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The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Properties
The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Performance The size of WC particles in the original powder directly affects the microstructure and performance of tungsten carbide coatings sprayed onto a substrate. Nanocrystalline tungsten carbide coatings prepared using nanoscale powders exhibit higher hardness and toughness, as well as superior wear resistance, compared to micron-sized tungsten carbide coatings made from conventional micrometer-scale powders. Recent studies have shown that tungsten carbide coatings prepared using micro-nano composite powders outperform those made from purely nanoscale powders. However, there are currently relatively few reports on this topic. Therefore, this paper systematically investigates the microstructure and performance of supersonic flame-sprayed nanoscale, micro-nano composite, and micron-sized tungsten carbide coatings, exploring the impact of the original powder’s WC particle size on coating microstructure and performance. 1 Experimental Setup 1.1 Preparation of Tungsten Carbide Coatings Three types of WC-CoCr powders—FN-WC, PN-WC, and M-WC—with nano-, nano-micron mixed, and micron-sized WC particles were used as spray powders. In the FN-WC powder, aggregated nanoscale WC particles form micron- or submicron-sized agglomerates, which are then bonded together by a binder, as shown in Figures 1(a) and 1(b). The average particle size of these agglomerates ranges from 18.85 to 37.56 μm, with a loose bulk density of 5.48 g/cm³. The morphology of the PN-WC powder is illustrated in Figures 1(c) and 1(d); its cross-sectional microstructure reveals some free nanoscale particles along with predominantly submicron- or micron-sized particles. The average particle size of the PN-WC powder is 23.33–44.79 μm, with a loose bulk density of 5.6 g/cm³. The morphology of the M-WC powder is shown in Figures 1(e) and 1(f); the WC particles in the powder end-face microstructure range from 0.5 to 3 μm in diameter, with an average particle size of 21–50 μm and a loose bulk density of 5.0 g/cm³. XRD diffraction comparisons (Figure 2) and analysis results (Table 1) indicate that the WC particle size in the FN-WC powder is slightly smaller, followed by the PN-WC powder, while the M-WC powder has slightly larger WC particles. Table 1: Half-Width at Half-Maximum of Main WC Peaks Powder FWHM/(°) FN-WC 0.194 PN-WC 0.157 M-WC 0.148 The substrate used was 0Cr13Ni5Mo martensitic stainless steel. Before spraying, the substrate surface was cleaned and sandblasted. The spraying equipment was an HVOF system manufactured by SulerMecto in the United States. Propane was used as the fuel gas, high-pressure oxygen as the oxidizer, and nitrogen as the powder feed gas during spraying. The spraying process parameters are listed in Table 2. Table 2: Spraying Parameters Parameters Values Pressure (O₂)/MPa 1.0 Flow rate (O₂)/(L·min⁻¹) 240 Pressure (C₃H₈)/MPa 0.6 Flow rate (C₃H₈)/(L·min⁻¹) 68 Spray distance/mm 200 1.2 Microstructural and Mechanical Property Testing The microstructure of the coatings was analyzed using a FeiQuata400HV scanning electron microscope. Coating porosity was determined according to JB/T75059-1994. The bond strength of the coatings was tested using the paired specimen tensile test method specified in GB/T8642-2002. The bond strength tests were conducted on a CSS-44300 electronic testing machine at a loading rate not exceeding (1000 ± 100) N/s. The microhardness of the coatings was measured using an HDX-1000TMC/LCD microhardness tester under a load of 300 g for 15 seconds; nine points were tested per sample, and the average microhardness value of each coating was calculated. 1.3 Abrasive Wear Testing The abrasive wear tests were performed using a particle erosion wear testing machine similar in structure to the ACT-JP testing machine from Japan. The erosion test parameters were as follows: erosion distance 100 mm, nozzle inner diameter 3.6–4.0 mm, nozzle length 22 mm, abrasive material brown corundum with a particle size of 149 μm (100 mesh), compressed air pressure 0.3 MPa, and erosion angles of 15° and 90°. 2 Results and Discussion 2.1 Microstructure of the Coatings Figure 3 shows the SEM images of the cross-sections of the sprayed coatings. The porosity of the three coatings was statistically analyzed at 5000x magnification. The results show that the porosities of the FN-WC, PN-WC, and M-WC coatings were 2.1%, 2.0%, and 2.3%, respectively, indicating comparable porosity levels among the coatings. At higher magnifications, most of the WC particles in the FN-WC coating had diameters less than 100 nm, as shown in Figure 3(a2). Additionally, some flat particle boundaries showed no presence of nanoscale WC particles, as seen in the bright white metallic regions in Figure 3(a2). These regions likely resulted from partial melting of the nanoparticles in the supersonic flame jet, causing the small nanoscale WC particles to decompose at high temperatures. In the PN-WC coating, most of the WC particles had diameters greater than 500 nm, even reaching around 2 μm; however, some nanoscale particles were also present in the coating, as shown in Figure 3(b2). In the M-WC coating, the WC particles were micron-sized, and large WC particles broke during the spraying process, retaining their fractured morphology within the coating. The metal bonding phase between the fragmented tungsten carbide particles was insufficient, as shown in Figure 3(c2). 2.2 Phase Structure of the Coatings Figure 4 shows the XRD analysis results for the FN-WC, PN-WC, and M-WC coatings. After processing, the FN-WC coating exhibited a slightly higher relative peak intensity for the W₂C phase, indicating a higher degree of decomposition during spraying. This result is consistent with the microstructural analysis. Nanoscale tungsten carbide particles tend to decompose easily in the supersonic flame jet; when most of the WC particles in the powder exist as nanoparticles, their decomposition becomes more severe. In the PN-WC and M-WC coatings, most of the WC particles were micron- or submicron-sized and did not easily decompose, resulting in only minor traces of the W₂C phase observed in the XRD patterns. 2.3 Microhardness of the Coatings Coating hardness refers to the material's ability to resist deformation or fracture within a small volume on the surface, and its magnitude significantly influences the coating's wear resistance and erosion resistance. Figure 5 shows the microhardness test results for the three tungsten carbide coatings. The Vickers hardness values of the PN-WC and FN-WC coatings were 1241 HV0.3 and 1254 HV0.3, respectively, slightly higher than the M-WC coating’s hardness of 1229 HV0.3. The hardness of the PN-WC coating was more concentrated. Combined with the microstructural photographs of the three coatings shown in Figure 3, it can be seen that the FN-WC coating contains pure metal areas resulting from the decomposition of WC particles, whereas the M-WC coating has many fragmented WC particles. The uneven microstructures of these two coatings led to dispersed hardness values, while the PN-WC coating had uniformly distributed micron-nano WC particles, resulting in a more concentrated distribution of hardness values. 