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Article

Study on the Wear Resistance of Ni-Co-ZrO2 Composite Coatings with Different ZrO2 Nanoparticle Concentrations Prepared Using Electrodeposition on the Micro-Surface of Spindle Hook Teeth

by
Tianxin Dong
,
Xingyu Wang
,
Fei Li
,
Yifan Zhu
* and
Xiuqing Fu
*
College of Engineering, Nanjing Agricultural University, Nanjing 210031, China
*
Authors to whom correspondence should be addressed.
Metals 2023, 13(7), 1251; https://doi.org/10.3390/met13071251
Submission received: 5 June 2023 / Revised: 29 June 2023 / Accepted: 6 July 2023 / Published: 9 July 2023
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Abstract

:
To improve the wear resistance of the surface of the cotton picker spindle, a Ni-Co-ZrO2 composite coating with different ZrO2 nanoparticle concentrations was prepared using electrodeposition technology on the micro surface of spindle hook teeth, and the morphologies of the surface and cross-section, element contents, grain sizes, microhardness and friction coefficients of the Ni-Co-ZrO2 composite coating were obtained; a simulated wear test was conducted based on the independently developed spindle hook tooth wear device, and the morphologies and elemental distributions of the composite coating before and after wear were obtained; the effects of different ZrO2 nanoparticle concentrations (0, 2, 4, 6, 8 g/L) on the morphology, element content, grain size, microhardness, friction coefficient and wear resistance of the coating were discussed. The test results indicated that compared with Ni-Co coatings, Ni-Co-ZrO2 composite coatings featured a more compact coating structure, a greater coating thickness, and a smaller grain size. The presence of ZrO2 nanoparticles led to further improvement of the coating’s microhardness, friction coefficient and wear resistance. When the mass concentration of ZrO2 nanoparticles reached 4 g/L, the microhardness of Ni-Co-ZrO2 composite coating reached the maximum value, 545.4 Hv0.1, and the friction coefficient decreased to 0.06. At the same time, in the simulated wear test, the composite coating with this concentration had the smallest wear area and the highest wear resistance.

1. Introduction

As the core component of a cotton picker, the spindle is critical for agricultural machinery and equipment. It is prone to wear in the cotton picking process, leading to a shorter service life of the spindle, higher picking costs, and increased economic losses [1]. Wear of the spindle generally occurs on the micro surface of hook teeth, which starts from the front and rear tooth tips, extends to tooth edges and backs, and then extends backwards along tooth edges, forming a boot-type wear area. The wear of the micro surface of hook teeth is the result of combined actions of abrasive wear, fatigue wear and oxidation wear [2]. To decrease the wear of the spindle, spindle manufacturers electroplate Cr coatings on the surface of the spindle to enhance the surface properties of the spindle [1]. However, studies indicate extensive microcracks on the surface of Cr coating after deposition [3]. These microcracks have adverse effects on the coating [4]. This narrow limitation of Cr coating has prompted researchers to search for alternative coatings to enhance the performance of the micro surface of spindle hook teeth. As a kind of wear-resistant coating, Nickel-based composite coating features high hardness and good wear resistance and is widely used for improving the surface properties of substrate materials. Researchers prepared Ni-P [5], Ni-W [6], Ni-B [7], Ni-Mo [8], Ni-Zn [9], Ni-Cu [10], Ni-Fe [11], Ni-Graphene [12] and other nickel-based composite coatings on different substrates to improve the hardness of the substrates and strengthen their wear resistance. Because the nickel-base coating is made from environmentally friendly and economical materials, it has become a substitute for traditional coatings such as Cr.
It is found through a study that the Ni-Co alloy coating features better physical properties and wear resistance, which plays an essential role in the improvement of surface properties. Wang et al. [13] prepared a Ni-Co alloy coating by means of electrodeposition and conducted tests of the coating. They found that adding the Co element improved the microhardness and wear resistance of the coating. Hu et al. [14] prepared a Ni-Co alloy coating by means of electrodeposition in the high gravity field. They found that the increase of Co concentration was beneficial to the improvement of the microhardness of the coating. Liu et al. [15] prepared a Ni-Co alloy coating on a brass substrate using supercritical carbon dioxide (SC-CO2) assisted electrodeposition technology, which successfully improved the microhardness and wear resistance of the composite coating. Karimzadeh et al. [16] prepared a Ni-Co-P alloy coating on a carbon steel substrate by Pulsed reverse electrodeposition technology, which features excellent wear resistance. Babak Bakhit et al. [17] prepared a Ni-Co/Sic alloy composite coating using traditional co-electrodeposition and sediment co-deposition technology. Ni-Co alloy coating features higher wear resistance than pure Ni coating.
In recent years, researchers began to improve the wear resistance of coatings by adding TiN [18], AlN [19], GO [20], ZnO [21], WC [22], SiC [23], Al2O3 [24] and other hard nanoparticles into coatings. Among the hard nanoparticles, ZrO2 particles have aroused the researchers’ interest because of their excellent physical properties, high hardness, and outstanding wear resistance. Wang et al. [25] prepared a Ni-ZrO2 composite coating on copper substrate by means of pulse reverse electrodeposition. They found that under the same electrodeposition conditions, the hardness and wear resistance of Ni-ZrO2 composite coating were higher than those of pure Ni coating. Beltowska Lehman et al. [26] prepared a Ni-W/ZrO2 composite coating on a steel substrate by means of ultrasonic-assisted electrodeposition, which improved the microhardness of the composite coating. Shen et al. [27] prepared a Ni-P-ZrO2 composite coating on the surface of 45 steel workpieces using the magnetic platform-assisted jet electrodeposition technology. They found that ZrO2 nanoparticles formed a hard, wear-resistant framework in the coating, which significantly improved the microhardness of the coating. Xu [28] et al. prepared a nanocrystalline Ni-Mo/ZrO2 coating by means of the DC electrodeposition process and found that with the addition of ZrO2 nanoparticles, the surface roughness of the alloy coating increased, and the hardness and wear resistance was further improved. Yan et al. [29] prepared a Ni-Al-ZrO2 composite coating with high wear resistance on aluminum alloy by means of pulse electrodeposition technology, which expanded the industrial application range of aluminum alloy.
In summary, various studies have been conducted by researchers on the preparation of composite coatings with high wear resistance on the surface of general substrates. However, few studies have been conducted on composite coatings’ preparation and wear resistance on the micro surface of cotton picker spindle hook teeth. Based on this, in this study, Ni-Co-ZrO2 composite coatings with different ZrO2 nanoparticle concentrations (0, 2, 4, 6, 8 g/L) were prepared using electrodeposition technology on the micro surface of spindle hook teeth. And simulated wear tests were conducted based on the independently developed spindle hook tooth wear device. The effects of different ZrO2 nanoparticle concentrations on the morphology, element content, grain size, microhardness, friction coefficient and wear resistance of the coatings were discussed. This study is designed as a reference for relevant studies on preparing composite coatings with high wear resistance on the micro surface of spindle teeth.

