Figure
1.
A schematic diagram of the composite coating fabrication process.
| Citation: |
Xinluo TIAN, Heping LI, Liyu ZHENG, Fangjian LI, Zhongyang ZHENG, Shengming YIN, Xinyun WANG, Youwei YAN. Effect of Cr2O3 nanosheet insertion on the deuterium permeation behavior of a Cr-Zr-O coating[J]. Plasma Science and Technology, 2022, 24(12): 124017. DOI: 10.1088/2058-6272/aca7ae
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In this study, a Cr2O3 nanosheet (Cr2O3 NS) inserted Cr-Zr-O coating was developed as a hydrogen isotope permeation barrier. The Cr2O3 NSs, fabricated by rapid heat treatment, were amorphous with a thickness of only several nanometers. These Cr2O3 NSs were then incorporated into a Cr-Zr-O multi-metal oxide composite coating via a dip-coating method to form a coating. The effect of the Cr2O3 NS concentration on the morphology, microstructure and deuterium permeation resistance of the coating was studied. With the addition of 1.0 g l-1 Cr2O3 NSs, compared with the Cr-Zr-O coating without NSs, the permeation reduction factor of the resultant coating was enhanced from 249 ℃ to 575 ℃ at 500 ℃. The coating, with a thickness of nearly 193 nm, achieved a comparable deuterium resistance that was above two orders of magnitude higher than the steel substrate. The results show that ceramic NSs can serve as effective fillers for enhancing the coating performance when functioning as a hydrogen isotope barrier.
In a fusion reactor like ITER, one representative feature is a high hydrogen isotope concentration in the work environment. Structural materials such as EUROFER-97, 316 L and F82H always suffer from tritium permeation. The leakage of hydrogen isotopes will lead to the loss of fuel and cause a radioactive hazard in the fusion reactor. For the practical use of fusion energy and for the safety of humankind, prevention of the leakage of hydrogen isotopes in a fusion reactor is necessary. Construction of a tritium permeation barrier (TPB) is an effective method that is used to address this issue. A ceramic coating is a type of effective TPB. Aluminum oxide (Al2O3) coatings [1–3], zirconia (ZrO2) [4–6] and erbium oxide (Er2O3) [7, 8] are all potential TPB materials. However, with the exception of tetragonal ZrO2, which has a thermal expansion coefficient of 9.0×10-6–10.0×10-6 K-1 at 400 ℃, and the closer thermal expansion coefficient of austenitic alloys (nearly 17.2×10-6–17.9×10-6 K-1 at 400 ℃ (referring to 321 steel)) [9, 10], alternative TPB materials, such as Al2O3 and Cr2O3, usually have poorer thermal expansion coefficients (8.0×10-6–8.8×10-6 K-1 and 7.0×10-6–7.3×10-6 K-1 at 400 ℃ [1–3, 11]) compared with austenitic steel substrates. Such a thermal mismatch will lead to defects and even peeling of TPBs. The introduction of components with better matching thermal expansion coefficients to eliminate the failure risk of ceramic coatings is therefore key toward fabrication of reliable hydrogen isotope barriers. The construction of a composite coating to balance hydrogen permeation resistance and adaptability with metal substrates is therefore necessary. By considering great thermal stability, chemical inertness and the greatest matching thermal expansion coefficients in ceramic materials, in this study, ZrO2, with high thermal stability chemical inertness and good matching thermal expansion coefficients with austenitic steels [12–15], is chosen as the matrix to construct composite coatings as a hydrogen isotope permeation barrier.
The sol-gel method is a practical way to fabricate ZrO2 coatings, which has low expenses and adaptability to complex components. The most important factor of this method is that it is adjustable, which means both the type of metal source and the ratio of metal ions in the sol can be adjusted. However, as the thickness of the sol-gel coating increases, defects, cracks and even holes will appear [6]. For applications such as TPB, defects in the coating will deteriorate its performance substantially. The introduction of a nanofiller is a common method that is used to improve the coating performance. However, for the ultra-thin sol-gel coating (commonly less than 200 nm), a typical nanofiller with a diameter of dozens or hundreds of nanometers will affect the coating integrity and is detrimental to its performance, as it will impale the thin sol-gel layer and influence the construction of the coating. The use of two-dimensional (2D) nanomaterials as a new kind of filler is a promising strategy to address the above issues and enhance the coating properties.