2.4 Bond Strength of the Coatings Table 3 shows the bond strength of the coatings. The average bond strength of the PN-WC coating was over 73.5 MPa, and the primary fracture during the tensile test occurred within the adhesive layer. The average bond strength of the M-WC coating was comparable to that of the PN-WC coating, and both of these coatings had slightly higher bond strengths than the FN-WC coating. This may be related to oxidation and WC particle decomposition phenomena occurring in the FN-WC all-nanoscale coating during the supersonic flame jet. In the FN-WC all-nanoscale coating, samples 3–5 all fractured within the coating. Table 3: Bond Strength of the Coatings Coating Bonding Strength/MPa Mean Value/MPa Fracture Position 1 2 3 4 5 FN-WC 72.3 74.8 62.6 70.4 63.2 68.7 Coating + Glue PN-WC 70.7 75.8 72.0 76.9 72.3 73.5 Glue M-WC 73.2 69.4 77.2 76.3 68.6 72.9 Glue 2.5 Erosion Resistance Performance The erosion tests were conducted by subjecting the coatings to abrasive particles corresponding to 100 g every 15 seconds, weighing the coatings after each test cycle. After the erosion tests, the cumulative mass loss due to erosion was calculated and converted into volumetric loss caused by coating erosion, using this volumetric loss as a criterion for evaluating erosion resistance. A linear fit was applied to the cumulative volumetric loss data, and the reciprocal of the slope of the fitted line was defined as the erosion resistance coefficient Re. Under the same test conditions, a higher Re value indicates better erosion resistance of the coated material. The erosion resistance results for the FN-WC, PN-WC, and M-WC coatings at a small angle (15°) are shown in Figure 6. Although the FN-WC coating used all-nanoscale WC particles, its erosion resistance did not improve significantly. On the contrary, the PN-WC coating, prepared using a mixture of nano- and micron-sized WC particles, showed a significant increase in erosion resistance. Compared to the M-WC coating, the PN-WC coating prepared with a nano-micron mixed WC particle composition demonstrated markedly improved erosion resistance, with an erosion resistance approximately 1.5 times that of traditional coatings and 2.3 times that of the 0Cr13Ni5Mo substrate. The hard WC phase in the coating is bonded by the CoCr alloy matrix; under real turbine operating conditions—specifically, at small-angle erosion—the metal matrix exhibits poorer wear resistance compared to the hard phase. Figure 6: Volumetric Loss of Coating Erosion at 15° Angle The PN-WC coating contains both large and small WC particles, evenly distributed within the CoCr alloy matrix, as shown in Figures 3(b1) and 3(b2). When abrasive particles erode the coating at a small angle, the metal matrix is easily worn away, exposing the large hard particle phase. As the erosion continues, the CoCr alloy matrix surrounding the large particles is gradually removed, leading to the detachment of these large particles. However, since the PN-WC coating contains small WC particles distributed within the metal bonding phase surrounding the large particles, these small particles can resist the erosion of the abrasive particles, mitigating the erosion of the metal bonding phase and delaying the detachment of the large WC particles. Thus, the PN-WC coating demonstrates superior erosion resistance. The decomposition of WC particles in the FN-WC coating is the main reason for its reduced erosion resistance. In the M-WC coating, the insufficient metal bonding phase between the fragmented small tungsten carbide particles negatively impacts the coating’s erosion resistance. Figure 7 shows the volumetric loss of erosion for the FN-WC, PN-WC, and M-WC coatings at a 90° angle.As can be seen, the erosion volume loss trends of the three coatings are quite similar. The erosion resistance Re of the PN-WC and FN-WC coatings are 4.70×10⁴ g/cm³ and 4.68×10⁴ g/cm³, respectively, slightly higher than that of the M-WC coating. Under a 90° impingement angle, the erosion volume loss of all three coatings is significantly greater than that of the substrate. The study indicates that metallic materials exhibit better erosion resistance than WC coatings at a 90° impingement angle. Figure 8 shows a comparison of the erosion wear morphologies of the FN-WC, PN-WC, and M-WC coatings. The erosion wear marks on all three coatings under a 90° impingement angle are more pronounced than those observed at a 15° impingement angle. The furrow-like erosion wear marks appear coarser, confirming that the volume loss during erosion at a 90° impingement angle is more severe than at a 15° angle. At a 15° impingement angle, the erosion furrow marks on the surface of the PN-WC coating are less distinct compared to those on the FN-WC and M-WC coatings; only a few shallow furrows can be observed. Combined with the erosion resistance of the three coatings at a 15° impingement angle, the PN-WC coating, owing to its superior erosion resistance, exhibits shallower and narrower furrows on its surface. In contrast, the FN-WC and M-WC coatings have lower erosion resistance, resulting in more prominent furrow marks. Conclusion: (1) Tungsten carbide coatings with three different WC particle sizes were prepared using the HVOF process. The FN-WC, PN-WC, and M-WC coatings have comparable porosity but differ in their phase structures. The FN-WC coating shows severe decomposition of tungsten carbide, whereas the PN-WC and M-WC coatings exhibit only slight decomposition of tungsten carbide particles. (2) The PN-WC coating has a more uniform microstructure, with minimal decomposition of the WC phase, a more concentrated hardness distribution, and slightly higher bonding strength, giving it excellent overall performance. It demonstrates superior erosion resistance at a 15° impingement angle and holds great potential for application in the field of anti-abrasive damage control for hydraulic turbine flow components. (3) The size of tungsten carbide particles is an important factor influencing coating performance; by selecting powders with appropriately sized tungsten carbide particles, high-performance coatings can be produced. We have accumulated extensive experience in material, equipment, process, and solution development for coating applications, and we are currently replicating these successful cases. 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The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Properties |
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The particle size of WC in the original powder determines the size of tungsten carbide particles in the spray coating, and the particle size of tungsten carbide in the coating directly affects the performance of the sprayed coating. Nanocrystalline tungsten carbide coatings prepared using nanoscale powders exhibit higher hardness and toughness as well as superior wear resistance compared to micron-scale tungsten carbide coatings made from conventional micrometer-sized powders. Recent studies have shown that tungsten carbide coatings prepared using micro-nano composite powders outperform those made from purely nanoscale powders. However, there are currently relatively few reports on this topic. Therefore, this paper systematically investigates the microstructure and properties of supersonic flame-sprayed nanoscale, micro-nano composite, and micron-scale tungsten carbide coatings, and explores the influence of the original powder’s WC particle size on the microstructure and performance of the coatings. |
As shown by the XRD diffraction comparison (Figure 2) and the analysis results (Table 1), the WC particle size in FN-WC powder is slightly smaller, followed by that in PN-WC powder, while the WC particle size in M-WC powder is slightly larger.
