Preparation and tribological performance of electrodeposited Ni-TiB2-Dy2O3 composite coatings

JOURNAL OF RARE EARTHS, Vol. 27, No. 3, Jun. 2009, p. 480

Preparation and tribological performance of electrodeposited Ni-TiB2-Dy2O3 composite coatings LIU Xiaozhen (刘小珍)1, LI Xin (李 昕)1,2, YU Aibing (余艾冰)3, HUANG Weijue (黄玮珏)1 (1. Department of Chemical Engineering, Shanghai Institute of Technology, Shanghai 200235, China; 2. College of Food Science and Technology, Shanghai Ocean University, Shanghai 200090, China; 3. School of Material Science and Engineering, University of New South Wales, Sydney 2052, Australia) Received 3 September 2008; revised 24 November 2008

Abstract: TiB2 and Dy2O3 were used as codeposited particles in the preparation of Ni-TiB2-Dy2O3 composite coatings to improve its performance. Ni-TiB2-Dy2O3 composite coatings were prepared by electrodeposition method with a nickel cetyltrimethylammonium bromide and hexadecylpyridinium bromide solution containing TiB2 and Dy2O3 particles. The content of codeposited TiB2 and Dy2O3 in the composite coatings was controlled by adding TiB2 and Dy2O3 particles of different concentrations into the solution, respectively. The effects of TiB2 and Dy2O3 content on microhardness, wear mass loss and friction coefficients of composite coatings were investigated. The composite coatings were characterized by X-ray diffraction (XRD), inductively coupled plasma-atomic emission spectrometer (ICP-AES) and scanning electron microscopy (SEM) techniques. Ni-TiB2-Dy2O3 composite coatings showed higher microhardness, lower wear mass loss and friction coefficient compared with those of the pure Ni coating and Ni-TiB2 composite coatings. The wear mass loss of Ni-TiB2-Dy2O3 composite coatings was 9 and 1.57 times lower than that of the pure Ni coating and Ni-TiB2 composite coatings, respectively. The friction coefficient of pure Ni coating, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings were 0.723, 0.815 and 0.619, respectively. Ni-TiB2-Dy2O3 composite coatings displayed the least friction coefficient among the three coatings. Dy2O3 particles in composite coatings might serve as a solid lubricant between contact surfaces to decrease the friction coefficient and abate the wear of the composite coatings. The loading-bearing capacity and the wear-reducing effect of the Dy2O3 particles were closely related to the content of Dy2O3 particles in the composite coatings. Keywords: electrodeposition; composite coatings; nickel; TiB2; Dy2O3; friction and wear; rare earths

In recent years, development of metal matrix composite coatings produced by electrodeposition has been important due to their high hardness, good wear resistance and corrosion resistance compared with pure metal or alloy coatings[1–3]. These properties mainly depend on both the matrix phases of a composite coating and the amount and distribution of codeposited particles, which is related to many process parameters, including particle characteristics, electrolyte composition and applied current[1]. Insoluble materials are suspended in a conventional plating bath and are captured in the growing metal film during the codeposition process. These insoluble materials can be powder, fiber or encapsulated particle. The oxide or carbide particles, such as SiC, ZrO2, Al2O3, TiO2, MoO2, CeO2, WC, Si3N4, and B4C, and polymers, such as PTFE and PE, were added to the electrolyte, which were codeposited with Ni or Co-Ni alloy to form composite coatings[1–15]. TiB2 is a ceramic material with super-hardness, very stable chemical stability, and strong

anti-corrosion. Rare earth compounds have been widely used in optics, electronics, metallurgy, chemical and materials engineering, due to their spectrascopic physical and chemical characteristics. We studied the electrodepositing of rare earth oxides with nickel; rare earth oxides particles in composite coatings increased the microhardness of the composite coatings[16]. TiB2 and Dy2O3 were used as codeposited particles in preparing Ni-TiB2-Dy2O3 composite coatings to improve its performance of microhardness, wear mass loss and friction coefficients. In this paper, Ni-TiB2-Dy2O3 composite coatings were prepared by electrodeposition method with a nickel cetyltrimethylammonium bromide (CTAB) and hexadecylpyridinium bromide (HPB) solution containing TiB2 and Dy2O3 particles. The effect of TiB2 and Dy2O3 content on microhardness, wear mass loss and friction coefficients of the composite coatings were investigated. The composite coatings were characterized with X-ray diffraction (XRD), inductively