A nanosheet (NS) is a type of 2D nanomaterial with a large specific surface area and several nanometer thickness. When it is inserted into the coating as a nanofiller, a large number of heterogeneous interfaces will be generated inside the coating correspondingly. As reported in the literature, the introduction of more heterogeneous interfaces can extend the pathway for hydrogen isotopes to permeate through the coating [16]. Besides increasing the hydrogen permeation resistance, NSs can be arranged in an orderly manner in the coating because of the surface tension, which is rooted in its large specific surface area [15]. The orderly arrangement of NSs will apply regular layer-by-layer construction, which can guarantee the integrity of the coating and reduce pores and cracks.
Chromium oxide (Cr2O3), which has adequate corrosion protection, high hardness, a low friction coefficient and good wear resistance, is usually used as a corrosion resistance coating and in other application fields [17, 18]. In our previous work, we found that Cr2O3 also exhibited attractive hydrogen isotope permeation reduction properties [19–21].
In this study, we further prepared Cr2O3 NSs via a rapid heat treatment method. To improve the compatibility between the NSs and the coating, a Cr-Zr-O hybrid sol was modulated as the precursor for the coating matrix. The dip-coating method was used to obtain a Cr-Zr-O composite coating with Cr2O3 NS inserted. Both the morphology and microstructure of the composite coating were characterized. The effect of Cr2O3 NS insertion on the hydrogen permeation resistance was evaluated. The aim of this study is to explore the potential of 2D materials as nanofillers for enhancing the hydrogen permeation resistance of ceramic coatings.
A rapid heat treatment method was used to fabricate the Cr2O3 NSs. In this study, 0.3 g of CrCl3·6H2O (Analytically pure, Aladdin) was heated by a rapid heat furnace (OTF-1200X). The temperature of the heat treatment was 450 ℃, and the heating rate was 25 ℃ s-1. The heat treatment lasted for 600 s. The product of the heat treatment was washed and then separated by centrifugation. After cleaning processes, the Cr2O3 NSs were then collected by lyophilization for characterization and subsequent experiments.
The Cr-Zr-O hybrid sol was prepared as follows. First, 3 g zirconium (Ⅳ) acetate hydroxide (AR, SCR) was dissolved in a mixture solvent, which was composed of ethanol (50 ml, AR, SCR), acetone (2.5 ml, AR, SCR) and glacial acetic acid (50 μl, AR, SCR). After the whole solid dissolved, the solution stood for 24 h to obtain ZrO2 sol, and then 4.9 g chromic acetate (AR, Aladdin) was dissolved in the ZrO2 sol to obtain the Cr-Zr-O hybrid sol.
In this study, 321 stainless steel was used as the substrates. The size of the substrates was ϕ12×0.5 mm. Before the coating process, the substrate plates were ground by SiC abrasive paper to 2000 grids and then polished using diamond paste (1 μm particles). After the polishing process, the substrates were degreased in ethanol by an ultrasonic cleaner.
Cr2O3 NS concentration gradients of 0 g l-1, 0.5 g l-1, 1.0 g l-1 and 1.5 g l-1 were implemented to make the Cr2O3 NSs@Cr-Zr-O hybrid sol. All these types of hybrid sol were used to deposit coatings for subsequent experiments and characterizations. The dip-coating method was used to make the coated sample. As in a typical dip-coating procedure, the polished substrate was firstly sunk into the hybrid sol and pulled out at a speed of 400 μm s-1. The sample was dried at 80 ℃ for 40 min to remove volatilization organics, and then the sample was calcined at 400 ℃ for 30 min. This dipping-stoving-calcination cycle was repeated three times to form a coating. Finally, the coated sample was calcined at 600 ℃ to form a stable crystal structure. A diagram of the coating fabrication process is shown in figure 1.
