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Journal of Thermal Spray Technology

, Volume 27, Issue 8, pp 1652–1663 | Cite as

Microstructure, Mechanical Properties and Dry Sliding Wear Behavior of Cu-Al2O3-Graphite Solid-Lubricating Coatings Deposited by Low-Pressure Cold Spraying

  • Wenyuan Chen
  • Yuan YuEmail author
  • Jun Cheng
  • Shuai Wang
  • Shengyu Zhu
  • Weimin Liu
  • Jun YangEmail author
Peer Reviewed
  • 193 Downloads

Abstract

In this study, Cu-Al2O3-graphite solid-lubricating coatings were deposited on the 304 stainless steel substrate by low-pressure cold spray technique. The influences of Cu-coated graphite content on the microstructure, mechanical properties and dry sliding wear behavior of the Cu-based solid-lubricating coatings were investigated. The results showed that the mixture addition of Al2O3 and Cu-coated graphite is an effective strategy to improve the solid lubricity of Cu-based coatings while simultaneously retaining favorable mechanical properties and bonding strength. When the Cu-coated graphite content increased from 0 to 20 wt.% in the spray powder, the Brinell hardness and the interface bonding strength of the Cu-based coatings declined, but the solid-lubricating property improved obviously. The Cu-based solid-lubricating coating with 10 wt.% Al2O3 and 10 wt.% Cu-coated graphite exhibited the lowest friction coefficient of 0.29, which was attributed to the formation of a lubricating tribo-layer and the reduction in cracks on the worn subsurface. Additionally, the wear mechanism changed from adhesive wear to abrasive wear and delamination with the increase in graphite content.

Keywords

Cu-based coating graphite low-pressure cold spray solid lubrication 

Introduction

Copper alloys and coatings thereof are important solid-lubricating materials in many moving mechanical assemblies such as bearings and gears (Ref 1, 2). It is reported that the deposition methods usually have a great influence on the composition, microstructure and properties of Cu-based solid-lubricating coatings (Ref 3, 4). Compared to the conventional thermal spraying technology, low-pressure cold spraying (LPCS) is an emerging coating deposition method with unique advantages. It is based on the principle of gas dynamics, where the micron-sized feedstock powders are accelerated through a De Laval nozzle by the compressed (0.3-1.0 MPa) and preheated (25-650 °C) gas, impacting the substrate and then forming the coating by plastic deformation (Ref 5-9). Thus, this technique inflicts low-temperature spraying and little thermal damage to the substrates, especially for the readily oxidized, heat-sensitive materials and polymers (Ref 10-13). In view of these advantages, LPCS is a feasible deposition approach to prepare ductile metal-based coatings, especially for the common metal copper (Ref 14-21).

In general, hard ceramic reinforcements (Al2O3, WC, etc.) mixed with ductile metals (Cu, Al, Zn, Ni, etc.) can be used as feedstock powders for LPCS, improving the degree of plastic deformation and bringing good properties such as high strength, low porosity and compressive residual stress (Ref 22-24). In recent years, much attention is paid to improving the mechanical properties and wear resistance of LPCS Cu-based coatings by adding various hard particles (Ref 5, 11, 22). The LPCS Cu-based composite coating with addition of Al2O3 has higher strength and density compared to that without Al2O3 additive (Ref 7, 24). In addition, the tribological behavior of the Cu-based coating is also improved by adding Al2O3 reinforcement (Ref 25). Nevertheless, a shortcoming of the Cu-based coatings with addition of hard ceramic reinforcement is that the friction coefficient (0.4-0.5) is relatively high. Thus, it is essential to add solid lubricant in the coating to obtain good solid lubricity, thereby decreasing the frictional energy loss effectively.

It is well known that solid lubricants (graphite, MoS2 and WS2, etc.) can reduce obviously the friction coefficient of Cu-based coatings. For instance, a cold-sprayed Cu-MoS2 composite coating exhibits desirable solid lubricity (Ref 26, 27). However, the solid lubricant added into Cu matrix diminishes the mechanical properties and interface bonding.

