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Tungsten

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Microstructure evolutions of the W–TiC composite conducted by dual-effects from thermal shock and He-ion irradiation

  • Yu-Fen Zhou
  • Xiao-Yue Tan
  • Lai-Ma LuoEmail author
  • Yue Xu
  • Xiang Zan
  • Qiu Xu
  • Kazutoshi Tokunaga
  • Xiao-Yong Zhu
  • Yu-Cheng WuEmail author
Original Paper
  • 34 Downloads

Abstract

Considering that tungsten (W) materials served as the plasma-facing material in the fusion reactor would be exposed to edge-localized modes (ELMs)-like thermal shock loading accompanied with He-ion irradiation, the W–TiC composite produced with a wet-chemical method was conducted by the dual effects from the laser beam thermal shock first and He-ion irradiation later in this work. The microstructure changes of the W–TiC composite before and after two tests were characterized by scanning electron microscopy or transmission electron microscopy. After the laser beam thermal shock test, there was an obvious interface on the exposed surface of the W–TiC composite. Several main cracks and melting areas could be found nearby the interface and center, respectively. Furthermore, a mixture of tungsten oxide and TiC was easy to aggregate and form into circle areas surrounding the melting area. The thermal shock tested that W–TiC composite was then subjected to the He-ion irradiation. The typical features of fuzz structures could be detected on the surface of the W–TiC composite apart from the center of the melting area. Notably, several nano-sized He bubbles deeply distributed at grain boundaries in the melting area, owing to the grain boundary functioning as the free path for He diffusion.

Keywords

Plasma-facing materials Wet-chemical method W–TiC composite Thermal shock He-ion irradiation 

1 Introduction

Tungsten (W) is considered as one of the most promising candidates for plasma-facing materials (PFMs) because of its several decisive advantages of high thermal conductivity, high melting point, low tritium retention, and low coefficient of thermal expansion [1, 2, 3, 4]. However, there exist severe disadvantages of recrystallization embrittlement, irradiation embrittlement, and high ductile–brittle transition temperature (DBTT) for W severed as PFMs [5, 6, 7]. Currently, many researchers consider that the addition of the second phase such as TiC [8], ZrC [9], Y2O3 [10], and La2O3 [11] could be an efficient way to improve the brittle behavior of W. The TiC with a high melting point and low thermal expansion coefficient could be used to improve the toughness of W and reduce the DBTT.

When the plasma operates normally, PFMs are subjected to the steady-state heat load, which can reach up to 20 MW m−2 (~ 10 s). However, PFMs are still subjected to the high-energy transient heat load because of the instability of plasma, such as vertical displacement events (VDEs, ~ 60 MJ m−2, ~ 300 ms) and edge-localized modes (ELMs, ~ 1 MJ m−2, < 0.5 ms) [12, 13]. Such a high-energy density can lead to recrystallization (for deformed W materials), surface melting, ablation, cracking, and other serious irreversible damages for PFMs [14], resulting in reducing its basic physical properties and shortening its service life [15, 16]. The particle irradiation from the plasma also causes some damages for PFMs. For example, He-ion irradiation can induce some surface damages in W materials, such as helium bubbles, filaments, and fuzz structures [17, 18].

W materials served as PFMs would be subjected to the dual actions from the transient thermal loading and He-ion radiation simultaneously. Actually, it is hard to find a facility that could conduct these two tests at the same time. Sinclair et al. [19] conducted the He-ion irradiation first and thermal shock test later on pure W to study the surface structure changes during the process of these two tests, and found that the fuzz density on the damaged surface decreased gradually and disappeared finally with the increasing energy density of thermal shock. In addition, melting and cracking could also be detected. In this work, we tried to figure out the surface change behaviors of the produced W–TiC composite exposed to the thermal shock first and then conducted by He-ion irradiation. The laser beam thermal shock test was designed to simulate the ELMs-like transient thermal shock loading. The He-ion irradiation experiment was to simulate the behavior of He ion on W materials during plasma operation. To further study the changes of microstructures of the irradiated W–TiC composite, the composite was cut by a focused ion beam (FIB).

