CN112695264A - Method for preparing large equiaxed grains with different orientations - Google Patents
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Abstract
A method for preparing large equiaxed grains with different orientations specifically comprises the following steps: rolling and deforming a metal material through a rolling mill, wherein the different rolling speeds and the different pressing quantities can cause different structures formed by the metal material, so as to obtain equiaxed grains with different orientations; then, carrying out quartz tube packaging on the samples subjected to different rolling deformation, and vacuumizing and filling inert gas for protection; then, carrying out high-temperature treatment on the packaged sample in a high-temperature heat treatment furnace, wherein the heat treatment time is more than or equal to 1 hour, and the temperature is cooled to room temperature along with the furnace, and the slower the cooling speed is, the better the cooling speed is; and finally, taking out the sample, observing the metallographic phase, determining the orientation by an EBSD (Electron Back-scattered diffraction) technology, and cutting the sample in different directions by a wire cutting machine to obtain large equiaxed grains with different orientations.
Description
Technical Field
The invention belongs to the field of material analysis, and particularly relates to a method for obtaining large equiaxial grains with different orientations in rolling deformation, high-temperature heat treatment, EBSD (Electron Back-scattered diffraction) and sampling modes in different directions.
Background
Before the material is actually applied, the material is often subjected to mechanical processing in different modes, such as forging, rolling, punching and forming and the like. And the mechanical processing causes severe deformation of the material, and the most main deformation modes are dislocation slip and twinning. The deformation degree of the material is mainly determined by the mechanical properties of the material, and the mechanical properties of the material are mainly related to the composition, the structure, the grain size and the like of the material. Often in order to obtain better mechanical properties of the material, fine equiaxed grains are prepared, such as the famous Hall-Petch grain refining effect. However, in order to better study the deformation mechanism of the material or macroscopic in-situ deformation study, etc., the preparation of large equiaxed grains and single crystal materials is the first choice for researchers. At present, most of materials belong to polycrystalline materials, so that the preparation of large equiaxed grains has great significance for the basic research of the polycrystalline materials.
Nuclear materials such as zirconium, hafnium and their alloys have a very low thermal neutron absorption cross section and good corrosion resistance, and are mainly used for cladding and control materials of reactors, etc. Zirconium, hafnium and their alloys are often prone to corrosion problems when in service in reactors. According to the current research, the crystal orientation has a large influence on the corrosion of the nuclear materials, and crystal planes with different orientations have different oxidation corrosion rates. In addition, zirconium, hafnium and their alloys need to be machined in different ways (e.g. rolling deformation) during the machining of the final product, and the machining results in the formation of a structure. The formation of the structure can influence the starting of a crystal sliding system and the formation of twin crystals, thereby influencing the mechanical property of the material. Therefore, it is important to find a method for producing large equiaxed grains of different orientations.
Disclosure of Invention
The invention provides a method for obtaining large equiaxial grains with different orientations by rolling deformation, high-temperature heat treatment, EBSD and sampling in different directions, which is a method for simply, effectively and accurately preparing large equiaxial grains.
The invention is obtained by the following technical scheme:
a method for preparing large equiaxed grains with different orientations is characterized by comprising the following specific steps:
1) firstly, rolling and deforming the metal material through a rolling mill, wherein the different rolling speeds and the different pressing quantities can cause different structures formed by the metal material, and then equiaxed grains with different orientations are obtained;
2) packaging the samples subjected to different rolling deformation by using a quartz tube, vacuumizing the quartz tube, and then filling inert gas for protection;
3) and carrying out high-temperature treatment on the packaged sample in a high-temperature heat treatment furnace, wherein the heat treatment temperature is the highest temperature of an alpha single-phase region, namely the temperature (preferably T) which is slightly lower than a phase transformation point (alpha → beta)(α→β)-10 ℃ of which T(α→β)Is the phase transition temperature of a metal material), the heat treatment time is more than or equal to 1 hour (preferably more than or equal to 3 hours, and the longer the time, the better), and the furnace is cooled to the room temperature, the slower the cooling speed, the better;
4) and taking out the sample, observing the metallographic phase, determining the orientation by an EBSD technology, and cutting the sample in different directions by a wire cutting machine to obtain large equiaxial grains with different orientations.