To solve the incompatibility problem of tribological properties and mechanical properties for the LPCS Cu-based coating, it may be a promising and feasible approach to add the solid lubricant and hard reinforcement simultaneously into the Cu matrix. To the best of our knowledge, there are few studies focused on the improvement in the mechanical properties, solid lubricity and wear resistance of LPCS Cu-based coatings simultaneously (Ref 16, 19, 28, 29).

In this work, Cu-coated graphite as the solid lubricant was added into Cu-10 wt.% Al2O3 spray powder to prepare Cu-Al2O3-graphite solid-lubricating coatings. It should be noted that Cu-coated graphite is selected as solid lubricant due to its good interface with copper compared to the uncoated one (Ref 30, 31). The influences of Cu-coated graphite contents on the microstructure, mechanical properties and dry sliding wear behavior of Cu-Al2O3-graphite solid-lubricating coatings were investigated. Meanwhile, the wear mechanisms of all LPCS Cu-based solid-lubricating coatings were discussed.

Experimental Procedures

The commercially available powders of electrolytic copper (BGRIMM Advanced Materials Science & technology Co., Ltd, Beijing, China), Al2O3 (Zhengzhou liangyan new material Co., Ltd, Zhengzhou, China) and Cu-coated graphite (50 wt.% graphite, Jiande hengxin copper material Co., Ltd, Hangzhou, China) were selected as the feedstock powders. The morphologies and size distributions of spray powders were characterized by a scanning electron microscope (SEM, JSM-5600LV) and a laser diffraction sizer (Bettersize 2000LD, Bettersize Instrument Ltd., China), respectively. The morphologies and size distribution curves of spray powders are shown in Fig. 1. The electrolytic copper particles exhibit a dendritic structure, and their average particle size (D50) is 20.18 μm. The Al2O3 and Cu-coated graphite particles reveal angular and sheet structures, and their average particles sizes (D50) are 4.41 μm and 47.77 μm, respectively.
Fig. 1

SEM images showing the morphologies of (a) Cu, (c) Al2O3 and (e) Cu-coated graphite particles and the corresponding size distribution curves (b), (d) and (f)

Pure Cu, Cu-10 wt.% Al2O3 and Cu-10 wt.% Al2O3-Cu-coated graphite powders were selected and mechanically blended as the spray powders. The coatings were prepared on the 304 stainless steel plates (Φ 25 × 4 mm) by the DYMET 423 equipment (Obninsk Center for Powder Spraying, Obninsk, Russia). According to the different contents of Cu-coated graphite (0, 5, 10, 20 wt.%) in Cu (90, 85, 80, 70 wt.%)-10 wt.% Al2O3 feedstock powders, the coatings were denoted by the CA, CAC5, CAC10, CAC20 and the pure copper coating was denoted by the letter C. Compressed air was used as the working gas during the spraying process. The spraying gun was controlled by a three-dimensional USB CNC manipulator, and the 304 stainless steel substrate was 45° grit-blasted (Al2O3 grits, ~ 100 mesh) prior to spraying. A commercial round (Φ 6 mm) tubular nozzle was used in this experiment. The spraying parameters for the different coatings are provided in Table 1.
Table 1

Spraying parameters of LPCS coatings

Sample

Number of layers

Powder feed rate, g/min

Gas pressure, MPa

Gas preheating temperature, °C

Linear speed, mm/s

Spray distance, mm

Adjacent beam distance, mm

C

3

16

0.80

500

30

10

1

CA

3

16

0.80

500

30

10

1

CAC5

3

14

0.80

500

30

10

1

CAC10

3

17

0.80

500

30

10

1

CAC20

4

14

0.80

500

30

10

1

The thicknesses of coatings were measured, and the cross sections were etched with an etching solution of 5 g FeCl3, 10 mL HCl and 100 mL H2O. The cross-sectional microstructures of the LPCS Cu-based coatings with and without etching treatment were observed by SEM. The contents of Al2O3 and graphite inside the LPCS Cu-based solid-lubricating coatings were measured by an image analysis software (Image J). Ten random backscattered electron images (500 ×) of polished cross sections were measured by the pixel count in the software to calculate the volume fractions of Al2O3 and graphite in the coatings. The density values of Cu (8.93 g/cm3), Al2O3 (3.99 g/cm3) and graphite (2.27 g/cm3) were employed for the conversion of the volume fraction into their respective weight fraction.