Table 1: Full Width at Half Maximum of the WC Main Peak
Powder FWHM/(°)
FN-WC 0.194
PN-WC 0.157
M-WC 0.148
The substrate material is 0Cr13Ni5Mo martensitic stainless steel. Before spraying, the substrate surface was cleaned and then sandblasted. The spraying equipment used is an HVOF system manufactured by SulerMecto of the United States. During spraying, propane serves as the fuel gas, high-pressure oxygen acts as the oxidizing gas, and nitrogen is used as the powder-feeding gas. The spraying process parameters are shown in Table 2.
Table 2: Spraying Parameters
Parameters Values
Pressure (O2)/MPa 1.0
Flow rate (O2) / (L·min⁻¹) 240
Pressure (C3H8) / MPa 0.6
Flow rate (C3H8) / (L·min⁻¹) 68
Spray distance/mm 200
1.2 Coating Microstructure and Mechanical Property Testing
The microstructural analysis of the coating was performed using a FEI Quanta 400HV scanning electron microscope, and the porosity of the coating was determined according to JB/T 75059-1994. The bonding strength of the coating was tested using the tensile test method for mating parts specified in GB/T 8642-2002. The bonding strength test was conducted on a CSS-44300 electronic testing machine at an loading rate not exceeding (1,000 ± 100) N/s. The microhardness of the coating was measured using an HDX-1000TMC/LCD microhardness tester with a load of 300 g and a dwell time of 15 s. Nine measurement points were taken on each specimen, and the average value of the microhardness was calculated as the final result for the coating.
1.3 Coating Erosion and Wear Testing
The test was conducted using a particle erosion wear testing machine with a structure similar to that of the Japanese ACT-JP testing machine. The erosion test parameters were as follows: erosion distance, 100 mm; nozzle inner diameter, 3.6–4.0 mm; nozzle length, 22 mm; abrasive material, brown corundum with a particle size of 149 μm (100 mesh); compressed air pressure, 0.3 MPa; and erosion angles, 15° and 90°.
2 Results and Discussion
2.1 Microstructure of the Coating
Figure 3 shows the SEM micrographs of the cross-sections of the sprayed coatings. The porosity of the three coatings was statistically analyzed at a magnification of 5,000×. The results indicate that the porosities of the FN-WC, PN-WC, and M-WC coatings are 2.1%, 2.0%, and 2.3%, respectively, showing comparable porosity levels among the coatings. In the magnified microstructures, most of the WC particles in the FN-WC coating have diameters smaller than 100 nm, as shown in Figure 3(a2). Moreover, at the boundaries of some flattened particles, regions devoid of nano-sized WC particles can be observed, as indicated by the bright white metallic areas in Figure 3(a2). These regions likely result from partial melting of the nanoparticles in the supersonic flame jet, causing the fine nano-sized WC particles to decompose under high temperatures. In the PN-WC coating, most of the WC particles have diameters greater than 500 nm, with some even reaching around 2 μm; however, a few nano-sized particles are also present in the coating, as shown in Figure 3(b2). In the M-WC coating, the WC particles are on the micrometer scale. During spraying, larger WC particles undergo fragmentation, and this fragmented morphology is retained in the coating. After fragmentation, the metallic bonding phase between the smaller tungsten carbide particles becomes insufficient, as illustrated in Figure 3(c2).
2.2 Coating Phase Structure
Figure 4 shows the XRD analysis results for the FN-WC coating, PN-WC coating, and M-WC coating. After treatment, the FN-WC coating exhibited a slightly higher relative peak intensity for the W2C phase, indicating that the FN-WC coating underwent a greater degree of decomposition during the spraying process. This result is consistent with the findings from the microstructural analysis of the coatings. Nanoscale tungsten carbide particles tend to decompose easily in supersonic flame jets; the more of the WC in the powder particles exists as nanoparticles, the more severe the decomposition will be in the flame jet. In contrast, the WC particles in the PN-WC and M-WC coatings mostly exist in micrometer- or submicrometer-sized forms, making them less prone to decomposition. Consequently, only a small amount of the W2C phase was observed in the XRD patterns of these coatings.
2.3 Microhardness of the Coating
Coating hardness refers to a material's ability to resist deformation or fracture within a small volume on its surface; its magnitude significantly influences the coating's wear resistance and erosion resistance. Figure 5 shows the microhardness test results for three tungsten carbide coatings. The Vickers hardness values of the PN-WC and FN-WC coatings are 1,241 HV0.3 and 1,254 HV0.3, respectively, slightly higher than that of the M-WC coating, which is 1,229 HV0.3. Notably, the hardness of the PN-WC coating exhibits greater uniformity. Combined with the microstructural photographs of the three coatings shown in Figure 3, it can be observed that the FN-WC coating contains regions of pure metal resulting from the decomposition of WC particles, whereas the M-WC coating features numerous fragmented WC particles. The non-uniform microstructures in these two coatings lead to a dispersed distribution of hardness values. In contrast, the PN-WC coating has a uniform distribution of micron- and nanoscale WC particles, thus resulting in a more concentrated distribution of hardness values.