2. Materials and Methods

2.1. Experimental Procedure

The spindle of the PRO-16 cotton picker was taken as the object of study, and the spindle is made of 20CrMnTi steel. With ZrO2 particles with different concentrations added into the plating solution, a Ni-Co-ZrO2 composite coating was prepared on the micro surface of spindle hook teeth by means of electrodeposition technology. The micro surface of spindle hook teeth was first ground and polished and then was subject to electrolytic deoiling and weak activation. After each step, the spindle was rinsed with deionized water. The composition, content and effect of the plating solution are shown in Table 1. The reagents used are all pure analytical reagents. Before preparation of the plating solution, the nanoparticles were immersed in deionized water, fully stirred, and then ultrasonic-treated for 30 min and mechanically stirred for 2 h to prepare a nanoparticle suspension. The plating solution was prepared using nanosuspension, and the coating was prepared using the electrodeposition process parameters shown in Table 2. After the preparation of the coating, the spindle was cleaned with deionized water, subject to ultrasonic vibration for 3 min, and then dried and sealed.
Figure 1 is a schematic diagram of the deposition process of Ni-Co-ZrO2 composite coating on the micro surface of spindle hook teeth. As shown in Figure 1a, the spindle was fixed on the clamping device, the clamping device was immersed in the electroplating solution, the nickel sheet was placed under the clamping device, the nickel sheet was connected to the anode of the DC power supply for oxidation, and the clamping device was connected to the cathode of the DC power supply for reduction. The electroplating solution contained a large coating on the micro surface of the spindle hook teeth.
Based on Guglielmi’s two-step adsorption model [30], the entire electrodeposition process involves the following steps: (a) weak adsorption: as shown in Figure 1c, the ZrO2 nanoparticles with Ni2+ and Co2+ adsorbed number of Ni2+, Co2+ and ZrO2 nanoparticles. After power on, a closed loop was formed by the electroplating solution, spindle, and nickel sheet, so that it was possible for the uniform deposition of Ni-Co-ZrO2 composite on the surface were weakly adsorbed on the micro surface of spindle hook teeth under the action of electric field force to form nucleation sites on the micro surface; (b) strong adsorption: as shown in Figure 1d, the Ni2+ and Co2+ were continuously reduced to Ni atoms and Co atoms on the micro surface of spindle hook teeth through reduction reaction, and were co-deposited with ZrO2 nanoparticles on the micro surface; in the deposition process, ZrO2 nanoparticles in strong adsorption state were embedded in the composite coating on the micro surface. A complete, compact Ni-Co-ZrO2 composite coating was deposited on the micro surface of spindle hook teeth through electrodeposition.

