CN120060748B - Ultra-wide temperature range low-expansion cage metal composite material, preparation and application - Google Patents
Ultra-wide temperature range low-expansion cage metal composite material, preparation and applicationInfo
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- CN120060748B CN120060748B CN202510541928.9A CN202510541928A CN120060748B CN 120060748 B CN120060748 B CN 120060748B CN 202510541928 A CN202510541928 A CN 202510541928A CN 120060748 B CN120060748 B CN 120060748B
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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
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- 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
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- 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
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- 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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/007—Heat treatment of ferrous alloys containing Co
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- 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
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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
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- Engineering & Computer Science (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The invention belongs to the technical field of new materials, in particular to a low expansion cage metal composite material with ultra-wide temperature range, and preparation and application thereof, wherein the preparation method introduces Co phase into Re-Fe binary cage metal, effectively widens the low expansion temperature range thereof, then introduces alpha-Fe, the dual-phase structure of the Re-Fe-Co matrix and the alpha- (Fe/Co) is constructed, wherein the Re-Fe-Co shows negative thermal expansion, the alpha- (Fe, co) shows positive thermal expansion, and the thermal expansion behavior is regulated and controlled by controlling the Fe content to regulate the two-phase proportion, so that the ultra-wide temperature range low expansion cage metal composite material is obtained. The ultra-wide temperature range low expansion cage mesh metal composite material prepared by the method constructs a soft/hard heterostructure, the synthesis steps are simple and easy to realize, and the remarkable improvement of the ultra-wide temperature range low expansion performance and the mechanical strength is realized through a two-step method.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a low-expansion cage-mesh metal composite material with an ultra-wide temperature range, and preparation and application thereof.
Background
In the fields of high-temperature precise instruments, aerospace and the like, the dimensional stability of components is directly related to the performance and service life of equipment. Thus, there is a need to develop low expansion materials that can maintain dimensions in extremely high temperature environments. However, the low expansion materials currently available are limited in variety, and particularly materials that retain low expansion characteristics in high temperature environments are more scarce.
Although the ceramic material has certain high temperature resistance, the ceramic material has the defects of mechanical property and heat conduction and electric conduction, so that the ceramic material is difficult to meet the requirements of high-temperature precise application. Although the metallic material is excellent in heat conduction and electric conduction, the intermetallic compound with high-temperature low-expansion performance has inherent brittleness, and the low-expansion temperature area is often low, so that the metallic material is difficult to be applied to high-temperature environments.
To solve the above problems, composite materials are designed as an effective strategy. Traditional composite materials are prepared by solid phase sintering, however, the method often leads to limited improvement of mechanical properties, and mismatch of thermal expansion coefficients of two materials is easy to cause thermal cracking, so that the materials are invalid. Therefore, how to scientifically design and prepare a composite material which can keep low expansion characteristic under a high-temperature environment and has excellent mechanical properties is a research hot spot and a difficult point in the current material science field.
Disclosure of Invention
The invention discloses a low expansion cage mesh metal composite material with ultra-wide temperature range, and preparation and application thereof, so as to solve any one of the above and other potential problems in the prior art.
In order to solve the technical problems, the technical scheme of the invention is that the ultra-wide temperature range low-expansion cage metal composite material has a chemical formula of R 2Fe11Co6Fex, wherein x is more than 0 and less than or equal to 50, R is a rare earth element, and the ultra-wide temperature range low-expansion cage metal composite material has an R-Fe-Co phase and an alpha- (Fe, co) phase.
Further, the R-Fe-Co phase is a hard matrix phase, exhibits strong magnetism and has a Curie temperature as high as 800K, and the alpha- (Fe, co) phase is a plastic second phase, and improves the strength of the matrix phase by chemical combination.
Further, the R-Fe-Co phase is a hexagonal system, the space group is P6 3/mmc, the alpha- (Fe, co) phase is a cubic system, and the space group is Im-3m.
Further, the chemical formula of the ultra-wide temperature range low expansion cage metal composite material is Lu 2Fe11Co6Fe9, the Lu 2Fe11Co6Fe9 has low expansion characteristic in a temperature range of 110-800K, the linear expansion coefficient alpha l is 0.98 multiplied by 10 -6, and the compression strength reaches 1110Mpa.
Further, the chemical formula Y 2Fe11Co6Fe9 of the ultra-wide temperature range low expansion cage metal composite material is that Y 2Fe11Co6Fe9 shows low expansion characteristics in a temperature range of 110-800K, the thermal expansion coefficient alpha l＜3×10-6 and the compression strength intensity are less than 1110Mpa.
