KR20160126702A - High strength tungsten alloy with low activation and manufacturing method for the same - Google Patents
High strength tungsten alloy with low activation and manufacturing method for the same Download PDFInfo
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Abstract
Description
The present invention relates to a tungsten alloy, and more particularly, to a high strength, low-activation tungsten alloy suitable for a diverter of a fusion device under development as a next generation energy source.
When the fusion device is driven, plasma particles collide with the primary inner wall by nuclear fusion to generate impurities due to spatter phenomena, and such impurities deteriorate the plasma purity which reduces the energy efficiency. In this fusion reaction, the divertor removes impurities in the core to minimize the contamination of the plasma, and it is possible to remove the plasma from the high temperature of the plasma, As a main device for protecting, a magnetic force line connecting with an outer circumference is set around a plasma to leak leaked plasma ions or electron impurity ions to the outside and to be led away from the plasma.
Due to this importance, many researches on high performance plasma counterparts have been carried out at home and abroad. In order for PFC to function properly in the operating conditions of extreme environments that are subject to high heat load from plasma and high-speed neutron irradiation, it is necessary to select suitable facing materials considering the interaction of plasma and wall surface, design with structural safety, It is essential to study the bonding method of facing material and structural material for removal.
Materials that have been studied as facing materials include beryllium (Be), carbon fiber composite material (CFC), and tungsten (W), which are used by bonding them with copper alloy (CuCrZr) or graphite or stainless steel.
Among these, beryllium and CFC have advantages of high melting temperature and durability against thermal shock, but they are disadvantageous because of high efficiency of tritium trapping, which is disadvantageous for long operation and high rate of erosion due to plasma. Pure tungsten, on the other hand, has the advantages of high melting temperature, low plasma erosion rate and low tritium impregnation effect, but with a small amount of erosion, the plasma stability is lowered and the ductile-plastic transition temperature is too high.
In the International Thermal Fusion Experiments (ITER), while the divertor facing material was provisionally determined to be pure tungsten, most of the material-related research is devoted to studying the method of bonding non-alloyed tungsten to various rear structural materials. It is necessary to develop a new alloy material to improve the characteristics of the tungsten facing material.
It is an object of the present invention to provide a high-strength and low-activation tungsten alloy having improved physical properties suitable for application to a divertor which is a plasma counterpart component.
In order to achieve the above object, the tungsten alloy of the present invention alloys at least one element selected from Ti, V, Cr, Mn, Fe, Y, Zr and Ta, which is a transition metal having low radiative properties, with tungsten, It is composed of more than 5% in order to induce changes in physical properties. It controls the kind and amount of alloying elements so that tungsten and solid solution can be formed, so that the entropy control of the alloying system enables high entropy entropy alloy, which is characterized in that at least 10 at% or more of tungsten is included to reflect the properties of the parent tungsten element in the solid solution even in the cocktail effect. Generally, when a solid solution is formed, alloying elements are randomly and randomly included in the crystal structure of a pure element, so that even when a small amount is added, the characteristics of the parent element are reflected. In the case of the tungsten-based solid solution alloy of the present invention, the additive elements are randomly arranged in the body-centered cubic structure of tungsten, and when the solid solution base is maintained, the characteristics of the parent tungsten alloy are reflected in the base.
The tungsten alloy of the present invention may contain at least two elements selected from the group consisting of low radiative transition elements Ti, V, Cr, Mn, Fe, Y, Zr and Ta, Tungsten and a medium entropy state including 5 to 35 at%, respectively. In this case, tungsten and two elements of Ta and V which form a tran- sitive solid solution in the entire composition range are included It is preferable to include three elements of Ta, V, and Ti.
In order to control entropy by the number of elements to be added, the tungsten alloy of the present invention is characterized in that at least 4 elements selected from low radiative transition elements Ti, V, Cr, Mn, Fe, Y, Zr, To 35 at%. In this case, tungsten and four elements of Ti, V, Cr and Ta, which form a tangible solid solution in the entire composition range, are included. .
