Kenkyu Journal of Nanotechnology & Nanoscience ISSN : 2455-183X
National Key Laboratory for Welding and Surface treatment Technologies, National Research Institute of Mechanical Engineering, 4 Pham Van Dong, Caugiay, Hanoi, Vietnam
Hanoi University of Industry, Hanoi, Vietnam
National Key Laboratory for Welding and Surface treatment Technologies, National Research Institute of Mechanical Engineering, 4 Pham Van Dong, Caugiay, Hanoi, Vietnam
Tuan Anh Nguyen, Institute for Tropical Technology, Vietnam Academy of Science and Technology, 18 Hoang Quoc Viet, CauGiay, Hanoi, Vietnam; Email: ntanh@itt.vast.vn
Received: 25-08-2020
Accepted: 20-10-2020
Published: 22-10-2020
Citation: Cuong Ngo Xuan, Ha Tuan Nguyen, Quy Le Thu, Tuan Anh Nguyen (2020) Fabrication of Plasma Sprayed SiC-Cu Cermet Coatings, Kenk Nanotec Nanosci 6:15-33
Copyrights: © 2020, Tuan Anh Nguyen et al,
In this work, SiC-Cucermet coatings were deposited on C45 steel substrate by using the plasma spray technique, at varying spaying parameters under atmospheric or Argon gas ambiances. The microstructure of sprayed coatings was exanimated by using scanning electron microscopy (SEM).The coating elemental and compositional analysis was performed by using Energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) techniques. SEM/ EDX/ XDR results indicate that the optimal factors were: (i) 85SiC : 15Cu powder feedstock, (ii) 42 g/min powderfeed rate, (iii) 380 A plasma current, (iv) 50 mm spraying distance, and v) under Argon gas protection. The apparent porosity of sprayed coatings was only in range from 1.38 % to 1.65 %. The average thickness of coatings was in range from 200 µm to 300 µm. By SEM images, many SiC particles are seen in the coating, but their shape become smoother than that in the as-received SiC powder - due to the presence of Cu in their surface as binder. XRD analysis indicated that content of SiC phases is 86 ±3 %.wt; and Cu content is 14 (±3%) wt.%. The application of this plasma spayed SiC-Cu coating is very promising in the severe corrosion environment.
Keywords: SiC; Cu; plasma spray; cermet coating, SiC-Cu coating
By having excellent thermal, chemical and mechanical properties, SiC has been considered as the most promising ceramic for high performance applications in the aggressive environments.
In the field of coating science, SiC is expected to provide the extremely high anti-corrosion, strong wear resistance, heat and chemical resistant properties for both industrial and space applications (against wear and high temperature oxidation) [1].
In this regard, SiC can be used in various types of coatings, such as organic, metallic and ceramic coatings. In case of organic coatings, SiC particles had been used as filler/reinforcer in various types of organic/polymeric matrices, such as polyfluo wax/polyurethane [2], polyetheretherketone [3, 4], poly(o-toluidine) [5], epoxy [6, 7]. For metallic coatings, SiC particles could be embedded into metallic matrices, such as Cu [8, 9], Al [10, 11], Ni [12-19], Ni-Co [20], Co [21] matrices.
SiC coatings have been mostly fabricated by using the chemical vapor deposition (CVD) [22, 23], with low growth rate (~10 µm/h - without adding HCl to the standard process [24] and small scale production. For industrial scale-up application, thermal sprayed SiC-based ceramic coatings have been developed.
Regarding the thermal sprayed SiC coatings, many efforts had been carried out to fabricate the pure (100%) SiC coating, but still being challenge due to the nature of SiC raw material. Several approaches have been developed, such as i) plasma spraying at high current/power to melt the SiC powder material, ii) conventional plasma spraying for mixture of SiC and other ceramics (with lower melting point for a eutectic phase, and iii) plasma spraying at low current/power to fabricate the SiC/metal cermet coating using metallic phases as binders (bonding agents).
On the first approach, many researchers, including our group, found that SiC was decomposed under plasma spraying process at high current/power. It was reported in literature that pure SiC coating could not be deposited by thermal spray because SiC materials should decompose before melting [25]. That is why we could only observe small amount of SiC phases in XRD pattern, along with its decomposed products.
On the second approach, Tului et al. [25] successfully fabricate the coatings containing up to 66 vol.% of SiC by plasma spray, using a mixture of SiC and ZrB2 as spraying material. As reported, these two compounds formed a eutectic phase, at a temperature lower than that of SiC decomposition.
