Laser processing as an alternative electrodeposition pretreatment

Accepted Manuscript Laser processing as an alternative electrodeposition pretreatment

Yao Wang, Lida Shen, Wei Jiang, Xin Wang, Mingzhi Fan, Zongjun Tian, Xiao Han PII: DOI: Reference:

S0257-8972(18)31215-5 https://doi.org/10.1016/j.surfcoat.2018.11.005 SCT 23971

To appear in:

Surface & Coatings Technology

Received date: Revised date: Accepted date:

9 August 2018 21 October 2018 2 November 2018

Please cite this article as: Yao Wang, Lida Shen, Wei Jiang, Xin Wang, Mingzhi Fan, Zongjun Tian, Xiao Han , Laser processing as an alternative electrodeposition pretreatment. Sct (2018), https://doi.org/10.1016/j.surfcoat.2018.11.005

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Laser Processing as an Alternative Electrodeposition Pretreatment Yao Wanga,1 , Lida Shena,*,1 , Wei Jianga , Xin Wanga , Mingzhi Fana , Zongjun Tiana ,Xiao Hanb a

College of Mechanical and Electrical Engineering, Nanjing University of

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Aeronautics and Astronautics, 210016 Nanjing, China, b

Beijing Institute of Space Mechanic & Electricity, 100080 Beijing, China,

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1 These authors contributed equally to this work.

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Abstract This study aimed to simplify jet electrodeposition pretreatments and improve its prospect for automatic application. A pretreatment method based on laser cleaning and laser texturing instead of the traditional electrodeposition pretreatment technology was proposed. The effects of laser energy density on the mechanical properties of electrodeposited coatings were evaluated. The topography, oxidation, adhesion, and hardness of the coating were characterized. Results indicated that with an increase in pulsed laser energy density, the mechanical properties of the coating initially exhibited strength and subsequently showed weakness. The laser thermal effect changed the topography of the substrate, forming a regular annular superimposed molten pool topography. This occurrence resulted in a mechanical interlock with a corresponding coating topography to improve the bond strength. When laser energy density increased from 0J/cm2 to 4J/cm2 , the adhesive force of the coating increased from 10.6 N to 32.5 N, and the microhardness increased from 345 HV to 515 HV. Keywords: laser cleaning, jet electrodeposition, adhesive force, laser energy density

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1. Introduction

Jet electrodeposition refers to electrodeposition using a jet stream instead of a standing solution. This technique exhibits high current density and fine grains [1–3] and is widely used in the preparation of nanocrystalline materials, composite coatings, and metal microstructures [4–8]. To remove surface contaminations and improve the mechanical properties of the coating, jet electrodeposition uses pre-cleaning treatments, which mainly include mechanical polishing, chemical cleaning, and ultrasonic cleaning [9–11]. However, these treatments contribute to environmental pollution, complex processes, and can hardly handle large workpieces, which processes are difficult to automate. Laser irradiation, an ideal alternative to jet electrodeposition pretreatment, is environment- friendly, accurate, and highly efficient. With respect to its effect on the substrate, this technique can be categorized into two: laser cleaning and laser texturing. Laser cleaning has low energy density and causes no damage to the

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substrate. The effect of laser cleaning on rust, paint, fine particles, and stones has been verified theoretically and experimentally [12, 13], and its applications in cultural relics, microelectronics, and optical devices have gradually increased [14–17]. Laser texturing exhibits high energy density, inducing regular microscopic deformation on the workpiece surface. The effect of interface roughness on adhesion has been confirmed theoretically and experimentally [18, 19]. Laser texturing has been widely used in enhancing coating adhesion, lifetime, and wear resistance [20–22]. We tried laser texturing to replace the traditional pre-treatment method of the spray electrodeposition process and verify the strengthening effect on the electrodeposited coating. In this process, the laser texturing power density was higher than the laser cleaning threshold, so the surface contaminants were also removed. In addition, the study sought a balance between the protection and damage of the substrate to enhance the bond strength of the coating to the substrate, and found the optimum process parameters.