2.2. Instruments

To observe the morphology of the composite coating on the micro surface of spindle hook teeth and conduct subsequent characterization tests, the spindle was cut using instruments such as an electric discharge cutting machine, ultrasonic cleaning instrument, and metallographic inlay machine for preparing spindle teeth surface observation specimens and spindle cross-section samples. The specific sample preparation process is shown in Figure 2. The morphologies of the surface and cross-section of the composite coating on the micro surface of spindle hook teeth were observed using a field emission scanning electron microscope (FREE-SEM Quanta FEG250, FEI Instruments, Hillsboro, OR, USA). The content and distribution of the elements in the coating were analyzed using an EDS energy spectrum analyzer (XFlash5030BrukerAXS, Inc., Berlin, Germany). The physical phase structure of the composite coating was analyzed using an x-ray diffractometer (incident ray according to Cu target Ka ray, step size of 0.02°, incidence angle of 20°–90°, PANalytical X‘pert; PANalytical Inc.,Malvern, UK), and the average grain size was calculated using Scherrer formula (Equation (1)).
D = K λ B cos θ
where D is the average grain size in the direction perpendicular to the crystal plane (nm), K is the Scherrer constant (generally 0.89); B is the half-height width of the diffraction peak of the sample (rad), θ is the Bragg diffraction angle (°), and λ is the X-ray wavelength (generally 0.15406 nm).
The hardness of the coating on the surface of spindle hook teeth was analyzed using a microhardness tester (Duramin-40struers, Copenhagen, Denmark), with a test load of 100 g and a holding time of 15 s. The friction coefficient of the coating was analyzed using a material surface comprehensive performance tester (CFT-I, Zhongke Kaihua Instrument Equipment Co., Ltd., Wuhan, China), with a load of 330 g load, a reciprocating length of 3 mm and a duration of 30 min. The wear of the spindle in the actual cotton-picking situation was simulated using the independently developed spindle hook tooth wear device, with quartz sand as the wear medium, the speed of the wear device set to 4000 r/min and a wear time of 6 h. The worn spindle was cut and prepared into a sample, and the micro surface and cross-section of the spindle hook teeth were observed and analyzed in the same manner.

3. Results and Discussion

3.1. Micromorphology

Figure 3 and Figure 4, respectively, show the surface and cross-section morphologies of composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of spindle hook teeth. As shown in the figures, adding ZrO2 nanoparticles changed the micromorphology and coating thickness of the composite coating on the micro surface of spindle hook teeth. As shown in Figure 3a and Figure 4a, with no ZrO2 nanoparticles added, the composite coating on the micro surface of spindle hook teeth had a large blocky structure, and there were a few precipitates on the surface of the composite coating, with uneven precipitation and a thickness of the composite coating of only 113 μm. With ZrO2 nanoparticles added, as shown in Figure 3b and Figure 4b, the blocky structure of the composite coating on the micro surface of spindle hook teeth became smaller, and the thickness of the composite coating increased. Still, there were cracks between the blocky structures. The size reduction of the blocky structure led to a more compact composite coating structure formed on the micro surface. When the ZrO2 nanoparticles were added at a concentration of 2-4 g/L, with an increase of the concentration of ZrO2 nanoparticles, the size of the blocky structure decreased, and the thickness of the composite coating increased. This is because the penetration of ZrO2 nanoparticles into the Ni-Co composite coating provided it with more nucleation sites in the electrodeposition process [27], accelerating the nucleation rate, thus reducing the lateral growth of grains and promoting the deposition process of the composite coating. As a result, the blocky structure of the composite coating decreased in size, and the composite coating was refined. At the same time, due to the surface effect of nanoparticles, the ZrO2 nanoparticles could adsorb more Ni2+ during deposition, leading to an increased thickness of the composite coating [31]. When the ZrO2 nanoparticles were at a concentration of 4 g/L, as shown in Figure 3c and Figure 4c, the composite coating was relatively dense, and the thickness of the composite coating reached the maximum of 148 μm With the continuous increase in the concentration of ZrO2 nanoparticles, as shown in Figure 3d,e and Figure 4d,e, the blocky structure of the composite coating on the micro surface of spindle hook teeth started to get larger, the composite coating surface started to agglomerate and crack, the composite coating started to get rough, and the composite coating started to decrease in thickness. This is because the nanoparticles have high surface activity and thus are prone to agglomeration [17]. When the nanoparticles reached a certain concentration level, the nanoparticles existed in the composite coating as aggregate. These aggregates would lead to the anisotropy of composite coating properties and change the stress distribution in the composite coating, resulting in uneven nucleation sites in the composite coating. As a result, the composite coating got a lowered deposition efficiency, cracks and other defects occurred on the surface of the composite coating, and the composite coating decreased in thickness. The effect of anisotropy caused by agglomeration on the properties of composite coatings can be weakened by optimizing the dispersion stability of nanoparticle solution and reducing the concentration of nanoparticles.