Regarding the third pathway, incorporation of metallic binders could facilitate the bonding of SiC particles, allowing SiC-based coating to be deposited. Recently, we successfully fabricated the ceramic/metal cermet coatings using plasma spaying (Cr3C2-25NiCr coating) for protection of steel from corrosion-erosion [26]. Thus we focus on the SiC-Cu cermet coating in this work.
The most common method for fabricating of SiC-Cu composite is the powder metallurgy (PM) with sintering or hot-pressing, at the temperature below the melting point of SiC (2830 0C). However, significant decomposition of SiC in PM process was observed by several researchers [27, 28]. Kang et al [9] fabricated the SiC/Cu metal matrix composite (MMC) using plasma spray. The authors prepared ball-milled Cu/SiC powder as spraying materials(powder feedstock)at different portions (Cu–27SiC, Cu–50SiC, Cu–60SiC) of SiC powder (<45 µm) and Cu powder (<45 µm). The authors indicated that SiC was decomposed into Si and C, and copper silicide was then formed under plasma spaying. Similarity, several works have been done for decomposition of SiC-Cu powder mixture. Suganuma et al. [29] indicated that when SiC was in contact with Cu, it decomposed into Si and fine carbon at 1100 oC. Lee et al. [30] found the formation of Cu7Si and very small amount of graphite in the interface of Cu and SiC at the reaction temperature of 1100 oC.
In this work, we focus on the third approach, using plasma spraying at low current/power to avoid the degradation of SiC material. Cu sub-micro particles will be mixed with SiC powder as spraying material. These Cu particles are expected not only to bond the SiC particles, but also to protect SiC from degradation during the plasma spraying process. In addition, in this study, we use the inert gas (Argon) to protect both spraying materials and coatings during the plasma spraying process. This idea comes from the fact that Argon can be used as inert/shielding gas in the plasma arc welding.
2.1. Materials
SiC powder (> 80%, density: 3.2 g.cm-3) was obtained from Ermakchim (Russian Federation).Cu powder (>95%, density: 8.96 g.cm-3) was provided by Guangzhou Hongwu Material Technology(China).The steel (C45 - DIN 17200, Russian) substrates were high carbon steel with the chemical composition: C(0.42-0.5%), Mn (0.5-0.8%), P (≤0.035%), S (≤0.04%), Si (0.17-0.37%), and Cr (0.2-0.4%). The size of steel coupons was 50×50×5 mm. Prior to the plasma spraying, the surface of steel coupons was cleaned by abrasive blasting (using Al2O3 powder) until their roughness (Rz) reached a value of ~ 50 μm.
2.2. Coating preparation
SiC-Cu coatings were fabricated by using 3710 Plasma spray equipment-PRAXAIR-TAFA (USA, Figure 1). The technology parameters (powder feed rate, spray distance, plasma current) has been presented in the Table 1.
Figure 2 shows the standard SG-100 gun (a) and customized SG-100 gun (b) for Argon protection of materials and coating during the spraying process. As can be seen in Figure 2, the size of plasma flame with standard gun (Fig. 2a) is much larger than that with the customized gun (Fig. 2b), due to the presence of oxygen in the ambience.
For comparison, SiC-Cu coatings are plasma sprayed with both standard (Air deposition) and customized (under Argon protection/under shielding Argon) SG-100 guns.
2.3. Characterization
The thickness of the coatings was measured by using Digi-Derm (Model DGE-745, Mituyo, Japan). The apparent porosity of sprayed coatings was determined by using the optical microscopy analysis (Axiovert 40 MAT, Carl Zeiss, Germany), according to the ASTM B276 standard.
The morphologyand elemental compositionof powder feedstock and coatings were analyzed by using FEI Nova Nano SEM 450 Scanning Electron Microscope (Japan) with Energy-dispersive X-ray spectroscopy (EDX) option.
To identify the possible phases that present in the powder and coatings, X-ray diffraction (D8- Advance, Bruker instrument, Germany) has been used at temperature of 25°C, with 2θ angle scanningfrom 15˚ to 65˚. The obtained X-ray diffraction patterns are analyzed (using the Eva software) and semi-quantitative evaluation (using Dquant software with an error of ± 3%).
3.1. Characterization of powder materials
a. SiC powder
Figure 3 shows the SEM image of as-received SiC particles. As can be seen in Fig. 3, the SiC has an angular morphology for hard particles, with a mean diameter of 40 - 50 μm. To evaluate the elemental composition of this as-received powder, EDX analysis was used (Figure 4). From the EDX spectrum, the content of Si element in this powder ranges from 58 wt.% to 60 wt.%. Whereas, the content of C element ranges from 35 wt.% to 37 wt.%. In addition, Aluminum and Oxygen elements are observed at the contents of 0.6-0.8 wt.% and 4-5 wt.%, respectively.