2.4 Coating Adhesion Strength
Table 3 shows the coating adhesion strengths. As can be seen, the average adhesion strength of the PN-WC coating exceeds 73.5 MPa, and during tensile testing, fracture predominantly occurs within the bonding adhesive. The average adhesion strength of the M-WC coating is comparable to that of the PN-WC coating, and both of these coatings exhibit slightly higher adhesion strengths than the FN-WC coating. This difference may be attributed to phenomena such as oxidation and decomposition of WC particles in the supersonic flame flow experienced by the all-nanometer FN-WC coating. Among the samples from the FN-WC all-nanometer coating, specimens Nos. 3 through 5 all fractured within the coating itself.
Table 3: Adhesion Strength of Coatings
Coating Bonding Strength/MPa Mean Value/MPa Fracture Position
1 2 3 4 5
FN-WC 72.3 74.8 62.6 70.4 63.2 68.7 Coating + glue
PN-WC 70.7 75.8 72.0 76.9 72.3 73.5 Glue
M-WC 73.2 69.4 77.2 76.3 68.6 72.9 Glue
2.5 Coating Erosion and Wear Performance
The erosion test was conducted by using sand particles with a mesh size corresponding to 15 seconds and 100 grams per batch. After each erosion cycle, the sample was weighed. Once the erosion process was complete, the cumulative mass loss due to erosion was used as the basis for calculating the volumetric loss caused by coating wear. This volumetric loss from wear was then adopted as the evaluation criterion for erosion resistance performance. A linear regression was performed on the cumulative volumetric loss, and the reciprocal of the slope of the fitted straight line was defined as the erosion wear coefficient Re. Under identical experimental conditions, a higher Re value indicates better erosion resistance performance of the coated material being tested.
The erosion wear results of the FN-WC coating, PN-WC coating, and M-WC coating at a small angle (15°) are shown in Figure 6. As can be seen, despite the use of all-nano WC particles, the FN-WC coating did not exhibit a significant improvement in its erosion wear resistance. In contrast, the PN-WC coating, prepared using a mixture of nano- and micro-sized WC particles, demonstrated a markedly enhanced resistance to erosion wear. Compared to the M-WC coating material, the PN-WC coating made from a mixed nano-micro WC particle composition showed a substantial improvement in erosion resistance—its erosion resistance was approximately 1.5 times that of conventional coatings and about 2.3 times that of the 0Cr13Ni5Mo substrate. In the coatings, the hard WC phase is bonded by the CoCr alloy matrix phase; however, under actual turbine operating conditions—specifically, under small-angle erosion conditions—the metal matrix phase exhibits poorer wear resistance compared to the hard WC phase.
Figure 6: Erosion Wear Volume Loss of the Coating at a 15° Angle of Attack
The PN-WC coating contains both large and small WC particles as hard phases, which are uniformly distributed within the CoCr alloy matrix, as shown in Figures 3(b1) and 3(b2). When sand particles erode the coating at a small angle, the metallic phase in the coating is easily abraded, exposing the larger hard-phase particles. As the erosion process continues, the CoCr alloy matrix surrounding the larger hard-phase particles will be eroded away, eventually leading to the detachment of these large particles. However, thanks to the smaller hard-phase particles dispersed within the metallic binder phase around the larger hard-phase particles in the PN-WC coating, the coating can better resist sand particle erosion and mitigate the erosion of the metallic binder phase, thereby delaying the detachment of the larger hard-phase particles. Consequently, the PN-WC coating exhibits superior erosion resistance. In the FN-WC coating, the degradation of WC particles is the primary factor responsible for its reduced erosion performance. In the M-WC coating, the insufficient metallic binder phase between the fragmented small tungsten carbide particles after fracture impairs the coating's erosion resistance.
Figure 7 shows the erosion wear volume loss of the FN-WC coating, PN-WC coating, and M-WC coating at a 90° impact angle. As can be seen, the trends in erosion volume loss for the three coatings are quite similar. The erosion resistance Re values of the PN-WC and FN-WC coatings are 4.70×10⁴ g/cm³ and 4.68×10⁴ g/cm³, respectively, slightly higher than that of the M-WC coating. Moreover, the erosion volume loss of all three coatings at a 90° impact angle is significantly higher than that of the substrate. The study indicates that, at a 90° impact angle, metallic materials exhibit better erosion resistance than WC coatings.
Figure 8 shows a comparison of the erosion wear morphologies of FN-WC, PN-WC, and M-WC coatings. Under a 90° impact angle, the erosion wear marks on all three coatings are more pronounced than those observed at a 15° impact angle. The erosion wear marks, which appear as plough-like grooves, are significantly coarser under the 90° impact angle, indicating that the volumetric material loss during erosion is more severe at this angle compared to the 15° impact angle. At the 15° impact angle, the erosion-induced plough-like grooves on the surface of the PN-WC coating are less distinct than those on the surfaces of the FN-WC and M-WC coatings; only a few minor grooves can be observed.
Combining the erosion resistance of the three coatings at an angle of attack of 15°, PN-WC exhibits superior erosion resistance, resulting in shallower and narrower grooves on its surface. In contrast, FN-WC and M-WC coatings have lower erosion resistance, leading to more pronounced grooves.
Conclusion
(1) Tungsten carbide coatings with three different WC particle sizes were prepared using the HVOF process. The FN-WC, PN-WC, and M-WC coatings exhibited similar porosity levels, but their phase structures differed. In the FN-WC coating, tungsten carbide showed severe decomposition, whereas in the PN-WC and M-WC coatings, only a small amount of tungsten carbide particles underwent decomposition.
(2) The PN-WC coating exhibits a more uniform microstructure, with slight decomposition of the WC phase. Its hardness distribution is more concentrated, and its bonding strength is slightly higher, resulting in excellent overall performance. At an attack angle of 15°, it demonstrates superior erosion resistance, showing promising application potential in the field of wear and corrosion protection for hydraulic turbine flow components.
(3) The particle size of tungsten carbide is an important factor influencing coating performance, and coatings with excellent performance can be prepared by selecting powders with appropriately sized tungsten carbide particles.