Foundation item: Project supported by the Science Technology Foundation of Shanghai (072305113), the Program for Professor of Special Appointment (Eastern Scholar) at Shanghai Institutions of Higher Learning and Science Technology Foundation of Shanghai Institute of Technology (KJ2008-07) Corresponding author: LIU Xiaozhen (E-mail: [email protected]; Tel.: +86-21-64941286) DOI: 10.1016/S1002-0721(08)60273-2

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LIU Xiaozhen et al., Preparation and tribological performance of electrodeposited Ni-TiB2-Dy2O3 composite coatings

coupled plasma-atomic emission spectrometer (ICP-AES) and scanning electron microcopy (SEM) techniques.

1 Experimental A suspension of TiB2 and Dy2O3 particles in a nickel sulfate, cetyltrimethylammonium bromide (CTAB) and cetylpyridinium bromide (CPB) electrolyte were electrodeposited to prepare Ni-TiB2-Dy2O3 composite coatings. The composition of the plating bath was: 300 g/L NiSO4·6H2O, 40 g/L NiCl2·6H2O, 30 g/L H3 BO3, 0.1 g/L CTAB, and 0.1 g/L HPB. The TiB2 particles were added to the solution with the content from 5 to 25 g/L, the mixture of TiB2 and Dy2O3 particles, concertration of which is 15 g/L, were added to the solution with the content from 1 to 5 g/L. The average sizes of the TiB2 and Dy2O3 particles (purity>99.99%) were estimated to be 5 μm and 80 nm, respectively. The mixture of TiB2, Dy2O3 particles and the electrolyte was magnetically stirred for 12 h. Subsequently, the suspension was ultrasonically agitated for 30 min just before electroplating. Electrodeposition was carried out in 1000 ml beaker. The Ni-TiB2-Dy2O3 composite coatings were deposited on a polished steel plate with dimensions 40 mm×25 mm× 0.5 mm. A nickel plate was used as anode. The plating bath was magnetically stirred in the electroplating process. The electroplating parameters were current density 4.5 A/dm2, stirring rate of 300 rpm and plating bath temperature of 50 °C. Pure Ni coating and Ni-TiB2 composite coatings were also prepared as control. X-ray powder diffraction patterns of pure Ni coating, NiTiB2 and Ni-TiB2-Dy2O3 composite coatings were acquired with a Rigaku D/max 2550 VB/PC X-ray diffractometer, using Cu Kα radiation. A continuous scan mode was used to collect 2θ data from 20°–80° with a 0.02 sampling pitch and a 2 (°)/min scan rate. X-ray tube voltage and current were set at 40 kV and 30 mA, respectively. The samples of NiTiB2 composite coatings (TiB2 concentration in bath: 15 g/L) and Ni-TiB2-Dy2O3 composite coatings (TiB2, Dy2O3 concentration in bath: 15, 2 g/L) were prepared, respectively. Elemental analysis of Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings were conducted with ICP-AES measurement on a VISTA-MPX ICP-OES atomic emission spectrometer with ICP as light source. To investigate the tribological performance of Ni coating, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings, the friction and wear tests were conducted on a TRB01-02539 sliding wear machine at room temperature, with a speed of 0.12 m/s and a load of 5 N. The diameter of friction pair ball was 6 mm. The friction pair was made of 100Cr6. Wear track radius was 5 mm. The ring number was 5000. The samples were cleaned by acetone before and after wear tests. The wearing

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quality of the sample was determined by BS224S analytical balance. Microhardness of Ni coating, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings were determined on a 401MVDTM microhardness tester. The load and load time were 50 gf and 15 s, respectively. The morphology of Ni coating, Ni-TiB2 and Ni-TiB2- Dy2O3 composite coatings before and after wear tests were made by a FEI Quanta 200FEG scanning electron microcopy.