Another method of manufacturing a solid entente base alloy having a high entropy state is to control entropy by controlling the amount of additive elements. In the alloying system of the present invention, all constituent elements are equiatomic in an allowable error range of 10 at% ).
Further, the two-component system is mixed so that the atomic fraction of A: B is 50 ± 10: 50 ± 10, and the three-component system is such that the atomic fraction of A: B: C is 33.3 ± 10: 33.3 ± 10: 33.3 ± 10 And the four component system is mixed so that the atomic fraction of A: B: C: D is 25 ± 10: 25 ± 10: 25 ± 10: 25 ± 10, The constituent entropy of each constituent alloy is maximized and the stability of the solid solution formed is improved. Similarly, when the atomic fraction of A: B: C: D: E is 20 ± 10: 20 ± 10: 20 ± 10: 20 ± 10: 20 ± 10, the entropy becomes maximum, However, it is preferable that at least 10 at% or more of tungsten is contained in order to reflect the characteristics of tungsten parent element even in the cocktail effect.
As described above, the tungsten alloy of the present invention contains only low-radiative transition elements and controls the number and amount of alloy constituent elements to control the entropy state of the alloy, thereby causing a large lattice distortion, And it is suitable as a high temperature material by suppressing the change of material properties due to formation of precipitation at high temperature by the increase of strength due to strengthening of employment and sluggish diffusion at a high temperature. In addition, in the case of the high entropy solid solution alloy, the chemical properties such as corrosion and erosion as well as physical properties such as hardness and fracture toughness are improved by the cocktail effect existing with the characteristics of the multi-component constituent elements.
In addition, by manufacturing an alloy of a solid solution state in which the formation of the second precipitate phase is controlled, it is possible to maintain the high melting point characteristic of pure tungsten by preventing the abrupt melting point problem due to formation of the invariant reaction while lowering the DBTT by the solid solution There is an effect. These tungsten alloys contain low-radiative transition elements to control the activation and realize high strength, making them suitable as a material for diverters in nuclear fusion, which is under development as one of the next generation energy sources.
The method for producing the tungsten alloy of the present invention can be applied to an arc melting method in which a raw material is alloyed by plasma arc melting and then cooled. The arc melting method is easy to form a homogeneous solid solution and can minimize the impurity elements such as oxides and pores compared with the sintering process and has a relatively low ductility-plasticity transition temperature (DBTT) as compared with the sintering process And the rupture time is increased.
In addition to the conventional casting method capable of dissolving the raw material metal, the raw material can be manufactured by powder and sintered at a high temperature and a high pressure using Spark Plasma Sintering or Hot Isostatic Pressing , And in the case of the sintering method, microstructure control and parts having a desired shape can be easily manufactured.
A diverter for a fusion device according to another embodiment of the present invention is characterized in that the above-mentioned tungsten alloy of the present invention is provided in the plasma opposing portion.
By providing the tungsten alloy of the present invention in the plasma confronting portion, the service life is increased compared with the case where pure tungsten is used in the past.
The present invention constituted as described above is suitable as a divertor material by controlling spin activation by containing only a low activation element and exhibiting a high strength property due to strengthening of solid solution by lattice strain while maintaining a solid solution.
In addition, the tungsten alloy of the present invention can suppress the abrupt melting point problem due to the formation of the invariant reaction while lowering the DBTT by the solid solution by manufacturing an alloy of the solid solution state in which the formation of the second precipitate phase is controlled, The high-melting-point characteristic of the high-melting-point metal can be maintained.
Further, the tungsten alloy whose entropy is controlled by the medium to high entropy alloy has a high lattice strain, slow diffusion rate, suppresses the brittle fracture of the material due to the formation of precipitation phase such as an intermetallic compound at high temperature, and exhibits improved high temperature stability The provision of the tungsten alloy having improved physical properties such as hardness and fracture toughness by the cocktail effect of the component constituent element can significantly increase the lifetime of the divertor for the fusion device.
Fig. 1 is a graph showing the relationship between (a) an element group in which the addition amount is limited in ppm units, (b) an element group which can be included according to the alloy design, and (c) The results are classified into three major categories.