Further, the chemical formula of the ultra-wide temperature range low expansion cage metal composite material is Tb 2Fe11Co6Fe9, tb 2Fe11Co6Fe9 shows low expansion characteristics in a temperature range of 110-800K, the thermal expansion coefficient alpha l is smaller than 3X 10 -6, and the compression strength is less than 1110Mpa.
The ultra-wide temperature range low expansion cage metal composite material has a chemical formula of Lu 2Fe11Co6Fe15, and Lu 2Fe11Co6Fe15 has strong anisotropic characteristics.
The invention also provides a method for preparing the ultra-wide temperature range low expansion cage mesh metal composite material, which specifically comprises the following steps:
s1) preparing corresponding raw materials according to R-Fe-Co ternary cage metal and alpha- (Fe, co) phases;
S2) mixing the raw materials prepared in the step S1);
s3) smelting the mixed raw materials of the S2) uniformly through an electric arc furnace;
s4) placing the uniformly smelted sample in a protective atmosphere for annealing;
And S5) after the annealing is finished, obtaining the ultra-wide temperature range low expansion cage mesh metal composite material.
The ultra-wide temperature range low expansion cage mesh metal composite material has low expansion characteristic in a temperature range of 110-800K, a thermal expansion coefficient alpha l＜3×10-6 and a compressive strength of less than or equal to 1110Mpa
Further, the purity of the R-Fe-Co ternary cage metal raw material and the alpha-Fe raw material in the S1) is more than 99.9 percent.
Further, the annealing in the step S4) is specifically performed at the temperature of 1100 ℃ for at least 72 hours, and the protective atmosphere is inert gas.
The ultra-wide temperature range low expansion cage mesh metal composite material is applied to the fields of optical instruments, microelectronic devices and high-precision instruments in aerospace.
The invention has the technical effects that due to the adoption of the technical scheme, the invention provides the ultra-wide temperature range low-expansion cage metal composite material and the preparation method thereof, and the R-Fe-Co ternary precursor compound is prepared by introducing a proper amount of Co into R-Fe binary cage metal (R refers to rare earth elements). Then, alpha-Fe is introduced to form an R-Fe-Co ternary cage metal composite material, a soft/hard heterostructure is constructed, the synthesis steps are simple and easy to realize, and the remarkable improvement of ultra-wide temperature range low expansion performance and mechanical strength is respectively realized through a two-step method.
On one hand, the invention provides a preparation method of an ultra-wide temperature range low expansion cage metal composite material, which introduces Co phase into R-Fe binary cage metal, effectively widens the low expansion temperature range of the composite material, then introduces alpha-Fe, constructs a dual-phase structure of an R-Fe-Co matrix and alpha- (Fe/Co), wherein the R-Fe-Co shows negative thermal expansion, the alpha- (Fe, co) shows positive thermal expansion, and the thermal expansion behavior is regulated and controlled by regulating the two-phase proportion by controlling the Fe content, so as to obtain the ultra-wide temperature range low expansion cage metal composite material.
The ultra-wide temperature range low expansion cage mesh metal composite material prepared by the invention has excellent dimensional stability, high precision and long service life, and is remarkably characterized in that the shape and the size are not influenced by temperature change, and the constant length/volume in a specific temperature range, namely the zero thermal expansion characteristic, is realized.
The ultra-wide temperature range low-expansion cage mesh metal composite material provided by the invention has the characteristics of high strength in a high temperature range, and the shape and the size of the composite material are stable when the temperature changes. The material widens the operating temperature range and eliminates its intrinsic brittleness compared to intermetallic compounds. Meanwhile, compared with ceramic materials, the material has more excellent heat conduction and electric conduction performance, and the raw material cost is lower, thus providing possibility for practical application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of the refinement of the X-ray diffraction structure of a Lu 2Fe11Co6Fe9 biphasic powder at 300K when R=Lu, for a low-expansion composite material according to the invention;
FIG. 2 is a crystal structure diagram of the R-Fe-Co phase and the alpha- (Fe, co) phase according to the present invention;
FIG. 3 is a back-scattered electron diffraction microstructure of the R-Fe-Co phase and the alpha- (Fe, co) phase according to the invention;
Fig. 4 is a graph of the expansion of the R 2Fe11Co6Fex (r=lu, x=9, 15, 25 and 50) and α -Fe phase lines according to the present invention;
FIG. 5 is a graph of engineering stress strain curve and shaped sample at 300K for Lu 2Fe11Co6Fe9 according to the present invention.
Detailed Description
For a better understanding of the technical solution of the present invention, the following detailed description of the embodiments of the present invention refers to the accompanying drawings.
It should be understood that the described embodiments are only some, but not all, of the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without undue burden, are within the scope of the invention.
The terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The invention provides an ultra-wide temperature range low-expansion cage metal composite material, which has a chemical formula of R 2Fe11Co6Fex, wherein 0<X is less than or equal to 50, R is a rare earth element, the ultra-wide temperature range low-expansion cage metal composite material comprises Lu 2Fe11Co6Fe9, the Lu 2Fe11Co6Fe9 shows low expansion characteristic in a temperature range of 110-800K, and a linear expansion coefficient alpha l is 0.98 multiplied by 10 -6.
According to the preparation method, a Co phase is introduced into the R-Fe binary cage metal, a low expansion temperature region of the alloy is effectively widened, then alpha-Fe is introduced, a dual-phase structure of an R-Fe-Co matrix and alpha- (Fe/Co) is constructed, wherein the R-Fe-Co shows negative thermal expansion, the alpha- (Fe, co) shows positive thermal expansion, and the regulation and control of thermal expansion behavior are carried out by controlling the proportion of Fe content to regulate and control the two phases, so that the ultra-wide temperature range low expansion cage metal composite material is obtained.
The preparation method comprises the following steps:
S1) preparing corresponding raw materials according to R-Fe-Co and alpha- (Fe, co) phases, wherein the purity of the raw materials is more than 99.9%, the R-Fe-Co phase is hexagonal system, the space group is P6 3/mmc, the alpha- (Fe, co) phase is cubic system, and the space group is Im-3m.
S2) mixing the raw materials prepared in the step S1);
S3, evenly smelting the mixed raw materials by an electric arc furnace;
s4, placing the uniformly smelted sample in a protective atmosphere, and annealing at 1100 ℃ for at least 72h;
And S5, after the annealing is finished, the ultra-wide temperature range low expansion cage mesh metal composite material is obtained.
The protective atmosphere is an inert atmosphere.
Example 1:
the ultra-wide temperature range low expansion cage mesh metal composite material block with the components of Lu 2Fe11Co6Fe9 is prepared and synthesized by an arc furnace smelting method respectively:
The specific operation is carried out according to the following steps:
8g of Lu, fe and Co raw materials with the molar ratio of 2:20:6 are weighed. The raw materials are mixed in an electric arc furnace, the furnace body is vacuumized (the vacuum degree is less than 2 multiplied by 10 -3 Pa), and then the raw materials are repeatedly smelted for 4 times under the protection of inert gas Ar, and each time is 2min. The resulting sample was placed under an inert atmosphere and annealed at a temperature of 1100 ℃ for 72 hours. The X-ray diffraction result shows that the obtained product is a composite phase of Lu 2(Fe,Co)17 and alpha- (Fe, co) and has no other impurities.
Example 2:
The preparation method comprises the steps of respectively synthesizing the ultra-wide temperature range low-expansion cage mesh metal composite material blocks with the components of Y 2Fe11Co6Fe9 by adopting an arc furnace smelting method:
The specific operation is carried out according to the following steps:
Weighing 8g of Y, fe and Co raw materials with the molar ratio of 2:20:6 respectively. Mixing raw materials in an arc furnace, and vacuumizing the furnace body
(Vacuum < 2X 10 -3 Pa), and then charging inert gas Ar to repeatedly smelt for 4 times each for 2min. The resulting sample was placed under an inert atmosphere at 1100 ℃ for an annealing time of 75 hours. The X-ray diffraction result shows that the obtained product is a composite phase of Y 2(Fe,Co)17 and alpha- (Fe, co) and has no other impurities.
Example 3:
The preparation method comprises the steps of respectively synthesizing Tb 2Fe11Co6Fe9 ultra-wide temperature range low-expansion cage mesh metal composite material blocks by adopting an arc furnace smelting method:
The specific operation is carried out according to the following steps:
Weighing 8g of Tb, fe and Co raw materials with the molar ratio of 2:20:6 respectively. The raw materials are mixed in an electric arc furnace, the furnace body is vacuumized (the vacuum degree is less than 2 multiplied by 10 -3 Pa), and then the raw materials are repeatedly smelted for 4 times under the protection of inert gas Ar, and each time is 2min. The resulting sample was placed under an inert atmosphere at 1100 ℃ for 80 hours of annealing time. The X-ray diffraction result shows that the obtained product is Tb 2(Fe,Co)17 and alpha- (Fe, co) composite phase, and has no other impurities.
The ultra-wide temperature range low expansion cage metal composite Lu2Fe11Co6Fe9、Y2Fe11Co6Fe9、Tb2Fe11Co6Fe9 obtained in examples 1, 2, and 3 was measured for linear expansion, which exhibited low expansion characteristics in the temperature ranges of 110 to 800k, and 110 to 800k, respectively, and the thermal expansion coefficient (α l) was less than 3×10 -6.