2 Results and discussion 2.1 XRD studies The X-ray diffraction patterns of the pure Ni coating, NiTiB2 and Ni-TiB2-Dy2O3 composite coatings are shown in Fig.1. With the addition of TiB2 (concentration in bath:15 g/L), new diffraction peaks, along with the Ni peaks, are observed at 27.637°, 34.160°, 57.009°, 61.153°, 68.163°, 71.888°, 78.647°, 88.434°, and 91.482°, respectively(Fig.1(1) and (2)). The diffraction peaks correspond to the TiB2 (001), (100), (002), (110), (102), (200), (201), (112), (003), respectively, demonstrating the presence of TiB2 in composite coatings. With the addition of TiB2 and Dy2O3 (TiB2, Dy2O3 concentration in bath: 15, 2 g/L), new diffraction peaks, along with the Ni and TiB2 peaks, are observed at 20.395°, 29.076°, 33.709°, 97.962°, the diffraction peaks correspond to the Dy2O3 (211), (222), (400), (1022), respectively, indicating the presence of Dy2O3 in composite coatings. As shown in Fig.1 and listed in Table 1, it is found that the diffraction angles θ of the coatings containing TiB2 and Dy2O3 , corresponding to Ni (111), (200), (220), (311) and (222), are different from that of the pure Ni coating, and the coatings containing TiB2 and Dy2O3 display stronger diffraction peaks. It suggests the replacement of TiB2 and Dy2O3 in the Ni lattice.

Fig.1 XRD spectra of different coatings (1) Pure Ni coating; (2) Ni-TiB2 composite coatings; (3) Ni-TiB2-Dy2O3 composite coatings

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JOURNAL OF RARE EARTHS, Vol. 27, No. 3, Jun. 2009

Table 1 Diffraction peaks 2θ of coatings (hkl)

Dy2O3(211)

TiB2(001)

Dy2O3(222)

Dy2O3(400)

TiB2(100)

Ni Ni-TiB2

27.637

34.160

Ni(111)

Ni(200)

44.560

51.841

TiB2 (002)

TiB2(110)

44.519

51.919

57.009

61.153 61.175

Ni-TiB2-Dy2O3

20.395

27.686

29.076

33.709

34.236

44.561

52.000

57.079

(hkl)

TiB2 (102)

TiB2(200)

Ni (220)

TiB2 (201)

TiB2(112)

TiB2(003)

Ni (311)

Dy2O3(1022)

Ni

76.637

98.481 98.359

Ni-TiB2

68.163

71.888

76.240

78.647

88.434

91.482

92.840

Ni-TiB2-Dy2O3

68.372

71.984

76.439

78.693

88.452

91.438

92.643

2.2 Elemental analysis Table 2 shows the results of elemental analysis of Ni-TiB2 composite coatings (concentration of TiB2 was 15 g/L in the plating bath) and Ni-TiB2-Dy2O3 composite coatings (concentration of TiB2, Dy2O3 were 15 and 2 g/L in the plating bath) by atomic emission spectroscopy, implying presence of TiB2 and TiB2, Dy2O3 in the coatings respectively. The results are consistent with the results of XRD. Table 2 Elemental concentrations of coatings/% Ni-TiB2 composite coatings