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2. Experimental

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2.1 Experimental mechanism

Fig.1 Schematic diagram of the experimental mechanism

The schematic of this experiment was presented in Figure 1. The thermal ablation effects of laser were first used to remove surface contamination and to form a specific texture [23, 24]. The clean surface was then subjected to jet electrodeposition to deposit the coating. The parameters of laser processing were used as variables and then combined with the fixed parameters of the electrodeposition process. The microstructure and testing parameters were ultimately analyzed to obtain the feasibility and optimized parameters. Multiple parameters influence laser processing. The pulse width and wavelength were fixed because of the limitations of laser device. The adjustable parameters mainly consisted of output power and scanning strategy. The scanning strategy

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included pulse frequency, scanning speed, and scanning pitch, which were mainly reflected in the influence on overlap ratio.

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Fig.2 Laser spot overlap diagram.

𝑂𝑙 =

𝑑𝑠 −𝑑𝑝 𝑑𝑠 𝑑𝑠−𝑑ℎ 𝑑𝑠

（1） （2）

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𝑂𝑝 =

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In order to improve the uniformity of the laser energy distribution, a certain overlap ratio had to be assigned, which was determined using the following laser overlap ratio formulas:

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where the pulse overlap (O p ) is the transverse overlap ratio, and the line overlap(O 1 ) is the longitudinal overlap ratio. An oscillating scanning strategy such as that illustrated in Figure 2, was employed to achieve an optimized overlap effect. The specific parameters were given in a subsequent chapter. Scanning strategy was set as fixed, and laser output power was a variable. 2.2 Experimental Devices and Parameters The experimental device contained a laser section and an electrodeposition section. The former consisted of the ZB-LM-20P laser system of Nanjing Advanced Laser Technology Research Institute. The parameters for the laser system were listed in Table 1. After calculation, Op was 42.86%, and O l was 28.57%. Table 1 Laser system parameters

Parameter

Value

Wave length (nm) Pulse width(ns) Spot diameter (µm) Frequency (kHz) Output power (W) Focal length (mm) Scanning line speed (mm/s) Scanning interval (µm)

1064 100 35 50 10 163±0.5 1000 40

ACCEPTED MANUSCRIPT Laser energy density is regarded as the main parameter that determines the thermal effect of the laser. This parameter is influenced by the output power and the scanning strategy. The formula was given by [25]: F=

ppeak ∙𝑡𝑜𝑛 𝑑𝑝 ∙𝑑ℎ

=

2×103𝑤×10−7𝑠 20𝑢𝑚×50𝑢𝑚

= 20𝐽/𝑐𝑚2

（3）

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Where F is the energy density, P peak is the peak output power, and ton is the pulse width. To illustrate parameter variations, the energy size is expressed as a percentage of energy density. For example, 10% laser fluence is actually 2 J/cm2 . The electrodeposition component was a self-developed jet electrodeposition machine tool. Fig. 3 illustrates the component, which includes the following: a solution circulation system, which controls the injection speed, shape of the injection port, and temperature of the solution; a mechanical transmission system, which controls the processing position, scanning range, and scanning speed; and the electric control system, which can select the constant voltage or constant current power mode and size, processing time, and so on. The composition of the plating solution used in this experiment was shown in Table 2. The parameters of jet electrodeposition processing were listed in Table 3.