The samples made from the hybrid sol with different NS concentrations of 0.5 g l-1, 1.0 g l-1 and 1.5 g l-1 were named as 0.5Cr2O3NS@Cr-Zr-O, 1.0Cr2O3NS@Cr-Zr-O and 1.5Cr2O3NS@Cr-Zr-O, respectively.
The permeation reduction factor (PRF) and permeation flux are two important indexes that are used to measure the performance of a deuterium permeation barrier. The self-constructed gas-driven deuterium permeation test device was depicted in our previous work [22–26], which is separated by the sample into upstream and downstream cavities. A dynamic vacuum (10-5 Pa) is kept in the upstream and downstream cavities by two molecular pumps. Before the experiment, the relationship between deuterium leakage and the current ion is calibrated by a standard D2 leakage. In the permeation experiment test, pressure dependent measurements were conducted under driven-pressure gradients of 20, 40, 60 and 80 kPa to calculate the pressure exponent. During the permeation experiments, the upstream D2 pressure is maintained at a constant 40 kPa. A tube furnace was used to control the temperature of the samples from 550 ℃ to 400 ℃. The D2 ion current is tracked by a quadrupole mass spectrometer in the downstream cavity.
The relationship between deuterium permeation leakage and upstream pressure is presented as the following equation [6]:
| J=Ppnd. | (1) |
In this equation, J is the permeation flux per unit area, which can be calculated from the D2 ion current, P is the permeability of the sample, p is the driven pressure of deuterium and d is the sample thickness. In this equation, the pressure exponent n is a constant at a certain test temperature and can be calculated from a fitting curve of the permeation flux and driven pressure. The PRF, which characterizes the barrier performance of the coating, is presented as the following equation:
| PRF=JsubstrateJcoating | (2) |
In the equation, Jsubstrate is the permeation flux of the uncoated sample, and Jcoating is the permeation flux through the coated substrate. All of the permeation flux and permeability indexes are used to analyze the performance of different composite coatings.
The chemical component of the coatings was characterized using grazing incidence x-ray diffraction (GIXRD, D8 ADVANCE, Cu Kα), and the incidence angle was 0.5°. The microstructures of the Cr2O3 NSs and coating samples were observed by a field emission scanning electron microscope (Sirion 200). The crystalline phases of the coated samples and Cr2O3 NSs were observed using transmission electron microscopy (TEM, Tecnai G2 F30/F20). The roughness of the coated samples and the thickness of the Cr2O3 NSs were observed using atomic force microscopy (AFM, SPA400). The firmness of the coating was measured by a scratch tester (CSM-MCT).
For many metal oxides, the non-existence of a layered structure leads to failure when producing NSs by exfoliation methods. However, a layered structure exists in the crystal lattice of some hydrous metal chlorides, of which the corresponding metal oxides are a research focus. When these hydrous chlorides are heated in the vacuum at a high temperature, the following reactions occur [12]:
| MClx(H2O)y→MClx+yH2O | (3) |
| MClx(H2O)y→M(OH)x+xHCl+(y-x)H2O | (4) |
| MClx+xH2O→M(OH)x+xHCl | (5) |
| 2M(OH)x→M2Ox+xH2O. | (6) |
Using the powerful rapid thermal process of hydration and hydrolysis, a large number of gaseous products, such as HCl and H2O steam, are formed in a short time, leading to a steep pressure rise inside the crystal lattice. The release of gas will drive exfoliation and produce layered intermediates. After exfoliation, a hydrated reaction occurs to transform the layered intermediates into metal oxide NSs. According to the above rapid thermal reactions, Cr2O3 NSs were produced from the CrCl3·H2O precursor.