3.2. Elemental Distribution

Table 3 and Figure 5 shows the mass fractions and EDS energy spectrums of elements in composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of spindle hook teeth. With the increase of ZrO2 nanoparticles in concentration, the relative Ni content in the composite coating presented a trend of increasing before decreasing. In contrast, the relative Co content showed a trend of decreasing before increasing. When the ZrO2 nanoparticles were at a concentration of 6 g/L, Ni reached the maximum relative content of 65.06 wt%; when the ZrO2 nanoparticles were at 4 g/L, Co reached the minimum relative content of 4.99 wt%. This indicated that the deposition efficiency of Ni2+ and Co2+ was relatively high, with a concentration of ZrO2 nanoparticles ranging from 4 to 6 g/L. With the continuous increase in the concentration of ZrO2 nanoparticles, since the ZrO2 nanoparticles began to agglomerate, the deposition efficiency decreased, the relative content of Ni deposited in the composite coating gradually decreased, and the relative content of Co gradually increased. However, this composite coating still had a superior relative content of Ni and Co to that with no ZrO2 nanoparticles added. This indicated that adding ZrO2 nanoparticles led to an increase in nucleation sites, improvement of the co-deposition of Ni and Co in the Ni-Co substrate [32], and higher deposition efficiency.
As shown in Figure 6, during line scanning of the cross sections of composite coatings with different ZrO2 nanoparticles concentrations, there was an element permeation area between the composite coating and the spindle hook teeth substrate. As can be seen from the figures, the overall content of each element in the composite coating was relatively stable both in the coating and substrate areas. In the element permeation area, the contents of Ni, Co, and Zr gradually decreased while the content of Fe gradually increased. With a concentration of ZrO2 nanoparticles ranging from 0 to 4 g/L, the thickness of the element permeation area gradually increased as the concentration of ZrO2 nanoparticles increased, as shown in Figure 6a–c. This is because the ZrO2 nanoparticles provided more nucleation sites for the composite coating, leading to higher deposition efficiency, stronger element permeation, and increased thickness of the element permeation area. With the continuous increase in concentration of ZrO2 nanoparticles, the element permeation area gradually decreased in thickness. This was caused by that an excessive amount of ZrO2 nanoparticles led to stronger agglomeration of nanoparticles. There occurred nanoparticles in the composite coating in the form of aggregate, resulting in increased internal stress and uneven nucleation points in the composite coating, thus leading to lower deposition efficiency, lower quality of the composite coating, and decreased thickness of the element permeation area.