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Fig.3 Schematic diagram of jet electrodeposition system. (1) Nickel rod,(2) electrolyte circulated loop,(3)flowmeter,(4) movable platform,(5)bump,(6)heater Table 2 Composition of plating solution Ingredient

Content(g/L)

NiSO4 .6H2 O

280

NiCl2 .6H2 O

40

H3 BO4

40

Temp(℃)

PH

50℃±1

4±0.1

Table 3 Electrodeposition processing parameters Parameter

Value

Nozzle size (mm)

20*1

Flow (L/h)

300

Machining gap (mm) Processing time (min)

4 30

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1000

Current density (A/dm2)

100

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2.3 Experimental material Stainless steel is a basic material used for industrial applications. In this experiment, 304 stainless steel plates measuring 30 mm × 20 mm × 2 mm were used as the substrate. 2.4 Characterization We observed the microstructure and oxidation of the surface by field emission scanning electron microscopy (Hitachi S-4800). An automatic scratch tester (Model WS-2005, Zhongkekaihua Science and Technology Development Co., Lanzhou) was used to determine the adhesive force. The microhardness of the coating was evaluated using the HXS-1000A Vickers microhardness tester (Chengdu Beesda).

3. Results and Discussion

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3.1 Scanning strategy The Surface topography of the workpiece under different laser power were presented in Fig. 4. In Fig. 4a, the original stainless steel surface has a large number of scratches and holes caused by machining, which can easily adsorb grease and particles, among others. With an increase in power, the metal begins to melt around the scan line and the width of the strip-shaped melting region is gradually increased. The substrate melting threshold is considerably higher than the cleaning threshold for grease and particulate contaminants. The presence of the molten pool indicates that cleaning has been completed.

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Fig.4 Surface topographies at different laser fluence. (a) 0%,(b) 6%,(c)12%,(d) 20%

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The parameters of the laser galvanometer scanning system were fixed. Thus, the actual scanning area remains basically the same. An increase in accumulated heat leads to a width increase in the fused zone and the expansion of individual puddles. The topography in Figure 4d shows that the scanned area formed by spot superposition completely covers the substrate. Thus, this scanning parameter completes the preset target. The laser spot and scan line overlap, ensuring the energy uniformity of laser processing. 3.2 Substrate oxidation Owing to the extremely high thermal effect of the laser, the metal in the air was easily oxidized. The main components of the oxide generated on the surface of the stainless steel were identified as Fe2 O3 and Cr2 O3 [26]. The deposited layer hardly adhered to the oxide layer because of the high proportion and high resistivity of Fe2O3. Excessive levels of oxidation can cause hydrogen embrittlement [27] and reduce coating adhesion. Thus, oxidation should be controlled during laser processing. In further experiments, the energy density was divided by 0%, 2%, 4%, and so on, up to 40%.As power increases, the surface of the workpiece changed from ordinary (0% to 6%),to bright silver white (8% to 14%),to dark silver white (16% to 26%),to dark brown (≥28%)and gradually losing metallic luster. The change in color was associated with the oxidation and texture structure—the darker the color, the higher the oxidation and the deeper the texture.

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Fig.5 Substrate EDS of oxygen

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3.3 Coating topography

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The area EDS (Energy Dispersive Spectroscopy) of surface oxidation is presented in Figure 5. The oxygen content increased with an increase in energy density. The initial oxidation rate increased fast and gradually stabilized. With substrate oxidation as a hidden factor for electrodeposition, laser energy density should be kept as low as possible. Chemical treatment methods such as pickling and removing the oxide layer cannot be easily replaced by laser treatment. This difficulty may be alleviated with the development of pulsed lasers. Ultrashort pulse width and high-power lasers could instantly vaporize the oxide layer [28] and produce small heat-affected zones [29].

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Fig.6 SEM of surface and plating topographies at different laser fluence.(a)0% substrate, (b)0% plating,(c)16% substrate,(d)16% plating,(e)32% substrate,(f)32% plating

Fig.7 Roughness of the coating and substrate

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After the scanning strategy has been confirmed to achieve the preset target, the laser-processed substrate is subjected to fixed-parameter jet electrodeposition. Figs. 6a, 6c, and 6e present the substrate topography, and Figs. 6b, 6d, and 6f present the corresponding coating topography. When energy density reaches 32%, as shown in Fig. 6e, the annular molten pools disappear and become a wavy surface, with apparent liquid metal turbulence characteristics can be observed. Finally, the molten pools are connected in a line shape along the laser scanning direction to form a groove. Owing to the excellent capability of jet electrodeposition, the coating is tightly bonded to the substrate, and the surface topography of the coating is highly consistent with the substrate topography. In Figure 6b, the deposited layer of the original stainless steel surface is a sand- like uniform with a single- unit cell diameter measuring less than 1µm. Vertical depressions and bulges in the coating can be observed, corresponding to the scratch topography of the substrate. When the energy density is 16%, as that shown in Fig. 6d, the shape of the