Scanning electron microscopy (SEM) and TEM were used to characterize the morphology of the Cr2O3 NSs. As shown in figures 2(a) and (b), a typical monolayer structure is observed, which indicates the existence of NSs. There is an obvious halo in the diffraction pattern, indicating that the sample is amorphous. Energy dispersive spectroscopy (EDS) was used to detect the chemical elementary component of the NS. As shown in figures 2(e)–(g), there are mere residual chlorides in the sample and the main ingredients are chromium and oxide.
To confirm the quality of the NS resulting from the rapid thermal method, AFM was used to measure the thickness of the Cr2O3 NSs. In the AFM image (figure 2(h)), a strip-like NS is observed with a thickness of only 4.6 nm (figure 2(i)). These results indicate that amorphous Cr2O3 NSs were successfully obtained using a rapid heat treatment method.
The surface morphology of the Cr2O3 NS inserted Cr-Zr-O coating with different NS concentrations is shown in figure 3. With the increase of the NS concentration in the precursor sol, the surface feature of the composite coating transforms dramatically. When the NS concentration is 0.5 g l-1, a smooth surface with a flake-like structure is shown in figures 3(a) and (b). With the NS concentration increasing, the flake-like NSs occupy a large area of the surface when it comes to 1.0 g l-1 (figures 3(c) and (d)). At an even higher concentration of 1.5 g l-1, a porous structure is shown on the coating surface with obvious agglomerates and holes found (figures 3(e) and (f)). These results indicate that the increase in the NS concentration influences the morphology of the coating directly and induces the formation of an orderly flake-like structure, which can help to hold the coating integrity and decrease porosity. However, when it reaches an excessive level, surplus NSs will deteriorate the integrity of the coating and lead to a porous structure conversely.
To verify the influence of NS concentration on the coating morphology, AFM was used to characterize the roughness of the coated samples. The roughness (Rq) of the 0.5Cr2O3NS@Cr-Zr-O, 1.0Cr2O3NS@Cr-Zr-O and 1.5Cr2O3NS@Cr-Zr-O samples is 51.6 nm, 79.4 nm and 55.8 nm, respectively. In figure 4, on the surfaces of the 0.5Cr2O3NS@Cr-Zr-O and 1.5Cr2O3NS@Cr-Zr-O samples a hump-like structure is found. For the 0.5Cr2O3NS@Cr-Zr-O coating, it demonstrates that the introduction of NSs increases the roughness of the coating (figures 4(a) and (b)), and for the 1.5Cr2O3NS@Cr-Zr-O sample, it indicates that surplus NSs combine with the sol-gel coating matrix and construct a similar hump-like surface (figures 4(e) and (f)). In the middle of these two concentrations, the coating with 1.0 g l-1 NSs shows greater roughness than the others. The difference in roughness is caused by the NS accumulation (figures 4(c) and (d)), which is also obvious in the SEM images. The varying roughness with the increase in NS concentration indicates that a specific concentration of Cr2O3 NSs can accumulate on the coating surface, but without deteriorating the matrix.
The cross-sectional microstructure of the 1.0Cr2O3NS@Cr-Zr-O coating was further observed by TEM and EDS. As shown in figure 5(a), a layer-like structure is observed and the thickness of the coating is about 193 nm, indicating that the repeated dip-coating process constructed an integral coating on the substrate. The EDS patterns display the formation of a Cr-Fe diffusion layer (figures 5(b) and (c)), and it is obvious that the heat treatment induces the segregation of Zr and Cr in the coating (figures 5(b)–(d)). Interestingly, the cross-section structure of the composite coating is composed of three layers of ZrO2 on the top and one layer of Cr2O3 at the bottom (figures 5(b), (d) and (e)). Due to the limited amount of NSs inserted into the coating, it is difficult to characterize the Cr2O3 NS in ZrO2 layers by TEM. The distribution of Cr2O3 NSs is not uniform because of their easy aggregation due to a big specific surface area and also their sedimentation during coating deposition. In the coating deposition process, the Cr2O3 NS sank to a Cr2O3 layer at the bottom, which affected its distribution and deteriorated the compaction of the ZrO2 layer, as the TEM image showed. Some NSs appear on the surface of the coating due to the surface tension. High-resolution TEM (HRTEM) was used to characterize the microstructure of the ZrO2 layer (figure 5(f)). An obvious nanocrystal structure is observed, and the growth directions of ZrO2 are (1 2 1) and (2 0 0). Cr2O3 in the (1 1 6) direction is also observed, which indicates that the segregation inside the coating was not complete. The absent distribution of Cr in the upper layer suggests that Cr2O3 nanocrystals were rarely formed in the ZrO2 layer. The strip-like amorphous phase may be related to the existence of amorphous Cr2O3 NSs in the coating.