The average Brinell hardness values were calculated after ten measurements by a HBS-62.5 small load Brinell hardness tester (Laizhou huayin test instruments Co., Ltd, Laizhou, China) with a 2.5 mm sintered carbide ball indenter and 62.5 kgf load for 30 s in this experiment. Bonding strength was measured according to the ASTM C633-13 standard by a tensile pull tester (WDW-200 universal material testing machine, Shenzhen, China). Each specimen was attached on the component by the commercial epoxy resin E-7 glue (Shanghai Huayi Resins Co., Ltd, Shanghai, China). Three measurements were carried out for each coating, and the fracture surfaces were analyzed by the SEM images and EDS (energy dispersive spectroscopy) maps.

Dry sliding wear behavior of the LPCS Cu-based solid-lubricating coatings was tested on a HT-1000 ball-on-disk tribo-meter (Zhong Ke Kai Hua Corporation, Lanzhou, China) at room temperature (about 25 °C). Before the test, the coatings were ground with 600, 1000 and 1500 grits SiC abrasive papers, and then polished by 0.1 µm colloidal silica. After polishing, all the coatings were ultrasonically cleaned with ethanol. Moreover, the Ra values of all coatings were tested by the Micro-XAM-800 (KLA-Tencor, USA) surface profiler and the values fell between 0.07 and 0.2 µm.

The 304 stainless steel ball (Φ 6 mm) was used as the counterpart. The applied load was 5 N, and the wear scar diameter was 10 mm. The rotating speed was 360 rpm, and the duration time was 60 min. After the dry sliding wear test, the wear volumes were measured by the Alpha Step D-100 (KLA-Tencor, USA) instrument, and three measurements were carried out to calculate the average values. The value of wear rate (Wr) was calculated by using the equation: Wr = V/(F·L), where V is the wear volume, F is the normal load and L is the sliding distance. The surface and cross-sectional morphologies of the wear scars of coatings were examined by SEM and EDS. Meanwhile, the 3D surface morphologies of wear scars on the steel balls were determined by the Micro-XAM-800 surface profiler.

Results and Discussion

Microstructure of the LPCS Cu-Based Solid-Lubricating Coatings

In view of the different effects of Al2O3 and Cu-coated graphite on the coating microstructure, Fig. 2 shows the cross-sectional micrographs of the LPCS Cu-based solid-lubricating coatings. It is found in Fig. 2(a) and (b) that the pure copper coating (C) has a dense microstructure with little pores (black dots) and a thickness of 365 ± 16 µm (average thickness of one layer is about 122 µm). Meanwhile, the deformation of the copper particles boundaries can be observed in Fig. 2(b). The addition of 10 wt.% Al2O3 can significantly eliminate the porosity and particle boundaries of the copper coating. Furthermore, the result indicates that the mixed spray powders are readily deposited on the steel surface, which is demonstrated by the thickness (859 ± 37 µm) of the CA coating (average thickness of one layer is about 286 µm) (Fig. 2c and d). This may be attributed to the mechanical hammering effect of the Al2O3 particles, which can improve the powder deposition efficiency and eliminate the porosity of pure copper coating during the spraying process (Ref 16). Additionally, when the Cu-coated graphite solid-lubricating powder is added into the Cu-10 wt.% Al2O3 spray powder, the density of CAC coatings is still high. However, the coatings become thin, their thickness values being 480 ± 11 µm, 400 ± 38 µm and 562 ± 45 µm for CAC5, CAC10 and CAC20 (average thickness of one layer is about 160 µm, 133 µm and 140 µm), respectively. It is inferred that the addition of the Cu-coated graphite powder decreases the copper particle deposition efficiency during the spraying process.
Fig. 2

SEM images showing the cross-sectional microstructures of (a) and (b) C, (c) and (d) CA, (e) and (f) CAC10 coatings

To investigate the distribution of Al2O3 and Cu-coated graphite in CAC10 coating, the cross-sectional morphology and the corresponding element distribution maps are evaluated. It is seen in Fig. 3 that Al2O3 and Cu-coated graphite particles distribute randomly in the copper matrix.
Fig. 3

SEM image and EDS maps of the cross section of the LPCS CAC10 solid-lubricating coating