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annular superposed coating appears, which is consistent with the topography of the substrate. This finding indicates a strong bonding between the coating and the substrate and uniform thickness of the coating at different topographies. A number of small cells with a diameter of 1µm appear in the vicinity of the annulus, indicating that the grain size remains unchanged. The coating topography of the 32% energy density is shown in Figure 6f. The height difference of molten pool is larger than that in Figure 6d, indicating a more severe “tip discharge” [30]. Which tends to cause the metal reduction process to occur at the peaks where it is easier to discharge, resulting in a thicker coating at the “peak” and a thinner coating at the “valley.” The internal stress on uneven coating thickness harms the structure and adhesion of the coating, causing it to fall off and tear. The topography of the coating is more complex, exhibiting a large number of randomly distributed circular nodule cells with a diameter of 3–5µm. This finding indicates that the unit cell becomes enlarged, and the coating quality deteriorates. We found that as the laser power increased, the surface roughness of the substrate generally increased. In the first stage, the metal surface was slightly melted, and the scratches and holes edges left by the machining became smooth and the roughness was basically unchanged. In the second stage, as the depth of the puddle increased, the texture was prominent, and the roughness rose rapidly. In the third stage, the crater was gradually replaced by the turbulent morphology, the texture morphology disappeared, the relative height difference decreased, and the roughness decreased. Specific data can be seen in Figure 7. The relative height difference of the puddle reached the maximum when the laser power density was about 28%, which was about 5um.

Fig.8 The coating cross-section topographies (a) 16% laser fluence (b) 0% laser fluence

Coating cross-section topographies are shown in Figure 8. Fig. 8a shows the strong bond between the plating and the substrate. The figure also presents a wavy topography of the bonding seam, which was attributable to the close attachment of the coating to the substrate. This tight interlock can effectively improve coating adhesion to the substrate and disperse the friction of the coating [31]. The strengthening mechanism was believed to be mainly attributable to the micro-pattern array structures which increase surface contact area between coating and substrate and the micro-roughness on the flanks of the patterned features [32]. A suitable interlocking depth can increase the bonding force; however, an extremely deep groove can reduce the wettability of the plating solution [33], hinder the generation and growth of the

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coating at the groove, and destroy the mechanical engagement. In Fig.8b, slight separation from plating occurs, indicating the weak bond between the plating and the substrate. The conclusion was drawn by combining the surface topography and cross-sectional topography. Proper laser texturing formed a mechanical interlock with the coating to improve the bonding force. As the laser energy density further increased, the coating quality may decreased, and the bonding may deteriorate. 3.4 Adhesion Current research demonstrates the relationship between scratching and coating adhesion through a series of effective models [34]. The principle behind the friction detection technology is described in the following: Apply a vertical load to the probe to rub the surface of the coating in a horizontal direction. When the coating near the probe tears, the frictional force will decrease, thereby determining the critical value of the coating adhesion. The scratch test results for nickel plating under different laser energy densities are shown in Fig. 9. Without laser pretreatment, the coating quickly appeared the bulge and then ruptured. The critical value of the bonding force was about 10.6 N. At 10% laser energy density, the coating adhesion increased to 22.6 N. The first half of the scratch was well combined, and the bulge appeared in the second half. At laser energy densities of 20% and 30%, the scratches caused no significant damage to the coating, and bonding was good. The corresponding load–friction diagram is presented in Figure 8e. The blue scatter line exhibits a generally stable trend, whereas the black scatter line was significantly interrupted at 29.9 N. This result showed that 20% of the laser energy density exerted an optimized bonding effect and that the coating performance was stable. When energy density increased from 0 J/cm2 to 4 J/cm2 , the adhesive strength of the coating increased from 10.6 N to 32.5 N. In other experiments conducted by our team, traditional pre-treatment methods had been used [1-4]. This process includes: ultrasonic cleaning with deionized water → ultrasonic cleaning with acetone solution → alkaline degreasing → ultrasonic cleaning with deionized water → ultrasonic cleaning with alcohol → drying. The goal is to completely remove surface machining residues and grease. In the case where other parameters are consistent, the traditional pre-processing method is adopted, and the bonding force test result is about 15N~20N. For example, in [3], the common jet electrodeposition coating exerted a bonding force of 17 N. This result proved the strengthening effect of laser texturing, which may improve with other processes.