The crystal phase of the coating was determined by x-ray diffraction (XRD). The main components are Cr2O3 and ZrO2, which is in agreement with the EDS results. As shown in figure 6, when the concentration of NSs reaches 1.0 g l-1, the signals of the (1 0 1) and (1 2 1) peaks become more obvious, which indicates that the crystallinity of tetragonal ZrO2 in the coating is improved [27]. The XRD results indicate that nanocrystal tetragonal ZrO2 is formed inside the amorphous ZrO2 layer [4–6], which may affect the permeation resistance of the coating.
The critical load of the coating for different NS concentrations is shown in figure 7. The scratching speed is 4 mm min-1 and the length of scratches is 2 mm. In scratch tests, the loading rate is 20 N min-1. The relationship between the NS concentration and bonding force is a positive correlation, which indicates that the addition of 2D nanomaterial improves the physical strength of the coating.
Different driven pressures were used for the 1.0Cr2O3NS@Cr-Zr-O samples in the deuterium permeation tests. The fitting curve of the driven pressure and permeation flux is shown in figure 8(a). The pressure exponent at different temperatures is near to 1.0, which indicates that the D2 permeation in a coated sample is a surface-limited process [6].
The PRF can be used to evaluate the coating quality for deuterium permeation reduction. The PRFs of four different coatings with different concentrations of Cr2O3 NSs are shown in figure 8(b). The 1.0Cr2O3NS@Cr-Zr-O has the highest PRF among these samples at a high temperature, which reaches 575 ℃ at 500 ℃, increasing from 249 compared with the PRF of the coating without NSs.
To measure the effect of NS concentration on deuterium permeation reduction ability, the permeability indexes of four coated samples at different temperatures are listed in figure 8(c), which indicates that adding 1.0 g l-1 NS in the precursor sol can restrain the permeability of deuterium to the lowest level at a high temperature above 450 ℃. However, the 0.5Cr2O3NS@Cr-Zr-O presents a better barrier performance than 1.0Cr2O3NS@Cr-Zr-O at 400 ℃.
As shown in figures 8(d) and (e), the composite coating reduces deuterium permeation flux by two orders of magnitude when compared with the substrate. Among the four coating samples, 1.0Cr2O3NS@Cr-Zr-O shows that the introduction of 1.0 g l-1 Cr2O3 NSs can improve the deuterium resistance obviously (increasing the PRF from 249 to 575). The activation energy of the 0.5Cr2O3NS@Cr-Zr-O, 1.0Cr2O3NS@Cr-Zr-O and 1.5Cr2O3NS@Cr-Zr-O samples, obtained by their permeability, is 74 kJ mol-1, 86 kJ mol-1 and 71 kJ mol-1, respectively, which indicates that the coating with a NS concentration of 1.0 g l-1 has the highest activation energy.