2 Experimental

The W–TiC composite powder was prepared by a wet-chemical method [20]. An appropriate amount of ammonium paratungstate ([NH4]10H2W12O42·xH2O) was dissolved into deionized water, and nano-sized TiC particles were added into the solution. Then, oxalic acid (C2H2O4·2H2O) severed as a precipitator was dissolved into the mixture solution. Heating up to 165 °C, the W–TiC precursor could be obtained by continuously stirring and evaporating the mixture solution until water was completely evaporated. The precursor was ground and then heated in a tubular furnace in a hydrogen atmosphere to obtain the W–TiC composite powder. The heating temperature was raised to 200, 500 and 800 °C at a heating rate of 5 °C min−1 and dwelled for 30, 60, and 60 min, respectively. Finally, the W–TiC composite bulk with a relative density of 18.71 g cm−3 was consolidated by the spark plasma sintering technique. The shape of the W–TiC bulk was a disk with the diameter of 20 mm and the thickness of 2 mm.

The specimen for the thermal shock test or He-ion irradiation with the dimensions of 10 mm × 10 mm × 1 mm was cut by wire cutting from the W–TiC bulk. The test surface was a square surface of 10 mm × 10 mm, which was polished to a mirror-quality surface before tests. In Fig. 1, TiC particles with a size of ~ 3 µm are distributed not only at the grain boundary, but also in the W matrix with an average grain size of ~ 15 µm. The ELMs-like transient thermal shock was simulated by a pulsed laser beam in an LSW-1000 laser beam-welding instrument. The energy density, current, and pulsewidth of the laser were 12.7 MW m−2, 60 A, and 1 ms, respectively. Based on the subsequent analysis of the specimen surface after thermal shock, the energy density had a gradient distribution from the center to the edge of the impact area, and the central area was subjected to the highest energy compared to the other areas. Notably, although the thermal shock test was conducted in an argon protection atmosphere, there still existed oxidation during the thermal shock process according to the subsequent analysis. After the thermal shock test, the W–TiC specimen was exposed to He-ion irradiation. The He-ion irradiation experiment was carried out by a large-power-induced-coupled plasma irradiation system. The incident energy of He ion was 80 eV, the He-ion flux was 1.5 × 1022 He+ m−2 s−1, and the total dose was 9.9 × 1024 He+ m−2. The surface temperature of the irradiated W–TiC specimen was measured from 1230 to 1280 °C using an infrared STL-150B pyrometer.
Fig. 1

Surface morphology of the W–TiC composite

The surface morphologies or the phase structures of the W–TiC specimens before and after the thermal shock test or He-ion irradiation were characterized by field-emission scanning electron microscope (FESEM, SU8020, Japan) and X-ray diffraction (XRD, D/MAX2500 V, Japan). To find out the influences during the thermal shock test or He-ion irradiation, the FESEM equipped with energy-dispersive X-ray spectrometry (EDS) was applied to confirm the composition changes of the W–TiC composite. To further investigate the microstructure changes of the W–TiC composite, the specimen was cut from the center of the melting area using the FIB (FEI Helios NanoLab 650 DualBeamTM field-emission electron microscope) technique, and the specimen was analyzed by transmission electron microscope (TEM, JEM-2100F, Japan) in detail.

3 Results and discussion

3.1 ELMs-like laser beam thermal shock test

Figure 2a shows the surface morphology of the W–TiC specimen after one single-pulse laser beam thermal shock. On the exposed surface of the specimen, a distinctly circular white interface with a diameter of ~ 425 μm can be found, which may be due to the contrast of light and shade under the FESEM detection condition. At the center of the circular region, a molten-state surface can be detected, which is named the melting area. Several small cracks are distributed in the circular white region, as marked by the arrows in Fig. 2a. There are two reasons that could result in the formation of the cracks. First, the formation of the melting area could be owing to the local overheating during the thermal shock test, which means that there would exist a temperature gradient between the melting area and un-melting area. Second, the laser beam thermal shock test includes beam-on and beam-off stages. During this period, a large temperature gradient would be generated on the surface of the composite, inducing that the thermal stress (tensile stress) worked on the surface of the specimen and resulted in the formation of cracks [21].
Fig. 2

a Surface morphology of the W–TiC composite after thermal shock; b, c magnified images of the selected areas in a; d surface morphology of the W–TiC composite; e, f EDS spectrums of the selected regions in c