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Fig.9 Scratch surface topographies of (a)0%, (b)10%,(c)20%,(d)30%, and (e)Load-friction diagram

3.5 Microhardness The change in the microhardness of the nickel coating under different energy densities are shown in Fig. 10. With an increase in energy density, the microhardness first increased and then decreased. In a low energy density (0%–12%) stage, the nickel coating exhibited a microhardness of about 390 HV. In the medium-energy density (16%–22%) stage, the nickel coating had a microhardness of about 500 HV. In the high-energy density (28% –36%) stage, the nickel coating exhibited a microhardness of about 420 HV. Compared with that of 345 HV at 0%, the hardness of 515 HV was achieved at 22%, and the improvement was remarkable. It was worth noting that the hardness of the substrate is also increased after laser irradiation, which may be attributed to laser quenching.

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Fig.10 Microhardness of the coating and substrate

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The hardness of the coating was affected by the microscopic grain size, density of the coating, and bonding of the coating. In the low-energy density stage, particulate dirt and oil stains, among others, on the coating surface were not completely removed, and bonding was weak and poor. In the middle-energy density stage, particulate dirt and oil stains were removed, and bonding was improved. The coating formed a mechanical interlocking structure with the substrate, which limited the expansion of the plated metal and formed a tight compression structure to improve the coating hardness. At high-energy density stages, tip discharge reduced plating uniformity and compactness and increased the grain size, which caused a decrease in hardness.

4. Conclusions

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Inspired by laser cleaning technology, we considered the introduction of lasers as a pre-treatment method for jet electrodeposition to replace traditional complex processes to remove impurities such as grease and machining residues. In order to ensure a more even distribution of the laser, we chose an optimized scanning strategy as a fixed parameter for the experiment. We performed a single variable comparison test using laser power density as a variable. During the experiment, we found that as the laser power increased, the plating peeling of the coating during the electrodeposition process was significantly reduced. With an increase in power, the substrate metal begins to melt around the scan line and the width of the strip-shaped melting region is gradually increased. At the same time, Owing to the excellent capability of jet electrodeposition, the coating is tightly bonded to the substrate, and the surface topography of the coating is highly consistent with the substrate topography. It has also been found in the subsequent test results that as the laser power is increased, the bonding strength of the plating layer is

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Acknowledgements:

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This work was supported by the following funds: (1) Jiangsu Provincial Science and Technology Plan (Grant No.BE2017001-3 and No.BE2015029); (2): National Natural Science Foundation of China (Grant No. 51475235, No. 51105204, No. 51605473 and No. U1537105); (3) Jiangsu Provincial Key Research and Development Plan (Grant No. BE2016010-3); (4) National Key Research and Development Program of China (Grant No. 2018YFB1105400); (5): Jiangsu Provincial Research Foundation for Basic Research (Grant No. BK20161476).

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ACCEPTED MANUSCRIPT Research highlights: 

Applying laser cleaning in electrodeposition pre-treatment.

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Innovatively combined laser cleaning and laser texturing for jet

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electrodeposition. Laser texture can improve the bonding strength of the coating

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Laser energy density has a great influence on the mechanical

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properties of the coating

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remarkably

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