3.3. Composition

Figure 7 and Figure 8, respectively, show the XRD spectrums and average grain sizes of composite coatings with different ZrO2 nanoparticles. As can be seen from Figure 7, there are three obvious diffraction peaks, i.e., a diffraction peak at 2θ = 44.4° with a crystal plane index of (111), a diffraction peak at 2θ = 51.7° with a crystal plane index of (200), and a diffraction peak at 2θ = 76.3° with a crystal plane index of (220), from which it can be judged that the composite coating has a face-centred cubic (FCC) structure [33] as its crystal structure. The peak of (111) is the strongest on the crystal plane. Since a solid solution was formed by Co in the Ni lattice, there was no Co peak [34]. With ZrO2 nanoparticles added, it can be seen that the peaks of (111) and (200) in the X-ray diffraction patterns decreased to varying degrees, and a ZrO2 peak appeared. The ZrO2 particles in the X-ray diffraction pattern were small due to the low content of ZrO2 nanoparticles in the composite coating. In the Ni-Co-ZrO2 composite coating, with the increase in concentration of ZrO2 nanoparticles, there was a trend of increasing before decreasing in intensity of the Ni (200) diffraction peak. The intensity of the Ni (200) diffraction peak reached the maximum at a ZrO2 concentration of 4g/L. The addition of ZrO2 nanoparticles promoted the dominant orientation of composite coating growth.
As shown in Figure 8, adding ZrO2 nanoparticles changed the grain size of the composite coating. The average grain size of all Ni-Co and Ni-Co-ZrO2 composite coatings was within the nanoscale (20–40 nm). However, the average grain size of Ni-Co-ZrO2 composite coating was smaller than that of Ni-Co composite coating, consistent with the microstructure analysis results. This is because the competition between nucleation rate and grain growth rate determined the grain size. The grains will be refined if the nucleation rate is faster than the grain growth rate [32]. The addition of ZrO2 nanoparticles led to an increase in the number of nucleation sites in the composite coating, promoting the nucleation process and inhibiting grain growth, and the grains of the composite coating were thus refined. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the average grain size of the coating was the minimum value of 26.5 nm. However, with the continuous increase in concentration of ZrO2 nanoparticles, the Ni-Co-ZrO2 composite coating gradually increased in grain size. This is because the relatively high specific surface energy of ZrO2 nanoparticles made the nanoparticles agglomerate in the composite coating, which weakened the fine-grain strengthening effect of nanoparticles in the composite coating.

3.4. Microhardness

A decrease in the grain size of the coating leads to an increase in microhardness [35], and an increase in microhardness contributes to improving the wear resistance of composite coatings [36]. Therefore, microhardness is one of the significant indicators that reflect the wear resistance of composite coatings. Figure 9 shows the microhardness of composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of spindle hook teeth. The standard deviation is calculated from the hardness measured multiple times for each sample concentration. As can be seen from the figure, with no ZrO2 nanoparticles added, the composite coating was only at a microhardness of 341.7 Hv0.1; with ZrO2 nanoparticles added, the composite coating was significantly improved in microhardness. This indicates that the addition of ZrO2 nanoparticles contributes to the improvement of the microhardness of composite coatings. This phenomenon was caused by the fact that the ZrO2 nanoparticles and Ni2+ were co-deposited in the composite coating, leading to more nucleation sites in the composite coating, higher deposition efficiency, and refined composite coating, with a fine grain strengthening effect; secondly, ZrO2 nanoparticles, as hard nanoparticles, feature higher hardness, which contributes to the increase of the microhardness of composite coatings. When the ZrO2 nanoparticles added were at a concentration of 4 g/L, the microhardness of the composite coating reached the maximum value of 545.4 Hv0.1. With the continuous increase in the concentration of ZrO2 nanoparticles, the composite coating decreased slightly in microhardness. With the concentrations of ZrO2 nanoparticles at 6 g/L and 8 g/L, the composite coating decreased in microhardness by 460.4 Hv0.1 and 445.9 Hv0.1, respectively. This phenomenon was caused by the fact that when the ZrO2 nanoparticles reached a certain level of concentration, there occurred agglomeration, and the agglomerated nanoparticles led to uneven stress distribution in the composite coating, thus reducing the mechanical strength and microhardness of the composite coating.

3.5. Tribological Behaviour

Tribological behaviour is closely related to wear resistance, and the friction coefficient of composite coatings can reflect the tribological behaviour of composite coatings [31]. Figure 10 and Figure 11, respectively, show the friction coefficient and average coefficient of friction of composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of spindle hook teeth during 30 min of friction test. The average coefficient of friction was the average value of the friction coefficients taken from the first 20–25 min of the friction test, at which the friction coefficients were relatively stable. Compared with composite coatings with no ZrO2 nanoparticles added, the composite coating with ZrO2 nanoparticles added had a smaller average coefficient of friction. This is because the pinning strengthening effect of ZrO2 nanoparticles made the atoms in the lattice subject to slip weakening by external forces so that the surface of the composite coating was not prone to plastic deformation, which improved the mechanical properties of the composite coating and thus reduced the friction coefficient. With the increase of ZrO2 nanoparticle concentration, the average coefficient of friction of the composite coating presented a trend of decreasing before increasing. With no ZrO2 nanoparticles added, the composite coating had an average coefficient of friction of 0.26. When the ZrO2 nanoparticles reached a concentration of 4 g/L, the average coefficient of friction of the composite coating reached the minimum value of 0.06. With the continuous increase in the concentration of ZrO2 nanoparticles, the average coefficient of friction of the composite coating increased, reaching 0.16 (6 g/L) and 0.19 (8 g/L), respectively, but still less than the average coefficient of friction of the composite coating with no ZrO2 nanoparticles added. The increase in the average coefficient of friction of the composite coating was due to too many nanoparticles agglomerated on the surface of the composite coating, resulting in uneven deposition of the composite coating, weakening the pinning strengthening effect of the composite coating [37], and reducing the mechanical properties. The average coefficient of friction of coatings is related to microhardness, and the results show that the variation trend of the average coefficient of friction of the composite coating is consistent with that of the above microhardness.