To study the detailed information of the W–TiC composite after the thermal shock test, the magnified images of selected areas were performed and are shown in Fig. 2b, c. From Fig. 2b, a nearly circular grey block with a diameter of 25 μm is located at the center of the melting area, and according to the EDS mapping, as shown in the insert of Fig. 2b, the grey block is composed of W and O elements. The presence of O would be ascribed to the oxidation during the thermal shock test. The melting point of formed tungsten oxides is lower than that of W, indicating that the molten state is more likely to occur. Notably, the width of cracks becomes more and more narrow from the outside to inside, as shown in Fig. 2c, indicating that the cracks are originated from the outside of the melting area. This means that the formation of cracks is due to the induced tensile stress during the beam-off stage. In general, the addition of the TiC particles acted as the strengthening phase to strengthen grain boundaries, thereby hindering the formation and propagation of cracks [22]. From Fig. 2c, the paths of crack are deflected at the location of the TiC particle, which would be an effective way to release the induced thermal stress. In addition, some grey or dark areas can be found on the surface of the W–TiC specimen after the thermal shock test, as shown in Fig. 2c. Based on EDS spectra of selected areas, which composed of W and O, or W, Ti, and O, indicating that these areas may exist tungsten oxide or a mixture of tungsten oxide and TiC. Notably, the grey or dark areas are presented with a dotted distribution, which might be resulted by the jet stream of argon sputtering in the local melting area.

3.2 He-ion irradiation

After the laser thermal shock test, the specimen was exposed to He-ion irradiation. The same region in Fig. 2a after He-ion irradiation is shown in Fig. 3a. There are no obvious damage characteristics and can be detected in the region under current conditions. To investigate the microstructure changes of the specimen during He-ion irradiation, the magnified SEM images are performed on the interested area in Fig. 3a, and the corresponding results are shown in Fig. 3b–d. Figure 3b shows the same region with Fig. 2b, which is found that the grey block shows obviously different morphology changes compared to other areas in Fig. 3c, d. Compared to Fig. 2b, the surface of the grey block in Fig. 3b becomes merely rougher, which might be related to the formation of tungsten oxides (the insert mapping in Fig. 2b). Notably, apart from the grey block in Fig. 3b, the nano-sized fuzz structures can be detected. The region in Fig. 3c is the same as that in Fig. 2c, where the typical fuzz structures are uniformly distributed on the surface of the W–TiC composite. In Fig. 2c, there exists some O-contained grey or dark areas; however, the surface morphologies of these areas have no obvious differences after He-ion irradiation. Owing to a small amount of formed oxides being sputtered out during He-ion irradiation, the composition of the irradiated region would be the “pure” W–TiC composite, producing the same irradiation damage behavior. Figure 3d shows the surface morphology of a region after He-ion irradiation, where is far from the region of the thermal shock test. Compared with Fig. 2d, some pits could be detected at the position of the TiC particles in Fig. 3d, because TiC particles composed of low Z elements of Ti and C possess a low sputtering resistance and are easy to be sputtered out during He-ion irradiation. The formation of fuzz is related to the formation and growth of He bubbles [23, 24, 25, 26]. During He-ion irradiation, He ions act on the surface of the W–TiC composite and form interstitial He atoms. At a high temperature, these He atoms are gathered by the diffusion and formation of the He clusters or He bubbles. With continuous He-ion irradiation, the fuzz structure is formed by the formation, growth, and burst of He bubbles. Compared with commercial W, the surface of the W–TiC composite exhibits different damage behaviors after He-ion irradiation. Liu et al. [27] found that the dense nano-fuzz was formed uniformly on the surface of W at the He-ion energy of > 70 eV or He-ion fluxes of > 1.3 × 1022 He+ m−2 s−1. Al-Ajlony et al. [28] found that the dense and tangled fuzz structure was formed on the surface of W with a high He-ion fluence of 9.2 × 1024 He+ m−2. For the He-ion irradiation of W–TiC in this work, the obviously different damage behaviors are that the fuzz structure with a lower concentration distributes unevenly on the surface and some of the pits are left by sputtered TiC particles.
Fig. 3

a Surface morphology of the irradiated W–TiC composite after thermal shock; b, c magnified images of the selected areas after irradiation in a; d surface morphology of the W–TiC composite after irradiation