In the preparation method, the R-Fe-Co ternary cage metal is a hard matrix phase, and the alpha- (Fe, co) phase is a plastic second phase, so that a low expansion temperature region can be widened step by step and the mechanical behavior of the matrix phase can be improved by a two-step method, and the high-temperature region high-strength low expansion performance can be realized.
Fig. 1 is an X-ray diffraction structure refinement diagram of Lu 2Fe11Co6Fe9 powder at 300K when r=lu, from which it can be seen that the X-ray diffraction diagram based on the crystal structure simulation thereof is consistent with the X-ray diffraction diagram obtained by the experiment, illustrating the correctness of the structural model of the ultra-wide temperature range low expansion cage metal composite material of the present invention.
FIG. 2 is a crystal structure diagram of the R-Fe-Co phase and the alpha- (Fe, co) phase according to the present invention. The crystal structures of the invention are respectively hexagonal phases rich in rare earth and 2:17, and cubic phases composed of Fe and a small amount of Co elements.
FIG. 3 shows the back-scattered electron diffraction microstructure of the R-Fe-Co phase and the alpha- (Fe, co) phase, wherein the R-Fe-Co phase is taken as a base phase, the alpha- (Fe, co) phase is taken as a precipitation phase, and the phases are uniformly mixed without component segregation.
Fig. 4 is a graph of the linear expansion of R 2 Fe11Co6Fex (r=lu, x=9, 15, 25 and 50) according to the present invention, and it is known from the linear expansion curve of Lu 2Fe11Co6Fex according to the present invention that the thermal expansion can be controlled by controlling the doping ratio of Fe, and the thermal expansion coefficient is 0.98×10 -6 at 110-800K because the component Lu2Fe11Co6Fe9 exhibits zero expansion.
FIG. 5 is a graph showing the engineering stress strain curve of Lu 2Fe11Co6Fe9 at 300K according to the present invention, from which it is known that the low expansion composite material described above exhibits excellent mechanical properties, and has a compressive strength of 1110MPa and workability.
The metal composite material with ultra-wide temperature range and low expansion cage mesh, the preparation and the application provided by the embodiment of the application are described in detail. While the foregoing examples have been provided to assist those of ordinary skill in the art in understanding the methods and concepts underlying the application, those skilled in the art will recognize that there may be variations in the embodiments and applications of the application in light of the foregoing, and that the application is not to be construed as limited to what is described herein.
Certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will appreciate that a hardware manufacturer may refer to the same component by different names. The description and claims do not take the form of an element differentiated by name, but rather by functionality. As referred to throughout the specification and claims, the terms "comprising," including, "and" includes "are intended to be interpreted as" including/comprising, but not limited to. By "substantially" is meant that within an acceptable error range, a person skilled in the art is able to solve the technical problem within a certain error range, substantially achieving the technical effect. The description hereinafter sets forth a preferred embodiment for practicing the application, but is not intended to limit the scope of the application, as the description is given for the purpose of illustrating the general principles of the application. The scope of the application is defined by the appended claims.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a product 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 product or system. Without further limitation, an element defined by the phrase "comprising one of the elements" does not exclude the presence of additional identical elements in a commodity or system comprising the element.
It should be understood that the term "and/or" as used herein is merely an association relationship describing the associated object, and means that there may be three relationships, e.g., a and/or B, and that there may be three cases where a exists alone, while a and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
While the foregoing description illustrates and describes the preferred embodiments of the present application, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as limited to other embodiments, and is capable of numerous other combinations, modifications and environments and is capable of changes or modifications within the scope of the inventive concept as expressed herein, either as a result of the foregoing teachings or as a result of the knowledge or technology of the relevant art. And that modifications and variations which do not depart from the spirit and scope of the application are intended to be within the scope of the appended claims.
Claims (7)
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| CN102888557A (en) * | 2011-07-18 | 2013-01-23 | 宝山钢铁股份有限公司 | High-strength and low-expansion coefficient alloy wire and manufacturing method thereof |
| CN112011717A (en) * | 2020-08-26 | 2020-12-01 | 北京科技大学 | A kind of high-strength low-expansion composite material and preparation method thereof |
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| WO2021215529A1 (en) * | 2020-04-23 | 2021-10-28 | 国立大学法人東京大学 | Thermoelectric conversion element and thermoelectric conversion device |
| CN115522133B (en) * | 2022-10-19 | 2023-06-23 | 北京科技大学 | A kind of isotropic low thermal expansion composite material and its preparation method and application |
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| CN102888557A (en) * | 2011-07-18 | 2013-01-23 | 宝山钢铁股份有限公司 | High-strength and low-expansion coefficient alloy wire and manufacturing method thereof |
| CN112011717A (en) * | 2020-08-26 | 2020-12-01 | 北京科技大学 | A kind of high-strength low-expansion composite material and preparation method thereof |
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