A retention test was conducted on the 1.0Cr2O3NS@Cr-Zr-O sample to measure the deterioration rooted in it. The first deuterium permeation test was conducted for the 1.0Cr2O3NS@Cr-Zr-O sample under 40 kPa. The repeated permeation test was conducted for the sample after the first test. The PRF indexes of the first and the second permeation tests are shown in figure 8(f). A decline in the PRF occurs in the second test; the results indicate that the retention effect of the coating can clearly affect the permeation resistance process. This feature may lead to the deterioration of the resistance effort in long-turn work. The permeation behavior of the coatings in this work is summarized in the table 1.
| NS concentration (g l-1) | Thickness (nm) | PRF at 500 ℃ | Permeability at 500 ℃ (mol m-1 s-1 Pa-1.05) | Permeation flux at 500 ℃ (mol m-2 s-1) | Permeation activation energy (kJ mol-1) |
| 0 | ~190 | 249 | 4.4491×10-17 | 6.04597×10-9 | 72 |
| 0.5 | 500 | 2.2237×10-17 | 3.02189×10-9 | 74 | |
| 1.0 | 575 | 1.9336×10-17 | 2.62773×10-9 | 86 | |
| 1.5 | 269 | 4.13336×10-17 | 5.61689×10-9 | 71 |
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The improving deuterium resistance may relate to the morphology of the coating shown in figures 3 and 5. An obvious multilayer structure is observed in the cross-section image of the coating. The formation of the Cr2O3 diffusion layer underneath the ZrO2 layer is beneficial to improve the barrier effect. On the other hand, the insertion of Cr2O3 NSs distributed inside the coating can create new interfaces that will prolong the pathway for deuterium permeation; however, the distribution of NSs is nonuniform because of the segregation of Cr2O3 in the coating fabrication process. All these factors can help to achieve a higher PRF [28, 29]. However, the addition of surplus NSs deteriorates the integrality of the coating and also increases the porosity, which will accelerate deuterium permeation undesirably. For this reason, the NS content incorporated in the coating should be optimized to a certain value to maximize the deuterium resistance of the composite coatings. However, the low-density structure of the coating leads to an obvious retention effect, which may instigate deterioration in long-term work. Further investigation is needed to check its viability in a practical situation.
In summary, a Cr2O3 NS induced Cr-Zr-O coating was fabricated on 321 stainless steel substrates. The composite coating was composed of a top ZrO2 layer and a bottom Cr2O3 layer. The content of the Cr2O3 NSs directly affects both the morphology and deuterium resistance of the composite coating. With 1.0 g l-1 Cr2O3 NSs added to the precursor sol, the resultant 1.0Cr2O3NS@Cr-Zr-O exhibits the best deuterium permeation reduction ability, the PRF of which was enhanced from 249 to 575 compared with the Cr-Zr-O coating. The composite coating with a thickness of nearly 193 nm increased the deuterium resistance of the substrate by above two orders of magnitude. However, the low-density structure of the coating leads to an obvious retention effect, which may deteriorate the long-term resistance. Further investigation is needed to check its viability in practical situations. The enhancement in deuterium resistance is related to the prolonged pathway for deuterium permeation by inserting NSs. This work demonstrates a new way to enhance the barrier performance of ceramic coatings such as TPBs.
This work was supported by the National MCF Energy R & D Program of China (No. 2018YFE0313300), National Natural Science Foundation of China (Nos. 52273224, 51402116), and the Fundamental Research Funds for the Central Universities (Nos. 2018KFYYXJJ028, 2019KFYXMBZ045). The authors thank the Analytical and Testing Center of Huazhong University of Science and Technology for their support.
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Figures(8) / Tables(1)
Supported by: Beijing Renhe Information Technology Co., Ltd. 
| NS concentration (g l-1) | Thickness (nm) | PRF at 500 ℃ | Permeability at 500 ℃ (mol m-1 s-1 Pa-1.05) | Permeation flux at 500 ℃ (mol m-2 s-1) | Permeation activation energy (kJ mol-1) |
| 0 | ~190 | 249 | 4.4491×10-17 | 6.04597×10-9 | 72 |
| 0.5 | 500 | 2.2237×10-17 | 3.02189×10-9 | 74 | |
| 1.0 | 575 | 1.9336×10-17 | 2.62773×10-9 | 86 | |
| 1.5 | 269 | 4.13336×10-17 | 5.61689×10-9 | 71 |
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