Additionally, Fig. 4 shows the weight fractions of graphite and Al2O3 deposited in the LPCS Cu-based solid-lubricating coatings. It can be clearly observed that the content of graphite in the coatings increases from 0.07 to 0.20 wt.% with increasing weight ratio of Cu-coated graphite (5-20 wt.%) powder in the feedstock. It is found that the actual content of graphite in the coating is much lower than that in the spray powder. Moreover, the actual content of Al2O3 in the coatings is also lower than that in the spray powder when adding the Cu-coated graphite. Additionally, when the content of graphite increases in the coating, the weight fraction of Al2O3 declines from 0.92 to 0.55 wt.% firstly and then increases from 0.67 to 0.76 wt.%. This means that the addition of Cu-coated graphite powder has a great influence on the deposition efficiency of Al2O3 in the coating. When the same content of Al2O3 particles (10 wt.%) is added into the spray powder, its actual content in the coating increases with the graphite content.
Fig. 4

Weight fractions of graphite and Al2O3 deposited in the LPCS Cu-based solid-lubricating coatings

The etched cross-sectional microstructure of the LPCS Cu-based solid-lubricating coatings is shown in Fig. 5. Obviously, the copper particle morphology transforms from the original dendritic structure into the stacked and needlelike structure, while Al2O3 (white dots) and Cu-coated graphite (black areas) distribute randomly in the form of irregular particles. Specifically, the needlelike copper lamellas undergo plastic deformation to stack together. Clear boundaries are observed in the pure copper coating (Fig. 5a). The cross-sectional microstructure of CA coating (Fig. 5b) shows that the needlelike copper lamellas around Al2O3 particles are refined, suggesting that the addition of hard Al2O3 particles is beneficial to prepare compact LPCS Cu-based coating. Al2O3 can also increase the interface bonding due to its mechanical hammering effect (Ref 32-34).
Fig. 5

SEM images showing the etched cross-sectional microstructure of the LPCS Cu-based solid-lubricating coatings (a) C, (b) CA, (c) CAC5, (d) CAC10 and (e) CAC20

Compared to the CA coating, it is seen from Fig. 5(c) that the copper lamellas of CAC5 are larger and have slight plastic deformation. With further increasing of the Cu-coated graphite content to 10 and 20 wt.% in the spray powder, the copper lamellas become finer and there is an obvious plastic deformation as compared to the CAC5 coating (Fig. 5d and e). This phenomenon could be attributed to the enhancement of the mechanical hammering effect because the relative content of Al2O3 is higher in CAC10 and CAC20 powders than that in CAC5 powder. In addition, it can be found that there are more inhomogeneous regions in the CAC20 due to its high content of Cu-coated graphite. These results indicate that the plastic deformation, microstructure homogeneity and the interface bonding of particles can be influenced by the compositions and characteristics of the feedstock powders in the cold spraying (Ref 25, 35).

Mechanical Properties of the LPCS Cu-Based Solid-Lubricating Coatings

Hardness of the LPCS Cu-Based Solid-Lubricating Coatings

Figure 6 shows the effect of Cu-coated graphite content on the Brinell hardness of the LPCS Cu-based solid-lubricating coatings. On the whole, the hardness of the LPCS Cu-based solid-lubricating coatings is higher than that of the pure copper coating or comparable to it. As expected, the single addition of the hard phase Al2O3 can improve the hardness from 97.0 for the C coating to 114.3 for CA coating. However, the mixture addition of Al2O3 and Cu-coated graphite decreases the hardness of the LPCS Cu-based solid-lubricating coatings. The hardness gradually declines from 107.3 to 88.2 with increasing Cu-coated graphite content from 5 to 20 wt.% in the spray powder.
Fig. 6

Effect of Cu-coated graphite contents on the hardness of the LPCS Cu-based solid-lubricating coatings