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The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Properties
The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Performance The size of WC particles in the original powder directly affects the microstructure and performance of tungsten carbide coatings sprayed onto a substrate. Nanocrystalline tungsten carbide coatings prepared using nanoscale powders exhibit higher hardness and toughness, as well as superior wear resistance, compared to micron-sized tungsten carbide coatings made from conventional micrometer-scale powders. Recent studies have shown that tungsten carbide coatings prepared using micro-nano composite powders outperform those made from purely nanoscale powders. However, there are currently relatively few reports on this topic. Therefore, this paper systematically investigates the microstructure and performance of supersonic flame-sprayed nanoscale, micro-nano composite, and micron-sized tungsten carbide coatings, exploring the impact of the original powder’s WC particle size on coating microstructure and performance. 1 Experimental Setup 1.1 Preparation of Tungsten Carbide Coatings Three types of WC-CoCr powders—FN-WC, PN-WC, and M-WC—with nano-, nano-micron mixed, and micron-sized WC particles were used as spray powders. In the FN-WC powder, aggregated nanoscale WC particles form micron- or submicron-sized agglomerates, which are then bonded together by a binder, as shown in Figures 1(a) and 1(b). The average particle size of these agglomerates ranges from 18.85 to 37.56 μm, with a loose bulk density of 5.48 g/cm³. The morphology of the PN-WC powder is illustrated in Figures 1(c) and 1(d); its cross-sectional microstructure reveals some free nanoscale particles along with predominantly submicron- or micron-sized particles. The average particle size of the PN-WC powder is 23.33–44.79 μm, with a loose bulk density of 5.6 g/cm³. The morphology of the M-WC powder is shown in Figures 1(e) and 1(f); the WC particles in the powder end-face microstructure range from 0.5 to 3 μm in diameter, with an average particle size of 21–50 μm and a loose bulk density of 5.0 g/cm³. XRD diffraction comparisons (Figure 2) and analysis results (Table 1) indicate that the WC particle size in the FN-WC powder is slightly smaller, followed by the PN-WC powder, while the M-WC powder has slightly larger WC particles. Table 1: Half-Width at Half-Maximum of Main WC Peaks Powder FWHM/(°) FN-WC 0.194 PN-WC 0.157 M-WC 0.148 The substrate used was 0Cr13Ni5Mo martensitic stainless steel. Before spraying, the substrate surface was cleaned and sandblasted. The spraying equipment was an HVOF system manufactured by SulerMecto in the United States. Propane was used as the fuel gas, high-pressure oxygen as the oxidizer, and nitrogen as the powder feed gas during spraying. The spraying process parameters are listed in Table 2. Table 2: Spraying Parameters Parameters Values Pressure (O₂)/MPa 1.0 Flow rate (O₂)/(L·min⁻¹) 240 Pressure (C₃H₈)/MPa 0.6 Flow rate (C₃H₈)/(L·min⁻¹) 68 Spray distance/mm 200 1.2 Microstructural and Mechanical Property Testing The microstructure of the coatings was analyzed using a FeiQuata400HV scanning electron microscope. Coating porosity was determined according to JB/T75059-1994. The bond strength of the coatings was tested using the paired specimen tensile test method specified in GB/T8642-2002. The bond strength tests were conducted on a CSS-44300 electronic testing machine at a loading rate not exceeding (1000 ± 100) N/s. The microhardness of the coatings was measured using an HDX-1000TMC/LCD microhardness tester under a load of 300 g for 15 seconds; nine points were tested per sample, and the average microhardness value of each coating was calculated. 1.3 Abrasive Wear Testing The abrasive wear tests were performed using a particle erosion wear testing machine similar in structure to the ACT-JP testing machine from Japan. The erosion test parameters were as follows: erosion distance 100 mm, nozzle inner diameter 3.6–4.0 mm, nozzle length 22 mm, abrasive material brown corundum with a particle size of 149 μm (100 mesh), compressed air pressure 0.3 MPa, and erosion angles of 15° and 90°. 2 Results and Discussion 2.1 Microstructure of the Coatings Figure 3 shows the SEM images of the cross-sections of the sprayed coatings. The porosity of the three coatings was statistically analyzed at 5000x magnification. The results show that the porosities of the FN-WC, PN-WC, and M-WC coatings were 2.1%, 2.0%, and 2.3%, respectively, indicating comparable porosity levels among the coatings. At higher magnifications, most of the WC particles in the FN-WC coating had diameters less than 100 nm, as shown in Figure 3(a2). Additionally, some flat particle boundaries showed no presence of nanoscale WC particles, as seen in the bright white metallic regions in Figure 3(a2). These regions likely resulted from partial melting of the nanoparticles in the supersonic flame jet, causing the small nanoscale WC particles to decompose at high temperatures. In the PN-WC coating, most of the WC particles had diameters greater than 500 nm, even reaching around 2 μm; however, some nanoscale particles were also present in the coating, as shown in Figure 3(b2). In the M-WC coating, the WC particles were micron-sized, and large WC particles broke during the spraying process, retaining their fractured morphology within the coating. The metal bonding phase between the fragmented tungsten carbide particles was insufficient, as shown in Figure 3(c2). 2.2 Phase Structure of the Coatings Figure 4 shows the XRD analysis results for the FN-WC, PN-WC, and M-WC coatings. After processing, the FN-WC coating exhibited a slightly higher relative peak intensity for the W₂C phase, indicating a higher degree of decomposition during spraying. This result is consistent with the microstructural analysis. Nanoscale tungsten carbide particles tend to decompose easily in the supersonic flame jet; when most of the WC particles in the powder exist as nanoparticles, their decomposition becomes more severe. In the PN-WC and M-WC coatings, most of the WC particles were micron- or submicron-sized and did not easily decompose, resulting in only minor traces of the W₂C phase observed in the XRD patterns. 2.3 Microhardness of the Coatings Coating hardness refers to the material's ability to resist deformation or fracture within a small volume on the surface, and its magnitude significantly influences the coating's wear resistance and erosion resistance. Figure 5 shows the microhardness test results for the three tungsten carbide coatings. The Vickers hardness values of the PN-WC and FN-WC coatings were 1241 HV0.3 and 1254 HV0.3, respectively, slightly higher than the M-WC coating’s hardness of 1229 HV0.3. The hardness of the PN-WC coating was more concentrated. Combined with the microstructural photographs of the three coatings shown in Figure 3, it can be seen that the FN-WC coating contains pure metal areas resulting from the decomposition of WC particles, whereas the M-WC coating has many fragmented WC particles. The uneven microstructures of these two coatings led to dispersed hardness values, while the PN-WC coating had uniformly distributed micron-nano WC particles, resulting in a more concentrated distribution of hardness values. 