To identify the phases that present in this powder, X-ray diffraction method has been used. Figure 5 presents the XDR pattern of SiC as-received powder. As can be seen in this figure, XRD of the prepared SiC shows the single phase of SiC was hexagonal (at content of 78.2%). In addition, one weak diffraction peak for SiO2 was observed.
Figure 1: Plasma spray equipment 3710-PRAXAIR-TAFA (USA)
|
Coatings |
Powder feed rate (g/min) |
Spray distance (mm) |
Plasma current (A) |
Voltage (V) |
Gas flow rate (L/min) |
|
|
Argon |
Hydrogen |
|||||
|
SiC-50Cu (in Air) |
42 |
50 |
380 |
58 |
50 |
8 |
|
SiC-20Cu (in Argon) |
42 |
50 |
380 |
58 |
50 |
8 |
|
SiC-15Cu (in Argon) |
42 |
50 |
380 |
58 |
50 |
8 |
Table 1: Technological regimes for plasma spraying of SiC-Cu cermet coatings
Figure 2: a) Standard SG-100 gun, b) Customized SG-100 gun for Argon shielding of materials and coating during the spraying
Figure 3: SEM image of SiC powder. Magnification: × 550
Figure 4: EDX spectrum of SiC as-received powder.
Figure 5: XRD diffraction pattern of SiC as-received powder
b. Cu powder
Figure 6 shows the SEM image of as-received Cu particles. As can be seen in Fig. 4, the Cu exhibits as soft flake particles, with a mean diameter of ~1 μm. Figure 7 presents the EDX spectrum for this Cu as-received powder. Calculation from this EDX spectrum indicates that the contents of elements that present in this powder are C (1.38 wt.%); O (0.3wt.%); Fe: (1.5 wt.%) and Cu (96.82%).
Regarding the mixture of Cu and SiC powders as feedstock, due to the density difference between Cu (ρ = 8.96 g.cm-3) and SiC (ρ = 3.2 g.cm-3), we have to select the different size of
Cu and SiC particles, such as 1 µm and 50 µm, respectively. In addition, in order to mix them uniformly, various portions (SiC : Cu) of mixture are prepared, such as 50:50; 80:20; 85:15 and 90:10.
3.2. Coating characterization
SiC-Cu cermet coatings have been deposited on C45 steel substrates with various Cu contents in the powder feedstock (from 10% to 50%) using plasma spraying method (Figure 1). Each sample was sprayed during 5 minutes (Figure 1b), and then its thickness was measured/checked on-site. Figure 8 presents the average values of their thickness. As can be seen in Figure 8, the thickness of coatings is these SiC-Cu coatings is in range of 200-300 μm, with the SiC-15Cu being the lowest (204.67 ± 26.5 µm). This lowest value might be attributed to the lowest content of Cu powder in the feedstock powder. In case of SiC-20Cu coating, its thickness has the highest value (295.67 ± 21.5 µm), whereas it is 220 (± 20.5) µm for SiC-50Cu coating.
We also estimate the thickness by using optical microscope for the cross section of the sprayed coatings. Figure 9 presents the cross-sectional image of SiC-20Cu coating att the optical magnification of 200 times. As can be estimated from this figure 9, the thickness is about 280 µm.
In addition, we had also tried to fabricate the coating at 90SiC:10Cu portion, but no coating had been deposited on the steel surface, due to the low content of Cu powder in the feedstock acting as the binders (to facilitate the bonding of SiC particles under spraying).
In the next parts, we discuss the morphology and elements/phases that present in these coatings.
Figure 6: SEM image of Cu powder. Magnification: × 500
Figure 7: EDX spectrum of SiC as-received powder.
Figure 8: Thickness values of plasma sprayed coatings
Figure 9: Cross-sectional image of SiC-20Cu coating. Magnification: × 200
a. SiC-50Cu coating sprayed in air
Figure 10 shows the SEM images of surface for SiC-50Cu coating. The surface is slightly rough and may round particles (1-5 µm) are obvious. No solid (hard) SiC particles (40-50 µm) are seen in Figure 10. To verify the presence of SiC in this coating, EDX and XRD have been carried out. Based on the EDX analysis (Figure 11), the element composition is C (6.3 wt.%); O (7.09 wt.%); Si: (3.66 wt.%) and Cu (81.13 wt.%). XRD analysis (Figure 12) confirms that this coating contains mostly of Cu (face centered cubic). Other weak diffraction peaks are contributed to CuO2 and Aluminum Silicon Carbide (Al8SiC7).
SEM/EDX/XRD analyses indicate the decomposition of powder feedstock during plasma spraying process due to spraying environment in air (using the standard plasma gun, Figure 2a). Thus, the content of SiC in this SiC-50Cu coating is undetectable or too low (few % ).