Bonding Strength of the LPCS Cu-Based Solid-Lubricating Coatings

Figure 7 shows the bonding strength of the LPCS Cu-based solid-lubricating coatings. Both C and CA coatings have high bonding strength of about 7.5 MPa, which is in accord with the dense microstructure and good interface bonding. However, when Cu-coated graphite is added, the bonding strength (3.0-4.7 MPa) of CAC solid-lubricating coatings is lowered, which is ascribed to the two following facts. Firstly, Cu-coated graphite particle can weaken the mechanical hammering effect of Al2O3 particles, and thus it is difficult to obtain the plastic deformation of copper particles. Secondly, the limited wettability among Cu-coated graphite, Al2O3 and copper particles leads to a poor interface bonding. It is found that the CAC10 (4.6 MPa) has the highest bonding strength compared to the CAC5 (3.1 MPa) and CAC20 (3.3 MPa). This may be due to its finer copper lamellas compared to CAC5 and lower Cu-coated graphite content compared to CAC20.
Fig. 7

Bonding strength of the LPCS Cu-based solid-lubricating coatings

Figure 8 shows the SEM images and EDS maps of fracture surfaces of the LPCS Cu-based solid-lubricating coatings. The fracture of C coating occurs mainly at the interface of the coating and the substrate, while part of the fracture occurs inside the coating. Therefore, the fracture type of pure copper coating is mostly adhesive. When Al2O3 is added, the plastic deformation of the copper particles increases. But the interface bonding between Al2O3 and copper particles is weaker than that among the copper particles. Most of CA coating fracture occurs inside the coating, and only a small part of the fracture takes place at the coating/substrate interface. Compared to the C coating, the fracture of CA coating has a greater cohesive component and a smaller adhesive component. It is implied that the fracture type is cohesive and adhesive (Ref 22, 36). However, the addition of Cu-coated graphite makes CAC10 coating fracture inside the coating completely, suggesting that the fracture type is cohesive.
Fig. 8

SEM images and EDS maps of fracture surfaces of the (a) C, (b) CA and (c) CAC10 coatings

Dry Sliding Wear Behavior of the LPCS Cu-Based Solid-Lubricating Coatings

Figure 9 shows the dry sliding wear behavior of the LPCS Cu-based solid-lubricating coatings. It is found that the friction coefficients of C and CA coatings are 0.82 and 0.94, respectively. The addition of Cu-coated graphite can provide a good solid lubricity for the LPCS Cu-based coatings. It is seen from Fig. 9(a) that the friction coefficient reduces to 0.69 for CAC5, reaches the minimum value of 0.29 for CAC10, and then slightly increases to 0.34 for CAC20. The results indicate that CAC10 coating has the best solid lubricity among the LPCS coatings.
Fig. 9

Friction coefficient (a) and wear rate (b) of the LPCS Cu-based solid-lubricating coatings

In terms of the wear behavior, the wear rates of CAC series coatings are slightly higher than those of the C and CA coatings (Fig. 9b). As mentioned above, the addition of Cu-coated graphite leads to a poor interface bonding between the Al2O3 and copper particles. Therefore, the surface material is readily removed during the sliding, resulting in a slight increase in wear rate (Ref 16, 25). In addition, it is found that the wear rates of CAC series coatings decrease from 2.53 × 10−4 mm3/N m for CAC5, to a moderate wear rate of 2.18 × 10−4 mm3/N m for CAC10 and at last reach the minimum wear rate of 1.20 × 10−4 mm3/N m for CAC20. Actually, the wear resistance of the coatings is mainly dominated by the combined effect of graphite and Al2O3. During dry sliding, graphite with lamellar structure and lower shear strength can easily form a tribo-layer on the worn surface of the coating. The tribo-layer can separate and prevent the direct contact of the tribo-pair effectively, resulting in the decrease in the friction and wear. Meanwhile, Al2O3 acts as a load-support and wear-resistant phase; therefore, it can also reduce the wear rate of the coating effectively. Thus, the combined effect of lamellar solid lubricant graphite and the wear-resistant phase Al2O3 can make the CAC20 coating to display the lowest wear rate among the graphite-containing composites. Also, a similar result has been reported by previous references (Ref 37, 38).