FIG. 2 is a schematic diagram showing a change in solubility according to an additive element, showing a binary state diagram of tungsten and transition elements in the periodic table.
Fig. 3 shows the results of XRD analysis of the alloys of the comparative examples and the examples of the present invention.
Figure 4 shows the FWHM value for the main peak in Figure 3.
FIG. 5 shows the XRD analysis results of the alloys of Comparative Examples and Examples in a high entropy state.
6 is a result of EBSD analysis of a microstructure and an intermediate entropy solid solution four-component alloy obtained by observing the W-Ta-V, W-Ta-V-Ti and W-Ta-V-Ti-Cr alloys of the present invention with an optical microscope .
7 shows the hardness measurement results of the alloys of the comparative examples and the inventive alloys of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Referring to the accompanying drawings, embodiments of the present invention will be described in detail.
One of the most important alloying design points for the development of the high-strength, low-activation tungsten alloy according to the present invention is to constitute an alloy with elements exhibiting low activation properties, (a) an element group in which the addition amount is limited in ppm, (b) an element group which can be included in accordance with the alloy design, and (c) an element group in which the addition amount is not limited. In the present invention, for the development of low-radioactive alloys, the group of elements limited in the amount added in ppm was excluded from the alloy design.
In addition, as shown in FIG. 2, the employment of the tungsten alloy and the additive element is investigated to enhance the hardness by solid solution strengthening. The low radiative transition elements Ti, V, Cr , Mn, Fe, Y, Zr, and Ta in an amount of 5% or more. The present invention comprises 5% or more of additive elements so as to induce changes in physical properties through alloying of dissimilar elements. By controlling the kind and amount of alloying elements, entropy control of the alloying system enables low entropy solid solution to high entropy solid solution . These tungsten alloys are suitable for divertor materials because they contain only low-radiative transition elements capable of controlling activation, while maintaining a solid solution state in which the second precipitation phase is controlled and exhibit high strength through solid solution strengthening.
Table 1 shows pure tungsten and high entropy alloys (comparative examples) and representative compositions (examples) of the present invention in order to confirm the characteristics of the high strength and low activation tungsten alloy of the present invention.
As the alloy manufacturing method, an arc melting method was applied, and alloy materials were melted at a high temperature through an arc plasma and cooled to prepare an alloy. The reason for applying the arc melting method in this embodiment and the comparative example is that it is easy to form a bulk solid homogeneous solid solution and impurity elements such as oxides and pores can be minimized as compared with the sintering process. In addition, the arc melting method has the advantage of increasing the rupture time because it can maintain relatively low ductility-plasticity transition temperature (DBTT) as compared with the sintering process for the same composition. However, the method of producing the alloy of the present invention is not limited to the arc melting method, and it is also possible to use a spark plasma sintering or hot It can be manufactured by sintering at a high temperature / high pressure using Hot Isostatic Pressing, and in the case of sintering method, microstructure control and parts having a desired shape can be easily manufactured.
The present invention relates to a tungsten-based alloy, which is alloyed according to characteristics required for diverters to have high strength and low radiative properties. Particularly, Ta, V, Ti, and Cr selected as the alloying elements of the examples are elements having tungsten and a tungsten solid solution region having low radiative characteristics, and are transition metals that are easy to form a solid solution upon alloying by arc melting. In the case of constituting the solid solution alloy of the present invention, the DBTT which makes it easy to secure the material reliability even in a sudden temperature change is reduced, the abrupt melting point problem due to the invariant reaction formation is prevented, and the high melting point characteristic of tungsten can be maintained There are advantages.
FIG. 3 shows the results of XRD analysis of the alloys of the comparative examples and the inventive examples, and FIG. 4 shows FWHM values with respect to the main peaks as a result of X-ray diffraction analysis in FIG.
As shown in the figure, when the alloying element of the present invention is added to pure tungsten, it is confirmed that even if the number of added elements is increased, solid solution having the body center cubic (BCC) structure is maintained, and entropy in the solid solution increases high entropy state), it can be seen that the lattice distortion (lattice distortion), which can be confirmed by the full width at half maximum (FWHM), increases.