2.4 Bond Strength of the Coatings Table 3 shows the bond strength of the coatings. The average bond strength of the PN-WC coating was over 73.5 MPa, and the primary fracture during the tensile test occurred within the adhesive layer. The average bond strength of the M-WC coating was comparable to that of the PN-WC coating, and both of these coatings had slightly higher bond strengths than the FN-WC coating. This may be related to oxidation and WC particle decomposition phenomena occurring in the FN-WC all-nanoscale coating during the supersonic flame jet. In the FN-WC all-nanoscale coating, samples 3–5 all fractured within the coating. Table 3: Bond Strength of the Coatings Coating Bonding Strength/MPa Mean Value/MPa Fracture Position 1 2 3 4 5 FN-WC 72.3 74.8 62.6 70.4 63.2 68.7 Coating + Glue PN-WC 70.7 75.8 72.0 76.9 72.3 73.5 Glue M-WC 73.2 69.4 77.2 76.3 68.6 72.9 Glue 2.5 Erosion Resistance Performance The erosion tests were conducted by subjecting the coatings to abrasive particles corresponding to 100 g every 15 seconds, weighing the coatings after each test cycle. After the erosion tests, the cumulative mass loss due to erosion was calculated and converted into volumetric loss caused by coating erosion, using this volumetric loss as a criterion for evaluating erosion resistance. A linear fit was applied to the cumulative volumetric loss data, and the reciprocal of the slope of the fitted line was defined as the erosion resistance coefficient Re. Under the same test conditions, a higher Re value indicates better erosion resistance of the coated material. The erosion resistance results for the FN-WC, PN-WC, and M-WC coatings at a small angle (15°) are shown in Figure 6. Although the FN-WC coating used all-nanoscale WC particles, its erosion resistance did not improve significantly. On the contrary, the PN-WC coating, prepared using a mixture of nano- and micron-sized WC particles, showed a significant increase in erosion resistance. Compared to the M-WC coating, the PN-WC coating prepared with a nano-micron mixed WC particle composition demonstrated markedly improved erosion resistance, with an erosion resistance approximately 1.5 times that of traditional coatings and 2.3 times that of the 0Cr13Ni5Mo substrate. The hard WC phase in the coating is bonded by the CoCr alloy matrix; under real turbine operating conditions—specifically, at small-angle erosion—the metal matrix exhibits poorer wear resistance compared to the hard phase. Figure 6: Volumetric Loss of Coating Erosion at 15° Angle The PN-WC coating contains both large and small WC particles, evenly distributed within the CoCr alloy matrix, as shown in Figures 3(b1) and 3(b2). When abrasive particles erode the coating at a small angle, the metal matrix is easily worn away, exposing the large hard particle phase. As the erosion continues, the CoCr alloy matrix surrounding the large particles is gradually removed, leading to the detachment of these large particles. However, since the PN-WC coating contains small WC particles distributed within the metal bonding phase surrounding the large particles, these small particles can resist the erosion of the abrasive particles, mitigating the erosion of the metal bonding phase and delaying the detachment of the large WC particles. Thus, the PN-WC coating demonstrates superior erosion resistance. The decomposition of WC particles in the FN-WC coating is the main reason for its reduced erosion resistance. In the M-WC coating, the insufficient metal bonding phase between the fragmented small tungsten carbide particles negatively impacts the coating’s erosion resistance. Figure 7 shows the volumetric loss of erosion for the FN-WC, PN-WC, and M-WC coatings at a 90° angle.As can be seen, the erosion volume loss trends of the three coatings are quite similar. The erosion resistance Re of the PN-WC and FN-WC coatings are 4.70×10⁴ g/cm³ and 4.68×10⁴ g/cm³, respectively, slightly higher than that of the M-WC coating. Under a 90° impingement angle, the erosion volume loss of all three coatings is significantly greater than that of the substrate. The study indicates that metallic materials exhibit better erosion resistance than WC coatings at a 90° impingement angle. Figure 8 shows a comparison of the erosion wear morphologies of the FN-WC, PN-WC, and M-WC coatings. The erosion wear marks on all three coatings under a 90° impingement angle are more pronounced than those observed at a 15° impingement angle. The furrow-like erosion wear marks appear coarser, confirming that the volume loss during erosion at a 90° impingement angle is more severe than at a 15° angle. At a 15° impingement angle, the erosion furrow marks on the surface of the PN-WC coating are less distinct compared to those on the FN-WC and M-WC coatings; only a few shallow furrows can be observed. Combined with the erosion resistance of the three coatings at a 15° impingement angle, the PN-WC coating, owing to its superior erosion resistance, exhibits shallower and narrower furrows on its surface. In contrast, the FN-WC and M-WC coatings have lower erosion resistance, resulting in more prominent furrow marks. Conclusion: (1) Tungsten carbide coatings with three different WC particle sizes were prepared using the HVOF process. The FN-WC, PN-WC, and M-WC coatings have comparable porosity but differ in their phase structures. The FN-WC coating shows severe decomposition of tungsten carbide, whereas the PN-WC and M-WC coatings exhibit only slight decomposition of tungsten carbide particles. (2) The PN-WC coating has a more uniform microstructure, with minimal decomposition of the WC phase, a more concentrated hardness distribution, and slightly higher bonding strength, giving it excellent overall performance. It demonstrates superior erosion resistance at a 15° impingement angle and holds great potential for application in the field of anti-abrasive damage control for hydraulic turbine flow components. (3) The size of tungsten carbide particles is an important factor influencing coating performance; by selecting powders with appropriately sized tungsten carbide particles, high-performance coatings can be produced. We have accumulated extensive experience in material, equipment, process, and solution development for coating applications, and we are currently replicating these successful cases. 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wc
pn-wc
fn-wc
m-wc
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Product Description
The Influence of Tungsten Carbide Spray Particle Size on Coating Microstructure and Properties |
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The particle size of WC in the original powder determines the size of tungsten carbide particles in the spray coating, and the particle size of tungsten carbide in the coating directly affects the performance of the sprayed coating. Nanocrystalline tungsten carbide coatings prepared using nanoscale powders exhibit higher hardness and toughness as well as superior wear resistance compared to micron-scale tungsten carbide coatings made from conventional micrometer-sized powders. Recent studies have shown that tungsten carbide coatings prepared using micro-nano composite powders outperform those made from purely nanoscale powders. However, there are currently relatively few reports on this topic. Therefore, this paper systematically investigates the microstructure and properties of supersonic flame-sprayed nanoscale, micro-nano composite, and micron-scale tungsten carbide coatings, and explores the influence of the original powder’s WC particle size on the microstructure and performance of the coatings. |
As shown by the XRD diffraction comparison (Figure 2) and the analysis results (Table 1), the WC particle size in FN-WC powder is slightly smaller, followed by that in PN-WC powder, while the WC particle size in M-WC powder is slightly larger.