Ni-TiB2-Dy2O3 composite coatings

Ni

TiB2

Ni

TiB2

Dy2O3

95.69

4.31

95.66

4.31

0.03

2.3 Tribological performance Fig.2 shows the relationships between the content of codeposited TiB2 and Dy2O3 in the composite coatings and the concentration of TiB2 as well as TiB2 (concentration of TiB2 was 15 g/L in the plating bath) and Dy2O3 particles in the plating bath respectively. According to Fig.2(a), the mass fraction of the codeposited TiB2 particles in the composite coatings increases significantly with the increase of TiB2 concentration in the plating bath at beginning, the mass fraction of the codeposited TiB2 particles in the composite coatings increases smoothly with the increase of TiB2 concentration in the plating bath in 15–25 g/L. According to Fig.2 (b),

Ni (222)

92.921

97.962

98.357

the concentration of TiB2 was 15 g/L in the plating bath, the mass fraction of the codeposited Dy2O3 particles in the composite coatings increases with the increase of Dy2O3 concentration in the plating bath at beginning, the mass fraction of the codeposited Dy2O3 particles in the composite coatings increases smoothly with the increase of Dy2O3 concentration in the plating bath in 2–5 g/L. The curves are quite similar to the well-known Langmuir adsorption isotherms, supporting a mechanism based on an adsorption effect. Once the particles are adsorbed, metal begins to deposit around the cathode slowly, encapsulating and incorporating the particles. The highest concentration of TiB2, as well as TiB2 and Dy2O3 particles on the codeposit are due to saturation in adsorption on cathode surface, respectively. Fig.3 shows the relationships between the microhardness of the composite coatings and the content of codeposited TiB2 and Dy2O3 in the composite coatings. According to Fig.3(a), the microhardness of the Ni-TiB2 composite coatings is higher than that of pure Ni coating, and it increases with the increase of TiB2 particles content in the Ni matrix. When the mass fraction of codeposited TiB2 is 4.89%, the microhardness of the Ni-TiB2 composite coatings is as high as 640 HV, which is 23% higher than that of the Ni coating (520 HV). According to Fig.3 (b), the microhardness of the Ni-TiB2-Dy2O3 composite coatings is higher than that of the Ni-TiB2 composite coatings. With the mass fraction of codeposited TiB2 being 4.31%, the microhardness of the Ni-TiB2-Dy2 O3 composite coatings increases with the in-

Fig.2 Effect of TiB2, TiB2 (concentration of TiB2 was 15 g/L in the plating bath) and Dy2O3 concentration in the plating bath on mass fraction of TiB2, Dy2O3 in the composite coatings (a) TiB2; (b) TiB2 (concentration of TiB2 was 15 g/L in the plating bath) and Dy2O3

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LIU Xiaozhen et al., Preparation and tribological performance of electrodeposited Ni-TiB2-Dy2O3 composite coatings

crease of Dy2O3 particles content in the Ni matrix in the beginning; when the mass fraction of codeposited Dy2O3 is 0.03%, the microhardness of the Ni-TiB2-Dy2O3 composite coatings is as high as 648.9 HV, which is 4.56% higher than that of the Ni-TiB2 composite coatings (620.6 HV); then the microhardness of Ni-TiB2-Dy2O3 composite coatings increases smoothly with the increase of Dy2O3 particles content in the Ni matrix. The enhancement in the hardness of Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings is related to the dispersion-strengthening effect caused by TiB2 as well as TiB2 and Dy2O3 particles in the composite coatings, respectively; which impede the motion of dislocations in metallic matrix. It is interesting that the Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings exhibite higher hardness value at the increased content of the codeposited TiB2 and Dy2O3 particles in the composite coatings, respectively.