In particular, the W-20Ta-20V-20Ti-20Cr alloys showed a significant increase in lattice strain, and these results are due to the formation of high-entrophy solid solution with increasing number and amount of alloy atoms. In general, the entropy alloy is mixed in the range of 5 to 35 at% (the closer to the equiatomic amount) the more than five alloying elements, resulting in a high entropy of mixing, Forming a solid solution rather than forming an intermetallic compound to be precipitated. In addition, solid enthalpy was formed in W-20Ta-20V alloy and W-20Ta-20V-20Ti alloy with medium entropy without intermetallic compound formation.
FIG. 5 shows the XRD analysis results of the alloys of Comparative Examples and Examples in a high entropy state. (a) shows the results for the W-20Ta-20V-20Ti-20Cr alloy according to the present invention, and (b) shows the results for the comparative example Zr-20Nb-20V-20Ti-20Cr alloy. The solid solution having the BCC structure was formed in the case of the present invention (a), whereas the Laves phase causing brittle fracture together with the BCC phase was simultaneously precipitated in the case of the comparative example (b). These results show that, even when five or more alloying elements are mixed in the range of 5 to 35 at% (as the amount closer to the same atomic fraction is increased), inducing high entropy does not necessarily form the solid solution base microstructure as in the present invention And in the case of a multi-component system, it is confirmed that such a solid solution base region is formed only within a specific composition range.
FIG. 6 is a graph showing the results of observation of alloys (W-Ta-V, W-Ta-V-Ti and W-Ta-V-Ti-Cr alloys) in the intermediate entropy to the high entropy state of the tungsten- EBSD analysis of one microstructure and four-component alloys. As can be seen from the figure, it can be seen that the microstructure of the dendritic structure is shown without precipitation of the second phase in all the compositions of the present invention. In addition, it can be confirmed from the results of the EBSD analysis of the intermediate entropy solid solution by the four-component system of the present invention that the growth of the dendritic phase is a result of growth in various orientations through the generation of polyphase nuclei in the crystal grains.
7 shows the hardness measurement results of the alloys of the comparative example and the example.
The hardness measurement results of FIG. 7 are shown in the following Table 2.
As shown in FIG. 7 and Table 2, although the content of tungsten having the highest hardness among the constituent alloying elements was decreased, the hardness was increased as the type of alloy element was increased. The reason for this is that as the entropy of the material increases, the compositional overcool increases and the dendritic arm spacing decreases and the solid solution alloy is formed. In particular, the W-20Ta-20V-20Ti-20Cr alloy exhibits a hardness characteristic that greatly increases the hardness up to about 600 HV due to the grain size of about 100 μm, the secondary dendritic gap of less than 10 μm, and the solid- .
The characteristics of the alloys according to the present invention in which low radiative transition elements Ti, V, Cr, Mn, Fe, Y, Zr and Ta were alloys were confirmed so as to exhibit high strength and low activation properties based on tungsten. The alloys of the present invention contain low-radioactive elements to maintain activation of tungsten and solid solution state while controlling the activation, and are therefore suitable as diverter materials because of their high strength properties due to solid solution strengthening. In addition, by producing a solid solution state in which the precipitation of the second phase is controlled, there is an effect that the high melting point characteristic of tungsten can be maintained by preventing the problem of the rapid melting point lowering due to the invariant reaction formation while lowering the DBTT by the solid solution. Particularly, the intermediate entropy alloy containing at least two selected from the low radiative transition elements Ti, V, Cr, Mn, Fe, Y, Zr and Ta and the high entropy alloy containing at least four alloys have a large lattice strain lattice distortion, a relatively slow diffusion rate, and a cocktail effect of the multicomponent constituent, thereby providing improved tungsten alloys with improved physical properties such as hardness and fracture toughness.
While the present invention has been particularly shown and described with reference to preferred embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. Those skilled in the art will understand. Therefore, the scope of protection of the present invention should be construed not only in the specific embodiments but also in the scope of claims, and all technical ideas within the scope of the same shall be construed as being included in the scope of the present invention.