Table 1: Full Width at Half Maximum of the WC Main Peak
Powder FWHM/(°)
FN-WC 0.194
PN-WC 0.157
M-WC 0.148
The substrate material is 0Cr13Ni5Mo martensitic stainless steel. Before spraying, the substrate surface was cleaned and then sandblasted. The spraying equipment used is an HVOF system manufactured by SulerMecto of the United States. During spraying, propane serves as the fuel gas, high-pressure oxygen acts as the oxidizing gas, and nitrogen is used as the powder-feeding gas. The spraying process parameters are shown in Table 2.
Table 2: Spraying Parameters
Parameters Values
Pressure (O2)/MPa 1.0
Flow rate (O2) / (L·min⁻¹) 240
Pressure (C3H8) / MPa 0.6
Flow rate (C3H8) / (L·min⁻¹) 68
Spray distance/mm 200
1.2 Coating Microstructure and Mechanical Property Testing
The microstructural analysis of the coating was performed using a FEI Quanta 400HV scanning electron microscope, and the porosity of the coating was determined according to JB/T 75059-1994. The bonding strength of the coating was tested using the tensile test method for mating parts specified in GB/T 8642-2002. The bonding strength test was conducted on a CSS-44300 electronic testing machine at an loading rate not exceeding (1,000 ± 100) N/s. The microhardness of the coating was measured using an HDX-1000TMC/LCD microhardness tester with a load of 300 g and a dwell time of 15 s. Nine measurement points were taken on each specimen, and the average value of the microhardness was calculated as the final result for the coating.
1.3 Coating Erosion and Wear Testing
The test was conducted using a particle erosion wear testing machine with a structure similar to that of the Japanese ACT-JP testing machine. The erosion test parameters were as follows: erosion distance, 100 mm; nozzle inner diameter, 3.6–4.0 mm; nozzle length, 22 mm; abrasive material, brown corundum with a particle size of 149 μm (100 mesh); compressed air pressure, 0.3 MPa; and erosion angles, 15° and 90°.
2 Results and Discussion
2.1 Microstructure of the Coating
Figure 3 shows the SEM micrographs of the cross-sections of the sprayed coatings. The porosity of the three coatings was statistically analyzed at a magnification of 5,000×. The results indicate that the porosities of the FN-WC, PN-WC, and M-WC coatings are 2.1%, 2.0%, and 2.3%, respectively, showing comparable porosity levels among the coatings. In the magnified microstructures, most of the WC particles in the FN-WC coating have diameters smaller than 100 nm, as shown in Figure 3(a2). Moreover, at the boundaries of some flattened particles, regions devoid of nano-sized WC particles can be observed, as indicated by the bright white metallic areas in Figure 3(a2). These regions likely result from partial melting of the nanoparticles in the supersonic flame jet, causing the fine nano-sized WC particles to decompose under high temperatures. In the PN-WC coating, most of the WC particles have diameters greater than 500 nm, with some even reaching around 2 μm; however, a few nano-sized particles are also present in the coating, as shown in Figure 3(b2). In the M-WC coating, the WC particles are on the micrometer scale. During spraying, larger WC particles undergo fragmentation, and this fragmented morphology is retained in the coating. After fragmentation, the metallic bonding phase between the smaller tungsten carbide particles becomes insufficient, as illustrated in Figure 3(c2).
2.2 Coating Phase Structure
Figure 4 shows the XRD analysis results for the FN-WC coating, PN-WC coating, and M-WC coating. After treatment, the FN-WC coating exhibited a slightly higher relative peak intensity for the W2C phase, indicating that the FN-WC coating underwent a greater degree of decomposition during the spraying process. This result is consistent with the findings from the microstructural analysis of the coatings. Nanoscale tungsten carbide particles tend to decompose easily in supersonic flame jets; the more of the WC in the powder particles exists as nanoparticles, the more severe the decomposition will be in the flame jet. In contrast, the WC particles in the PN-WC and M-WC coatings mostly exist in micrometer- or submicrometer-sized forms, making them less prone to decomposition. Consequently, only a small amount of the W2C phase was observed in the XRD patterns of these coatings.
2.3 Microhardness of the Coating
Coating hardness refers to a material's ability to resist deformation or fracture within a small volume on its surface; its magnitude significantly influences the coating's wear resistance and erosion resistance. Figure 5 shows the microhardness test results for three tungsten carbide coatings. The Vickers hardness values of the PN-WC and FN-WC coatings are 1,241 HV0.3 and 1,254 HV0.3, respectively, slightly higher than that of the M-WC coating, which is 1,229 HV0.3. Notably, the hardness of the PN-WC coating exhibits greater uniformity. Combined with the microstructural photographs of the three coatings shown in Figure 3, it can be observed that the FN-WC coating contains regions of pure metal resulting from the decomposition of WC particles, whereas the M-WC coating features numerous fragmented WC particles. The non-uniform microstructures in these two coatings lead to a dispersed distribution of hardness values. In contrast, the PN-WC coating has a uniform distribution of micron- and nanoscale WC particles, thus resulting in a more concentrated distribution of hardness values.