To avoid these issues, we use the customized plasma gun (for Argon protection, Figure 2b) and reduce the content of Cu powder in feedstock for other coating samples in the next sections.
b. SiC-20Cu coating sprayed in Argon
Figure 13 shows the surface of plasma-sprayed SiC-20Cu coating. The surface is rough and some pores are observed. In addition, numerous SiC particles are also seen, but their shape become smoother than that in the as-received SiC powder (due to the presence of Cu in their surface as binder). EDX analysis (Figure 14) indicates the high content of Si in the coating with the element composition: C (19.96 wt.%); O (29.96 wt.%); Si (28.37 wt.%); Fe (1.27 wt.%) and Cu (7.24 wt.%). Based on the XRD analysis (Figure 15), the content SiC phases is ~53 wt.% (~ 42%: crystalline phase; ~ 11%: amorphous phase), and Cu content is about ~ 47 wt.% (using Dquant software with an error of ± 3%).
Figure 10: SEM image of SiC-50Cu coating (sprayed in Air). Magnification: × 750
Figure 11: EDX spectrum of SiC-50Cu coating (sprayed in Air).
Figure 12: XRD diffraction pattern of SiC-50Cu coating (sprayed in Air).
Figure 13: SEM image of SiC-20Cu coating (sprayed in Argon). Magnification: × 500.
Figure 14: EDX spectrum of SiC-20Cu coating (sprayed in Argon).
Figure 15: XRD diffraction pattern of SiC-20Cu coating (sprayed in Argon).
c. SiC-15Cu coating sprayed in Argon
Figure 16 presents the surface of plasma-sprayed SiC-15Cu coating. As can see in this figure, there are many solid SiC particles. EDX analysis (Figure 17) indicates the higher content of Si in the coating, as compared to the SiC-15Cu coating. The elemental composition is C (29.81 wt.%); O (8.24 wt.%); Si (40.79 wt.%); Fe (3.18 wt.%) and Cu (17.01 wt.%). Based on the XRD analysis (Figure 18), the content SiC phases is ~86 wt.% (~ 71%: crystalline phase; ~ 15%: amorphous phase), and Cu content is about ~ 14 wt.% (using Dquant software with an error of ± 3%).
Figure 19 presents the cross-sectional photos of SiC-15Cu coating for evaluation of apparent porosity (taken by an optical microscope Axiovert 40 MAT). From the optical microscopy analysis, the values of apparent porosity are in range from 1.38 % to 1.65 %. This average value is much lower than that for the plasma sprayed Cr3C2-25NiCr cermet coating (from 3.1% to 3.4% [26]). In the previous work [26], we used the Cr3C2-25NiCr powder (35±5 µm) as feedstock, under plasma current of 600 A atmospheric ambiance (spray distance of 100 mm). Reduction of porosity for SiC-15Cu coating could be attributed to the combination of i) the presence of Cu sub-micro particles in powder feedstock, ii) low plasma current of 380 A, iii) short spray distance (50 mm) and iv) Argon gas protection under plasma spraying process.
The presence of Cu sub-micro particles (together with SiC particles) in powder feedstock is not only to bond the SiC particles, but also to protect SiC from degradation during the plasma spraying process, thus reduces significantly the porosity of coating.
Figure 16: SEM image of SiC-15Cu coating (sprayed in Argon). Magnification: × 500
Figure 17: EDX spectrum of SiC-15Cu coating (sprayed in Argon).
Figure 18: XRD diffraction pattern of SiC-15Cu coating (sprayed in Argon).
Figure 19: Cross-sectional photos of SiC-15Cu coating. Magnification: × 200 A) Optical image, B) Image with annotations
The main findings of this research were:
For the next study:
- For industrial application, SiC-15Cu coatings will be then sealed with polytetrafluoroethylene (PTFE) emulsion to enhance further their corrosion and wear resistances.
- The erosion resistance of this SiC-15Cu coating (with or without nano-PTFE sealant) will be carried out by using a slurry flow (SiC particles in HF/HCl solution) at 70 oC, under rotational speed 950 rpm (Figure 20).
- For industrial application, the nano-PTFE sealed SiC-15Cu coating will be used to protect pump chamber against the apatite sludge solution (Figure 21).
Figure 20: A) Customized corrosion testing chamber; B) systematic design: 1- PTFE based (chemical) tank, 2- Testing samples, 3- Rotator.
Figure 21: Protection of pump chamber against the sludge solution: a) sludge pump; b) pump chamber without coating, c) pump chamber with nano-PTFE sealed SiC coating
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