Claims (7)
Wherein all constituent elements are constituted of equiatomic ratios within an allowable tolerance of 10 at% to form a solid solution base in a high entropy state.
It is manufactured by arc melting method after cooling the raw material after arc melting, or by sintering at high temperature / high pressure by spark plasma sintering (Hot Isostatic Pressing) or hot isostatic pressing after preparing raw material as powder Wherein the tungsten alloy is produced by a method comprising the steps of:
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866498A (en) * | 2018-08-10 | 2018-11-23 | 合肥工业大学 | A kind of W self-passivation alloy and preparation method thereof with long-time high temperature oxidation resistance |
| KR20200006906A (en) * | 2018-07-11 | 2020-01-21 | 엘지전자 주식회사 | Medium-entropy alloys with spinodal decomposition-induced extended solubility |
| CN111074199A (en) * | 2019-12-03 | 2020-04-28 | 太原理工大学 | Preparation method of high-entropy alloy layer on surface of tungsten alloy |
| CN111254339A (en) * | 2020-03-06 | 2020-06-09 | 中国工程物理研究院材料研究所 | Five-tungsten-series high-entropy alloy and preparation method thereof |
| CN114150206A (en) * | 2021-11-29 | 2022-03-08 | 北京航空航天大学 | Tungsten-based columnar crystal high-entropy alloy surface-to-plasma material and preparation method thereof |
| KR20220039485A (en) * | 2020-09-22 | 2022-03-29 | 서울대학교산학협력단 | Tantalum alloy with high strength and high formability and manufacturing method thereof |
| CN115896580A (en) * | 2021-09-29 | 2023-04-04 | 合肥工业大学 | High-plasticity WTaTiVC (WTaTiVC) series refractory high-entropy alloy and preparation method thereof |
| CN117947326A (en) * | 2024-02-05 | 2024-04-30 | 中南大学 | Radiation-resistant low-activation refractory W-Ta-Cr-V multi-component alloy and preparation method thereof |
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| KR20200006906A (en) * | 2018-07-11 | 2020-01-21 | 엘지전자 주식회사 | Medium-entropy alloys with spinodal decomposition-induced extended solubility |
| CN108866498A (en) * | 2018-08-10 | 2018-11-23 | 合肥工业大学 | A kind of W self-passivation alloy and preparation method thereof with long-time high temperature oxidation resistance |
| CN111074199A (en) * | 2019-12-03 | 2020-04-28 | 太原理工大学 | Preparation method of high-entropy alloy layer on surface of tungsten alloy |
| CN111074199B (en) * | 2019-12-03 | 2022-02-18 | 太原理工大学 | Preparation method of high-entropy alloy layer on surface of tungsten alloy |
| CN111254339A (en) * | 2020-03-06 | 2020-06-09 | 中国工程物理研究院材料研究所 | Five-tungsten-series high-entropy alloy and preparation method thereof |
| KR20220039485A (en) * | 2020-09-22 | 2022-03-29 | 서울대학교산학협력단 | Tantalum alloy with high strength and high formability and manufacturing method thereof |
| CN115896580A (en) * | 2021-09-29 | 2023-04-04 | 合肥工业大学 | High-plasticity WTaTiVC (WTaTiVC) series refractory high-entropy alloy and preparation method thereof |
| CN115896580B (en) * | 2021-09-29 | 2024-03-19 | 合肥工业大学 | High-plasticity WTATiVC refractory high-entropy alloy and preparation method thereof |
| CN114150206A (en) * | 2021-11-29 | 2022-03-08 | 北京航空航天大学 | Tungsten-based columnar crystal high-entropy alloy surface-to-plasma material and preparation method thereof |
| CN114150206B (en) * | 2021-11-29 | 2023-11-21 | 北京航空航天大学 | Tungsten-based columnar crystal high-entropy alloy plasma facing material and preparation method thereof |
| CN117947326A (en) * | 2024-02-05 | 2024-04-30 | 中南大学 | Radiation-resistant low-activation refractory W-Ta-Cr-V multi-component alloy and preparation method thereof |
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