2.4 Coating Adhesion Strength
Table 3 shows the coating adhesion strengths. As can be seen, the average adhesion strength of the PN-WC coating exceeds 73.5 MPa, and during tensile testing, fracture predominantly occurs within the bonding adhesive. The average adhesion strength of the M-WC coating is comparable to that of the PN-WC coating, and both of these coatings exhibit slightly higher adhesion strengths than the FN-WC coating. This difference may be attributed to phenomena such as oxidation and decomposition of WC particles in the supersonic flame flow experienced by the all-nanometer FN-WC coating. Among the samples from the FN-WC all-nanometer coating, specimens Nos. 3 through 5 all fractured within the coating itself.
Table 3: Adhesion Strength of Coatings
Coating Bonding Strength/MPa Mean Value/MPa Fracture Position
1 2 3 4 5
FN-WC 72.3 74.8 62.6 70.4 63.2 68.7 Coating + glue
PN-WC 70.7 75.8 72.0 76.9 72.3 73.5 Glue
M-WC 73.2 69.4 77.2 76.3 68.6 72.9 Glue
2.5 Coating Erosion and Wear Performance
The erosion test was conducted by using sand particles with a mesh size corresponding to 15 seconds and 100 grams per batch. After each erosion cycle, the sample was weighed. Once the erosion process was complete, the cumulative mass loss due to erosion was used as the basis for calculating the volumetric loss caused by coating wear. This volumetric loss from wear was then adopted as the evaluation criterion for erosion resistance performance. A linear regression was performed on the cumulative volumetric loss, and the reciprocal of the slope of the fitted straight line was defined as the erosion wear coefficient Re. Under identical experimental conditions, a higher Re value indicates better erosion resistance performance of the coated material being tested.
The erosion wear results of the FN-WC coating, PN-WC coating, and M-WC coating at a small angle (15°) are shown in Figure 6. As can be seen, despite the use of all-nano WC particles, the FN-WC coating did not exhibit a significant improvement in its erosion wear resistance. In contrast, the PN-WC coating, prepared using a mixture of nano- and micro-sized WC particles, demonstrated a markedly enhanced resistance to erosion wear. Compared to the M-WC coating material, the PN-WC coating made from a mixed nano-micro WC particle composition showed a substantial improvement in erosion resistance—its erosion resistance was approximately 1.5 times that of conventional coatings and about 2.3 times that of the 0Cr13Ni5Mo substrate. In the coatings, the hard WC phase is bonded by the CoCr alloy matrix phase; however, under actual turbine operating conditions—specifically, under small-angle erosion conditions—the metal matrix phase exhibits poorer wear resistance compared to the hard WC phase.
Figure 6: Erosion Wear Volume Loss of the Coating at a 15° Angle of Attack
The PN-WC coating contains both large and small WC particles as hard phases, which are uniformly distributed within the CoCr alloy matrix, as shown in Figures 3(b1) and 3(b2). When sand particles erode the coating at a small angle, the metallic phase in the coating is easily abraded, exposing the larger hard-phase particles. As the erosion process continues, the CoCr alloy matrix surrounding the larger hard-phase particles will be eroded away, eventually leading to the detachment of these large particles. However, thanks to the smaller hard-phase particles dispersed within the metallic binder phase around the larger hard-phase particles in the PN-WC coating, the coating can better resist sand particle erosion and mitigate the erosion of the metallic binder phase, thereby delaying the detachment of the larger hard-phase particles. Consequently, the PN-WC coating exhibits superior erosion resistance. In the FN-WC coating, the degradation of WC particles is the primary factor responsible for its reduced erosion performance. In the M-WC coating, the insufficient metallic binder phase between the fragmented small tungsten carbide particles after fracture impairs the coating's erosion resistance.
Figure 7 shows the erosion wear volume loss of the FN-WC coating, PN-WC coating, and M-WC coating at a 90° impact angle. As can be seen, the trends in erosion volume loss for the three coatings are quite similar. The erosion resistance Re values of the PN-WC and FN-WC coatings are 4.70×10⁴ g/cm³ and 4.68×10⁴ g/cm³, respectively, slightly higher than that of the M-WC coating. Moreover, the erosion volume loss of all three coatings at a 90° impact angle is significantly higher than that of the substrate. The study indicates that, at a 90° impact angle, metallic materials exhibit better erosion resistance than WC coatings.
Figure 8 shows a comparison of the erosion wear morphologies of FN-WC, PN-WC, and M-WC coatings. Under a 90° impact angle, the erosion wear marks on all three coatings are more pronounced than those observed at a 15° impact angle. The erosion wear marks, which appear as plough-like grooves, are significantly coarser under the 90° impact angle, indicating that the volumetric material loss during erosion is more severe at this angle compared to the 15° impact angle. At the 15° impact angle, the erosion-induced plough-like grooves on the surface of the PN-WC coating are less distinct than those on the surfaces of the FN-WC and M-WC coatings; only a few minor grooves can be observed.
Combining the erosion resistance of the three coatings at an angle of attack of 15°, PN-WC exhibits superior erosion resistance, resulting in shallower and narrower grooves on its surface. In contrast, FN-WC and M-WC coatings have lower erosion resistance, leading to more pronounced grooves.
Conclusion
(1) Tungsten carbide coatings with three different WC particle sizes were prepared using the HVOF process. The FN-WC, PN-WC, and M-WC coatings exhibited similar porosity levels, but their phase structures differed. In the FN-WC coating, tungsten carbide showed severe decomposition, whereas in the PN-WC and M-WC coatings, only a small amount of tungsten carbide particles underwent decomposition.
(2) The PN-WC coating exhibits a more uniform microstructure, with slight decomposition of the WC phase. Its hardness distribution is more concentrated, and its bonding strength is slightly higher, resulting in excellent overall performance. At an attack angle of 15°, it demonstrates superior erosion resistance, showing promising application potential in the field of wear and corrosion protection for hydraulic turbine flow components.
(3) The particle size of tungsten carbide is an important factor influencing coating performance, and coatings with excellent performance can be prepared by selecting powders with appropriately sized tungsten carbide particles.
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