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Figs.4 and 5 show the relationships between the wear mass loss and friction coefficient of the composite coatings and the content of codeposited TiB2, TiB2 (4.31wt.%) and Dy2O3 in the composite coatings. According to Fig.4 (a), under non-lubricated conditions, the wear mass loss of the Ni-TiB2 composite coatings is lower than that of pure Ni coating, and it decreases significantly with the increase of the mass fraction of codeposited TiB2 in the composite coatings at the beginning; then it decreases smoothly with the increase of the mass fraction of codeposited TiB2 in the composite coatings in 4.31%–4.89%. When the mass fraction of codeposited TiB2 in the composite coatings is 4.31%, the wear mass loss of the Ni-TiB2 composite coatings is as low as 0.11 mg, which is lower 5.7 times than that of the pure Ni coating (0.63 mg). According to Fig.5 (a), under non-lubricated conditions, the wear mass loss of the Ni-

Fig.3 Effect of the mass fraction of codeposited TiB2, TiB2 (4.31wt.%) and Dy2O3 in the composite coatings on microhardness of Ni-TiB2 (a) and Ni-TiB2-Dy2O3 (b) composite coatings

Fig.4 Effect of the mass fraction of codeposite TiB2 in the composite coatings on the wear mass loss (a) and friction coefficient (b) of Ni-TiB2 composite coatings under non-lubricated conditions

Fig.5 Effect of the mass fraction of codeposite TiB2 (4.31wt.%) and Dy2O3 in the composite coatings on the wear mass loss (a) and friction coefficient (b) of Ni-TiB2-Dy2O3 composite coatings under non-lubricated conditions

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TiB2-Dy2O3 composite coatings is lower than that of Ni-TiB2 composite coatings. when the mass fraction of codeposited TiB2 in the composite coatings is 4.31%, the wear mass loss of the Ni-TiB2-Dy2O3 composite coatings decreases with the increase of the mass fraction of codeposited Dy2O3 in the composite coatings at the beginning; when the mass fraction of codeposited Dy2O3 in the composite coatings is 0.03%, the wear mass loss of the Ni- TiB2-Dy2O3 composite coatings is as low as 0.07 mg, which is lower 1.57 times than that of the Ni-TiB2 composite coatings (0.11 mg); then the wear mass losses of Ni-TiB2- Dy2O3 composite coatings decreases smoothly with the increase of Dy2O3 particles content in the Ni matrix. According to Fig.4(b), when the mass fraction of codeposited TiB2 in the composite coatings is 4.31%, the friction coefficient of the Ni-TiB2 composite coatings is 0.815, under the same conditions the friction coefficient of the Ni-TiB2 composite coatings slightly increased than that of the pure Ni coating (0.723). According to Fig.5(b), the friction coefficient of the Ni-TiB2-Dy2O3 composite coatings is lower than that of Ni-TiB2 composite coatings. The friction coefficient of the Ni-TiB2-Dy2O3 composite coatings decreases with the increase of Dy2O3 particles content in the Ni matrix at the beginning; the friction coefficient is 0.619 when the mass fraction of codeposited Dy2O3 in the composite coatings is 0.03%, under the same conditions the friction coefficient of the Ni-TiB2-Dy2O3 composite coatings is lower than that of the Ni-TiB2 composite coatings (0.815); then the friction

JOURNAL OF RARE EARTHS, Vol. 27, No. 3, Jun. 2009

coefficients of the Ni-TiB2-Dy2O3 composite coatings decreases smoothly with the increase of Dy2O3 particles content in the Ni matrix. The friction coefficient of pure Ni coating, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings are 0.723, 0.815 and 0.619, respectively. The friction coefficient of Ni-TiB2-Dy2O3 composite coatings is the least among pure Ni coating, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings. It is suggested that the friction and wear behaviors of Ni-TiB2-Dy2O3 composite coatings are closely related with the content of Dy2O3 in composite coatings. This implies that the friction and wear behaviors of Ni-TiB2-Dy2O3 composite coatings can be largely improved by adding Dy2O3 particles, therefore exhibit excellent tribological performance under non-lubricated conditions. 2.4 SEM image The surface morphology of the pure Ni coating, Ni-TiB2 composite coatings, and Ni-TiB2-Dy2O3 composite coatings, and morphology of worn surface of pure Ni coating, NiTiB2 composite coatings, and Ni-TiB2-Dy2O3 composite coatings are shown in Fig.6. The pure Ni coating shows a relatively smooth surface, as observed in Fig.6 (a). It is seen in Fig.6 (b) and (c) that, Ni-TiB2 and Ni-TiB2-Dy2O3 composite coatings have similar nodular microstructure. It is seen in Fig.6 (c) that, Ni-TiB2-Dy2O3 composite coatings have different sized nodular microstructure due to the different size of particles TiB2 (5 μm) and Dy2O3 (80 nm). It is evident that TiB2 and TiB2, Dy2O3 particles are distributed