In Fig. 3b, the surface morphology of the grey block after He-ion irradiation has an absolutely compared with other regions. To figure out the microstructure changes of the He-ion irradiated grey block, the cross section was cut by FIB for SEM and TEM characterizations. As shown in Fig. 4a, a micro-crack is located at the cross section of the grey block. Figure 4b, c shows FIB–TEM images of the grey block. From Fig. 4b, some nano-sized greyish dots (He bubbles) marked with white arrows can be detected and are distributed in the W matrix. To clearly confirm the details of these nano-sized greyish dots, a high-magnified image selected from the rectangle area in Fig. 4b was performed. In Fig. 4c, two sizes of greyish dots can be found. One is the nano-sized (below 20 nm) greyish dots with spherical structures which are He bubbles, and the other greyish dots with irregularly shape marked with white arrows are doped TiC particles. From Fig. 4b, the depth of the He-bubbles location can reach up to ~ 4 μm. Below the top-surface of ~ 2 μm, the nano-sized He bubbles distribute mainly in the W matrix (Fig. 4b), and the deeper distributed He bubbles are more likely to aggregate at grain boundary (Fig. 4c). The previous study [29] showed that the grain boundary could act as the path for He diffusion, explaining that why He bubbles would like to aggregate at grain boundary for the case of deep diffusion.
Fig. 4

a FIB-cutting diagram in the grey bulk area; b, c TEM images of the FIB-cutting specimen

4 Conclusion

In this work, the W–TiC composite was prepared with the wet-chemical method, and the microstructure changes of the W–TiC composite conducted by the laser beam thermal shock first and He-ion irradiation later were studied. After the laser beam thermal shock, a significant circular interface appeared on the surface of the composite. A melting area was detected in the center of the circular interface. Cracks were detected nearby the interface, which was owing to the thermal stress generated during the beam-off stage of the thermal shock test. In addition, a mixture of tungsten oxide and TiC was aggregated around the melting area, which might be related to gas sputtering. After He-ion irradiation, the fuzz structure was formed on the surface of the composite, except for the center of the melting area. Due to the grain boundary which might act as the diffusion path for He ions, He bubbles were more likely to aggregate at the deeper grain boundary rather than on the surface of the center of the melting area. This would be the reason why the fuzz structure was not formed on the surface of the center of the melting area.

Notes

Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (Grant No. 51574101), the Fundamental Research Funds for the Central Universities (Grant Nos. PA2018GDQT0010, PA2019GDZC0096, JZ2019HGTA0040), the Foundation of Laboratory of Nonferrous Metal Material and Processing Engineering of Anhui Province (15CZS08031), the Natural Science Foundation of Anhui Province (Grant Nos. 201904b11020034, 1908085ME115), the Foundation of Laboratory of Nonferrous Metal Material and Processing Engineering of Anhui Province, the Open Foundation of Key Laboratory of Advanced Functional Materials, Devices of Anhui Province and Double First Class enhancing independent innovation and social service capabilities of Hefei University of Technology (Grant No. 45000-411104/011).

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Copyright information

© The Nonferrous Metals Society of China 2019

Authors and Affiliations

  • Yu-Fen Zhou
    • 1
  • Xiao-Yue Tan
    • 1
  • Lai-Ma Luo
    • 1
    • 2
    Email author
  • Yue Xu
    • 1
    • 2
  • Xiang Zan
    • 1
    • 2
  • Qiu Xu
    • 3
  • Kazutoshi Tokunaga
    • 4
  • Xiao-Yong Zhu
    • 1
    • 2
  • Yu-Cheng Wu
    • 1
    • 2
    • 5
    Email author
  1. 1.School of Materials Science and EngineeringHefei University of TechnologyHefeiChina
  2. 2.Laboratory of Nonferrous Metal Material and Processing Engineering of Anhui ProvinceHefeiChina
  3. 3.Institute for Integrated Radiation and Nuclear ScienceKyoto UniversityKyotoJapan
  4. 4.Research Institute for Applied MechanicsKyushu UniversityKasugaJapan
  5. 5.National-Local Joint Engineering Research Centre of Nonferrous Metals and Processing TechnologyHefeiChina

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