The method is particularly suitable for metal materials with the phase transition temperature of more than 1000 ℃, and large equiaxed grains with the size of more than or equal to 500 microns can be obtained by the method. The higher the phase transformation point of the selected metal material is, the larger the equiaxial crystal grains are finally obtained, and the equiaxial crystal grains in millimeter level can be obtained at most. In order to obtain extra-large equiaxed crystals, such as millimeter-scale, a metallic material with a high transformation point (transformation temperature greater than 1400 ℃) such as pure hafnium (α → β transformation point 1743 ℃) is preferred.
As a preferred technical scheme:
in the step 1), in order to obtain a circumferential basal plane structure, the rolling speed is 50-100r/min, and the feeding speed is 1-5 mm/period (most preferably, the rolling speed is 80r/min, and the feeding speed is 3 mm/period);
in the step 2), the quartz tube is preferably a high-temperature-resistant quartz tube, and the vacuum degree is less than 10-3And Mpa, and the inert gas is preferably high-purity argon.
The method obtains equiaxial grains with different orientations through different rolling deformation, and performs quartz tube packaging and vacuumizing on a sample subjected to rolling deformation and fills inert gas for protection; then large equiaxed grains with different orientations are obtained through high-temperature heat treatment (lower phase transition point of metal material), EBSD and different direction sampling modes. The method can also be used for researching the influence of different temperature treatments on the growth of the crystal grains.
The features of the invention are as follows:
1. rolling deformation is carried out by a rolling mill at different rolling speeds and pressing amounts, so that equiaxed grains with different orientations can be obtained;
2. the optimized high-temperature-resistant quartz tube is vacuumized and filled with argon, so that the oxidation of a metal material during high-temperature heat treatment can be prevented, a protection effect is achieved, and the low oxygen pressure is favorable for grain growth;
3. the higher the phase change point of the selected metal material is, the larger the equiaxial crystal grain obtained finally is, and the equiaxial crystal of millimeter level can be obtained at most;
4. in combination with the orientation determined by the EBSD technology, the sample is cut in different directions by a wire cutting machine, so that large equiaxial grains with different orientations, such as {10-10} and {0001} oriented grains, can be obtained;
5. based on the method of the invention, the influence of different temperature treatments on the growth of crystal grains can be obtained. The related technical principle is as follows:
the Zhi Jian principle is as follows:
during the formation of the polycrystalline body, due to the influence of various conditions such as external force, heat, electricity, magnetism and the like, or the influence of different processing techniques after the polycrystalline body is formed, crystal grains in the polycrystalline body are arranged along certain directions, and a more or less statistically uneven distribution, namely aggregation and arrangement in certain directions are presented, so that the phenomenon that the orientation probability is increased in the directions is presented, and the phenomenon is called preferred orientation. This texture structure and regular aggregate arrangement is similar to the structure and texture of natural fibers or fabrics and is therefore referred to as texture.
The phase change principle is as follows:
the so-called phase transition is the process by which a substance changes from one phase to another. The physical and chemical properties of the substance system are completely the same, and the homogeneous part with a distinct interface with other parts is called a phase. Corresponding to the three states of solid, liquid and gas, the substance includes solid phase, liquid phase and gas phase. For solids, the physical properties of different lattice structures are different and belong to different phases, so that the same solid can have a plurality of different phases. The mutual transformation between different phases is called "phase change" or "change of state". For example, the alpha and beta phases are the predominant 2 phases in titanium, zirconium, hafnium alloys.
Drawings
In order to more clearly illustrate the technical solution of the present invention, the drawings that are required to be used in the present application will be briefly described below.
FIG. 1 is a schematic diagram of a process for preparing large equiaxed crystals.
FIG. 2 is a crystal grain orientation diagram of pure hafnium after rolling.
FIG. 3 is a phase diagram of pure hafnium after heat treatment.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
Example 1
Hafnium has a very low thermal neutron absorption cross section and good corrosion resistance, and is mainly used as a control material for reactors.
A method for preparing large equiaxed grains with different orientations comprises the following specific steps:
1) firstly, the pure hafnium material is rolled and deformed by a rolling mill (60% deformation, rolling speed: 80r/min, feed rate: 3 mm/period) to obtain equiaxed grains with different orientations, and the structure after rolling deformation is shown in figure 2;
2) carrying out high-temperature-resistant quartz tube packaging and vacuumizing (the vacuum degree is less than 10) on samples subjected to different rolling deformation- 3MPa), then filling high-purity argon for protection;
3) carrying out high-temperature treatment on the packaged sample in a high-temperature heat treatment furnace, wherein the heat treatment temperature is 1500 ℃, the heat treatment time is 3 hours, and the sample is cooled to room temperature along with the furnace;
4) the sample was taken out, the metallographic phase was observed and the orientation was determined by the EBSD technique, and the sample was cut in different directions by a wire cutting machine, finally obtaining large equiaxed grains of millimeter level with different orientations (shown in fig. 3).