Fig.6 SEM images of different coatings (a) Pure Ni coating; (a’) Worn surface of pure Ni coating; (b) Ni-TiB2 composite coatings; (b’) Worn surface of Ni-TiB2 composite coatings; (c) Ni-TiB2-Dy2O3 composite coatings; (c’) Worn surface of Ni-TiB2-Dy2O3 composite coatings

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LIU Xiaozhen et al., Preparation and tribological performance of electrodeposited Ni-TiB2-Dy2O3 composite coatings

in the Ni matrix by electrodeposition, respectively. The results are consistent with the results of XRD. For the pure Ni coating, furrows and spalling can be observed on the worn surface, as shown in Fig.6 (a’), the presence of the furrows and spalling yields larger worn debris. It is seen in Fig.6 (a’), (b’) and (c’) that, without the incorporation of TiB2 or TiB2 and Dy2O3 particles in Ni deposit, wear resistance of the pure Ni coating is weaker, for the Ni-TiB2 and Ni-TiB2Dy2O3 composite coatings, the abrasive grooves on the worn surface are significantly decreased, and the feature shows less abrasive width and depth. It is suggested that, the incorporation of TiB2 or TiB2 and Dy2O3 particles in the matrix can largely reduce the wear of the nickel composite coatings; furthermore, the wear resistance of the Ni-TiB2 and Ni-TiB2Dy2O3 composite coatings are enhanced with addition of TiB2 and TiB2, Dy2O3 particles in the deposit, respectively. According to Fig.6 (b’) and (c’), the worn surface of the Ni-TiB2Dy2O3 composite coatings is smoother than that of Ni-TiB2 composite coatings. It is deduced that, a certain amount of Dy2O3 particles in composite coatings contributes to improving the tribological performance of Ni-TiB2-Dy2O3 composite coatings, since the Dy2O3 particles provide both dispersion-strengthening and particle-strengthening. During the friction process, the codeposited Dy2O3 particles gradually protruded out of the matrix, which carried the loads transferred from the matrix, and as a result, the wear resistance of Ni-TiB2-Dy2O3 composite coatings was enhanced.

3 Conclusion Ni-TiB2-Dy2O3 composite coatings were prepared by electrodeposition method with a nickel, cetyltrimethylammonium bromide and hexadecylpyridinium bromide solution containing TiB2 and Dy2O3 particles. The content of codeposited TiB2 and Dy2O3 in the composite coatings was controlled by the addition of TiB2 and Dy2O3 particles in different concentrations into the solution, respectively. NiTiB2-Dy2O3 composite coatings showed higher microhardness and lower wear mass loss, friction coefficient compared with those of the pure Ni coating and Ni-TiB2 composite coatings. The wear mass loss of Ni-TiB2-Dy2O3 composite coatings was 9 and 1.57 times lower than that of the pure Ni coating and Ni-TiB2 composite coatings, respectively. The friction coefficient of pure Ni coating, Ni-TiB2 and Ni-TiB2Dy2O3 composite coatings were 0.723, 0.815 and 0.619, respectively, Ni-TiB2-Dy2O3 composite coatings was the least among the three coatings. Dy2O3 particles in composite coatings might serve as solid lubricant between contact surfaces, decreased the friction coefficient and abate the wear of composite coatings. The loading-bearing capacity and the wear-

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reducing effect of the Dy2O3 particles were closely related to the content of Dy2O3 particles in the composite coatings.

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