3.6. Wear Resistance

Table 4 shows the mass fractions of elements in composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of the spindle hook teeth after the simulated wear test; Figure 12 and Figure 13, respectively, show the surface micromorphology, EDS spectrum analysis and wear zone length of composite coatings with different ZrO2 nanoparticle concentrations on the micro surface of spindle hook teeth after simulated wear test. As can be seen from the results, after the simulated wear test, each composite coating on the micro surface of the spindle hook teeth contains Fe elements. This indicates that the surfaces of all composite coatings with different ZrO2 nanoparticle concentrations were worn. The wear of the spindle hook tooth coating is caused by abrasive wear. In addition, there were scratches and peeling on the surface of each composite coating. As shown in Figure 14, this phenomenon was caused by the hard particles contacted with the composite coating on the micro surface of spindle hook teeth in the process of wear and slid on the surface of the composite coating, causing plastic deformation and obvious scratches on the surface of the composite coating; additionally, in the process of spindle wear, the composite coating on the micro surface of spindle hook teeth collided with the hard particles in the process of wear, thus shortening the fatigue life of the composite coating and causing fatigue peeling [2]. With no ZrO2 nanoparticles added, the wear area of the composite coating was relatively large, involving the tooth tip, main tooth surface, and rear tooth edge. In addition, the content of Fe was high in the composite coating, and the area of Fe-concentrated distribution was large. With the addition of ZrO2 nanoparticles, the wear area of the composite coating on the micro surface of spindle hook teeth began to decrease, the content of Fe in the wear area decreased, and the area of Fe-concentrated distribution also decreased. This is because ZrO2 nanoparticles, as hard nanoparticles, are conducive to blocking the slipping of atoms in the lattice after being subject to external forces, weakening the plastic deformation of the surface of the composite coating, having dispersion strengthening [38] and pinning strengthening effects, and improving the wear resistance of the composite coating. In addition, the fine-grain strengthening effect of ZrO2 nanoparticles also significantly affected the improvement of the wear resistance of the composite coating. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the wear area of the composite coating on the micro surface of spindle hook teeth was the minimum, with slight wear only on the tooth tip of the surface of the composite coating and the minimum content of Fe in the wear area. With the continuous increase in the concentration of ZrO2 nanoparticles, the wear area of the composite coating on the micro surface of spindle hook teeth began to increase, the wear area also gradually extended from the tooth tip to the main tooth surface, the Fe content in the wear area increased, and the area of Fe-concentrated distribution also increased. This is because with the increase of the concentration of ZrO2 nanoparticles, there were too many nanoparticles that formed aggregates, and these aggregates made the internal stress distribution of the composite coating uneven, resulting in a reduction of the overall mechanical properties of the composite coating.

4. Conclusions

In this study, Ni-Co-ZrO2 composite coatings with different ZrO2 nanoparticle concentrations (0, 2, 4, 6, 8 g/L) were prepared on the micro surface of spindle hook teeth by means of electrodeposition technology, simulated wear tests were conducted based on the self-developed spindle hook tooth wear device, the effects of different ZrO2 nanoparticle concentrations on the morphology, element content, grain size, microhardness, friction coefficient and wear resistance of the coating were discussed, and the following conclusions were drawn:
(1)
There occurred a blocky structure on the surface of the Ni-Co-ZrO2 composite coating. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the composite coating had the most uniform and compact surface, with a thickness increased from 113 to 148 μm.
(2)
The addition of ZrO2 nanoparticles is conducive to the co-deposition of Ni and Co in the Ni-Co substrate, leading to higher deposition efficiency and stronger element permeation. When the ZrO2 nanoparticles were at a concentration of 4–6 g/L, Ni2+ and CO2+ had high deposition efficiency. At the same time, when the ZrO2 nanoparticles were at a concentration of 4 g/L, the element permeation was obvious.
(3)
The Ni-Co-ZrO2 composite coating has a face-centered cubic (FCC) structure as its crystal structure, and the ZrO2 nanoparticles in the Ni-Co-ZrO2 composite coating promoted the dominant orientation of composite coating growth played the role of grain refinement and reduced the average grain size of the composite coating.
(4)
The addition of ZrO2 nanoparticles led to a significant increase in the microhardness of the composite coating. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the composite coating had a microhardness of 545.4 Hv0.1. Compared with the Ni-Co composite coating, the microhardness value increased by 59.66%.
(5)
Compared with the Ni-Co composite coating, the Ni-Co-ZrO2 composite coating had a smaller friction coefficient. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the friction coefficient of the composite coating was a minimum of 0.06.
(6)
In the simulated wear test, the wear resistance of the Ni-Co-ZrO2 composite coating was higher than that of the Ni-Co composite coating. When the ZrO2 nanoparticles were at a concentration of 4 g/L, the wear area only occurred at the tips of the hook teeth, with the smallest wear area and the highest wear resistance.
Through a combination of the performance characterization results of the composite coating with the results of the wear test, it was found that the Ni-Co-ZrO2 composite coating with a ZrO2 nanoparticle concentration of 4 g/L had the highest wear resistance on the micro surface of spindle hook teeth. The preparation of composite coatings through the addition of ZrO2 nanoparticles led to a longer service life of cotton picker spindle, as a reference for the relevant studies on the preparation of composite coatings with high wear resistance on the micro surface of spindle hook teeth.