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A method for preparing large equiaxed grains with different orientations is characterized by comprising the following specific steps:
1) firstly, rolling and deforming the metal material by a rolling mill, and leading the metal material to form different structures through different rolling speeds and pressing quantities so as to obtain equiaxed grains with different orientations;
2) packaging the samples subjected to different rolling deformation by using a quartz tube, vacuumizing the quartz tube, and then filling inert gas for protection;
3) carrying out high-temperature treatment on the packaged sample in a high-temperature heat treatment furnace, wherein the heat treatment temperature is lower than T(α→β)-10 ℃ of which T(α→β)The phase transition temperature of the metal material is set, the heat treatment time is more than or equal to 1 hour, and the metal material is cooled to room temperature along with the furnace;
4) and taking out the sample, observing the metallographic phase, determining the orientation by an EBSD technology, and cutting the sample in different directions by a wire cutting machine to obtain large equiaxial grains with different orientations.
2. A method of producing large equiaxed grains of different orientations as claimed in claim 1, wherein: the large equiaxed grains have a size of 500 microns or greater.
3. A method of producing large equiaxed grains of different orientations as claimed in claim 1, wherein: in the step 1), the metal material is a metal material with a phase transition temperature of more than 1000 ℃.
4. A method of producing large equiaxed grains of different orientations according to claim 1 or 3, wherein: in the step 1), the metal material is pure hafnium.
5. A method of producing large equiaxed grains of different orientations as claimed in claim 1, wherein: in the step 1), the rolling speed is 50-100r/min, and the feeding speed is 1-5 mm/period.
6. A method of producing large equiaxed grains of different orientations as claimed in claim 1, wherein: in step 2), the quartz tube is vacuumized to ensure that the vacuum degree is less than 10-3Mpa and the inert gas is argon.
7. A method of producing large equiaxed grains of different orientations as claimed in claim 1, wherein: in the step 3), the heat treatment time is not less than 3 hours.
8. Use of the method of claim 1 to study the effect of different temperature treatments on grain growth.
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Citations (5)
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|---|---|---|---|---|
| JPH0565562A (en) * | 1991-09-10 | 1993-03-19 | Honda Motor Co Ltd | Production of structural member made of high strength tial intermetallic compound |
| JP2015071823A (en) * | 2013-09-04 | 2015-04-16 | 株式会社神戸製鋼所 | Aluminum alloy sheet |
| CN109468492A (en) * | 2019-01-17 | 2019-03-15 | 燕山大学 | A kind of titanium alloy plate and its processing technology of high impact toughness |
| CN110607470A (en) * | 2019-10-11 | 2019-12-24 | 中国科学院金属研究所 | Oxidation-resistant nickel-based alloy |
| CN111218632A (en) * | 2020-01-13 | 2020-06-02 | 中国科学院金属研究所 | Preparation method of zirconium and zirconium alloy coarse crystals |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0565562A (en) * | 1991-09-10 | 1993-03-19 | Honda Motor Co Ltd | Production of structural member made of high strength tial intermetallic compound |
| JP2015071823A (en) * | 2013-09-04 | 2015-04-16 | 株式会社神戸製鋼所 | Aluminum alloy sheet |
| CN109468492A (en) * | 2019-01-17 | 2019-03-15 | 燕山大学 | A kind of titanium alloy plate and its processing technology of high impact toughness |
| CN110607470A (en) * | 2019-10-11 | 2019-12-24 | 中国科学院金属研究所 | Oxidation-resistant nickel-based alloy |
| CN111218632A (en) * | 2020-01-13 | 2020-06-02 | 中国科学院金属研究所 | Preparation method of zirconium and zirconium alloy coarse crystals |
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| Title |
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| CHENGZE LIU: ""Texture and yielding anisotropy of Zircaloy-4 alloy cladding tube produced by cold Pilger rolling and annealing"", 《MATERIALS SCIENCE&ENGINEERING A》 * |
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