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core ideas; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
As used in the specification and claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
It should be understood that the term "and/or" as used herein is merely one type of association that describes an associated object, meaning that three relationships may exist, e.g., a and/or B may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.

Claims (10)

1. The wide-temperature-zone zero-expansion alloy with abnormal component fluctuation is characterized in that the atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal component fluctuation is Hf0.6Ti0.4Fe2+xWherein x is 0-1.
2. The wide temperature range zero expansion alloy with anomalous composition fluctuations in claim 1 wherein the zero expansion alloy phase is of the hexagonal system with Hf, Ti distributed in the 4f sites, Fe distributed in the 2a and 6h sites, and excess Fe occupying the Hf/Ti sites.
3. The wide temperature range zero expansion alloy with anomalous composition fluctuations of claim 1, wherein the microstructure of the zero expansion alloy is represented by periodic Hf-rich, Ti-rich regions alternating and macroscopically represented by wide temperature range zero expansion.
4. The wide-temperature-zone zero-expansion alloy with anomalous composition fluctuations in claim 3, wherein the-Hf rich region exhibits positive expansion and the Ti rich region exhibits negative expansion, and wherein the periodic compositional gradient is accompanied by continuous positive and negative thermal expansion coupling.
5. The wide-temperature-zone zero-expansion alloy with abnormal composition fluctuation according to claim 1, wherein the atomic percent expression of the wide-temperature-zone zero-expansion alloy with abnormal composition fluctuation is Hf0.6Ti0.4Fe2.5，Exhibits zero expansion characteristic and linear expansion coefficient alpha within the temperature range of 100-420KlIs 0.5X 10-6。
6. A method for preparing a wide-temperature-zone zero-expansion alloy having abnormal composition fluctuation,
the method specifically comprises the following steps:
s1) preparing high-purity raw materials of Hf, Ti and Fe;
s2) weighing the three raw materials in the S1) according to the stoichiometric ratio and mixing;
s3) smelting the mixed raw materials in inert gas for multiple times through an electric arc furnace until the mixed raw materials are uniform;
s4) polishing and brightening the uniformly smelted sample, then placing the sample in a protective atmosphere for storage, and then annealing, and after the annealing is finished, obtaining the wide-temperature-area zero-expansion alloy with abnormal component fluctuation.
7. The method as claimed in claim 6, wherein the raw material purity of S1) is equal to or more than 99.95%.
8. The method as claimed in claim 6, wherein the protective atmosphere in S4) is vacuum or inert gas, and the inert gas is argon.
9. The method as claimed in claim 6, wherein the annealing in S4) is performed at a temperature of 800-1200 ℃ for 3-10 d.
10. The method according to claim 7, wherein the wide-temperature-zone zero-expansion alloy with abnormal composition fluctuation exhibits zero-expansion characteristics within a temperature range of 100-500K and a linear expansion coefficient alphal≤1.8×10-6。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115323233A (en) * 2022-08-19 2022-11-11 北京科技大学 High-temperature zero-expansion alloy material and preparation method thereof

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