Wear Mechanisms of the LPCS Cu-Based Solid-Lubricating Coatings

Figure 10 shows the worn surfaces of the LPCS Cu-based solid-lubricating coatings and the corresponding steel balls. There are three distinct morphological features on the worn surfaces of the LPCS Cu-based coatings, which are strongly correlated to the composition of the worn surface. Firstly, the worn surface of the C coating is characterized by plastic deformation. Moreover, there are small debris particles and grooves on the worn surface of the coupled steel ball. Thus, the wear mechanism of the C coating is adhesion wear. Secondly, the worn surfaces of CA and CAC5 coatings are analogous, covered with plenty of scattered wear debris and grooves, leading to abrasion wear and higher wear rates. This is in accord with the abrasion characteristic of hard ceramic reinforcements (Ref 25). It also indicates that the low fraction of solid lubricant cannot provide an effective lubrication. Finally, the abrasion debris is significantly reduced on the worn surfaces of CAC10 and CAC20 coatings. A compact lubricating tribo-layer is formed on the CAC10 worn surfaces, together with little debris. However, as for CAC20 with high Cu-coated graphite content, the delamination is present at the graphite-rich areas of the worn surface (Fig. 10e). Additionally, some grooves are found on the surface of the steel ball. Thus, the wear mechanism is delamination and abrasion when the Cu-coated graphite content is above 10 wt.%. In addition, the 3D surface morphologies of wear scars produced on the steel balls after sliding against the C, CA and CAC10 coatings are shown in Fig. 11. It is found that most of the original curvature of the steel balls is still present and all the wear traces of the coupled steel balls are elliptical. This phenomenon indicates that the steel balls suffer very little wear during sliding.
Fig. 10

SEM images showing the worn surfaces of the LPCS Cu-based solid-lubricating coatings and the corresponding balls (a) C, (b) CA, (c) CAC5, (d) CAC10 and (e) CAC20

Fig. 11

3D surface morphologies of wear scars on the steel balls of (a) C, (b) CA and (c) CAC10 coatings

Figure 12 shows the worn cross sections of the C, CA and CAC10 coatings and the EDS analysis of the CAC10 tribo-layer. A mixed tribo-layer with a thickness of 5-10 µm forms on the surface of the pure copper coating, which contains numerous ultrafine and large copper grains. The plastic deformation of copper will improve the strength, thereby increasing the wear resistance (Ref 26). However, when Al2O3 particles are added, some cracks appear around the hard Al2O3 particles on the worn cross section of CA coating (Fig. 12b). This may be due to incompatibility between ceramic reinforcement and metal matrix, so that it is easy to induce cracks in their interface under high external stress (Ref 39). Further inspection shows that there are no cracks and obvious plastic deformation but a very thin mechanically mixed tribo-layer of Cu, Al2O3 and graphite (confirmed by the EDS) forms on the worn cross section of CAC10 coating, providing good solid lubricity.
Fig. 12

SEM images showing the worn cross sections of the coatings (a) C, (b) CA, (c) CAC10 and (d) EDS analysis of CAC10 tribo-layer

Conclusions

In this paper, Cu-based solid-lubricating coatings containing Al2O3 and graphite were deposited on the 304 stainless steel substrate by low-pressure cold spraying. The microstructure, mechanical and tribological properties were evaluated. The main conclusions are drawn as follows:
  1. (1)

    The addition of Al2O3 can increase the plastic deformation of copper particles and refine the needlelike copper lamellas, while the influence of the Cu-coated graphite on the copper particles is the opposite.

     
  2. (2)

    The hardness of the copper-alumina coating is improved compared to the pure copper coating; however, it decreases with the increase in Cu-coated graphite content. The bonding strength is closely related to the actual contents of Al2O3 and graphite in the coatings. Additionally, the fracture types change from cohesive/adhesive to purely cohesive with increasing Cu-coated graphite content.

     
  3. (3)

    The CAC10 coating exhibits a relatively low friction coefficient of 0.29, which is attributed to the combined effect of hard reinforcement Al2O3 and solid lubricant graphite in the Cu-based coating. The wear mechanism of the C coating is adhesive wear, and it transforms to abrasive wear for CA and CAC5 coatings. But for CAC10 coating, a compact and lubricating tribo-layer alleviates the abrasion wear. The delamination occurs on the CAC20 worn surface.

     

Notes

Acknowledgments

This work was supported by the National Natural Science Foundation of China (51675510 and 51675511).

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Copyright information

© ASM International 2018

Authors and Affiliations

  1. 1.State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical PhysicsChinese Academy of SciencesLanzhouPeople’s Republic of China
  2. 2.University of Chinese Academy of SciencesBeijingPeople’s Republic of China

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