Author Contributions

Conceptualization, T.D. and X.F.; methodology, T.D.; software, T.D.; validation, X.F., T.D. and X.W.; formal analysis, T.D.; investigation, T.D., X.W. and F.L.; resources, T.D.; data curation, T.D.; writing—original draft preparation, T.D.; writing—review and editing, Y.Z. and X.F.; visualization, T.D. and X.F.; supervision, T.D. and X.F.; project administration, Y.Z. and X.F.; funding acquisition, T.D. and X.F. All authors have read and agreed to the published version of the manuscript.

Funding

Financial support for this work was provided by the Fundamental Research Funds for the Central Universities (Grant No. KYLH2022002), Student Innovation Research and Entrepreneurship Training (Grant No. 202230XX314).

Data Availability Statement

The data presented in this study are available in this article.

Conflicts of Interest

The authors declare no conflict of interest.

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Figure 1. Schematic Diagram of the Deposition Process of Composite Coating: (a) schematic diagram of experimental apparatus, (b) schematic diagram of electrodeposition for single spindle, (c) weak adsorption process on the micro surface of a single spindle hook tooth, and (d) strong adsorption process on the micro surface of single spindle hook tooth.
Figure 1. Schematic Diagram of the Deposition Process of Composite Coating: (a) schematic diagram of experimental apparatus, (b) schematic diagram of electrodeposition for single spindle, (c) weak adsorption process on the micro surface of a single spindle hook tooth, and (d) strong adsorption process on the micro surface of single spindle hook tooth.
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Figure 2. Schematic Diagram of Sample Preparation Process: (a) sample of spindle, (b) wire cutting track of hook tooth surface, (c) wire cutting process of hook tooth surface, (d) hook tooth surface sample, (e) wire cutting track of hook tooth section, (f) wire cutting process of hook tooth section, (g) hook tooth section sample, (h) mosaic process, (i) sample after mosaic, (j) grinding and polishing process, (k) sample after grinding and polishing, and (l) wear device test process.
Figure 2. Schematic Diagram of Sample Preparation Process: (a) sample of spindle, (b) wire cutting track of hook tooth surface, (c) wire cutting process of hook tooth surface, (d) hook tooth surface sample, (e) wire cutting track of hook tooth section, (f) wire cutting process of hook tooth section, (g) hook tooth section sample, (h) mosaic process, (i) sample after mosaic, (j) grinding and polishing process, (k) sample after grinding and polishing, and (l) wear device test process.
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Figure 3. Surface Micromorphology of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2 and subscript 1—50 magnification; 2—1000 magnification; 3—5000 magnification.
Figure 3. Surface Micromorphology of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2 and subscript 1—50 magnification; 2—1000 magnification; 3—5000 magnification.
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Figure 4. Cross Section Microtopography of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2.
Figure 4. Cross Section Microtopography of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2.
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Figure 5. EDS Energy Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 5. EDS Energy Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 6. EDS Energy Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations Cross Section EDS Line Scanning of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2.
Figure 6. EDS Energy Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations Cross Section EDS Line Scanning of Composite Coatings with Different ZrO2 Nanoparticle Concentrations: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2.
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Figure 7. XRD Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 7. XRD Spectrum of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 8. Grain Sizes of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 8. Grain Sizes of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 9. Microhardness of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 9. Microhardness of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 10. Friction Coefficient of Composite Coatings with Different ZrO2 Nanoparticle Concentrations during 30 min of Friction Test.
Figure 10. Friction Coefficient of Composite Coatings with Different ZrO2 Nanoparticle Concentrations during 30 min of Friction Test.
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Figure 11. Average Coefficient of Friction of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 11. Average Coefficient of Friction of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 12. Surface Micromorphology (1, 2) and EDS Spectrum Analysis (3) of Composite Coatings with Different ZrO2 Nanoparticle Concentrations after Simulated Wear Test: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2 and subscript 1—50 magnification; 2—1000 magnification; 3—EDS Spectrum Analysis.
Figure 12. Surface Micromorphology (1, 2) and EDS Spectrum Analysis (3) of Composite Coatings with Different ZrO2 Nanoparticle Concentrations after Simulated Wear Test: (a) Ni-Co; (b) Ni-Co-2 g/L ZrO2; (c) Ni-Co-4 g/L ZrO2; (d) Ni-Co-6 g/L ZrO2; (e) Ni-Co-8 g/L ZrO2 and subscript 1—50 magnification; 2—1000 magnification; 3—EDS Spectrum Analysis.
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Figure 13. Wear Zone Length of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Figure 13. Wear Zone Length of Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
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Figure 14. Schematic diagram of wear equipment: (a) the independently developed spindle hook tooth wear device, (b) the spindle wear process, and (c) the wear principle of the micro surface of hook teeth.
Figure 14. Schematic diagram of wear equipment: (a) the independently developed spindle hook tooth wear device, (b) the spindle wear process, and (c) the wear principle of the micro surface of hook teeth.
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Table
Table 1. Composition of Electrodeposition Plating Solution.
Table 1. Composition of Electrodeposition Plating Solution.
CompositionContent (g/L)Effect
NiSO4·6H2O200Provide Ni2+
NiCl4·6H2O50Reduce free cations
CoSO4·7H2O5Provide Co2+
H3BO330pH SRP
C12H25SO4Na0.05Surfactant
CH4N2S0.002Stabilizer
ZrO2 nanoparticles0/2/4/6/8Secondary phase nanoparticles
Table
Table 2. Major Process Parameters of Electrodeposition.
Table 2. Major Process Parameters of Electrodeposition.
Process ParametersValue
Temperature60 °C
Magnetic stirring speed400 r/min
Electrodeposition time2 h
Current1 A
Table
Table 3. Mass Fraction of Elements in Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
Table 3. Mass Fraction of Elements in Composite Coatings with Different ZrO2 Nanoparticle Concentrations.
ZrO2 (g/L)C (wt.%)Ni (wt.%)O (wt.%)Co (wt.%)Zr (wt.%)
034.1449.428.118.330
244.3040.015.337.872.50
425.2361.096.034.992.66
621.5865.064.526.302.54
821.6261.945.946.384.12
Table
Table 4. Mass Fractions of Elements in Composite Coatings with Different ZrO2 Nanoparticle Concentrations after Simulated Wear Test.
Table 4. Mass Fractions of Elements in Composite Coatings with Different ZrO2 Nanoparticle Concentrations after Simulated Wear Test.
ZrO2 (g/L)C (wt.%)Ni (wt.%)O (wt.%)Co (wt.%)Fe (wt.%)Zr (wt.%)
030.3215.9718.492.2532.970
222.7717.8523.692.5511.7121.43
414.0430.5227.853.941.2722.38
629.0514.1727.702.216.0220.85
818.748.4428.052.5318.8323.41
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Dong, T.; Wang, X.; Li, F.; Zhu, Y.; Fu, X. Study on the Wear Resistance of Ni-Co-ZrO2 Composite Coatings with Different ZrO2 Nanoparticle Concentrations Prepared Using Electrodeposition on the Micro-Surface of Spindle Hook Teeth. Metals 2023, 13, 1251. https://doi.org/10.3390/met13071251

AMA Style

Dong T, Wang X, Li F, Zhu Y, Fu X. Study on the Wear Resistance of Ni-Co-ZrO2 Composite Coatings with Different ZrO2 Nanoparticle Concentrations Prepared Using Electrodeposition on the Micro-Surface of Spindle Hook Teeth. Metals. 2023; 13(7):1251. https://doi.org/10.3390/met13071251

Chicago/Turabian Style

Dong, Tianxin, Xingyu Wang, Fei Li, Yifan Zhu, and Xiuqing Fu. 2023. "Study on the Wear Resistance of Ni-Co-ZrO2 Composite Coatings with Different ZrO2 Nanoparticle Concentrations Prepared Using Electrodeposition on the Micro-Surface of Spindle Hook Teeth" Metals 13, no. 7: 1251. https://doi.org/10.3390/met13071251

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