Examination of the metallization behaviour of an ABS surface

Abstract

The main scope of this work is the metallization of high density Acryonitrile Butadiene Styrene (ABS) surfaces for aerospace applications. Originality and main focused area of the study is to grasp the mechanism of physical properties of the surface and the effect of wet chemical processes on the surface of the ABS substrate. After surface sensitization and metallization with nano-sized ions, the polyurethane surface is metallized and nickel (Ni) coated with electroless and elecrolytic Ni plating processes. The ultimate goal of these advances is the production of composite lay-up tools for the production of primary and secondary composite aircraft parts from nanoscale to macro level. Composite lay-up tool requirements of the aerospace industry include a minimum thickness of 5 mm, acceptability of airtightness testing and reduced surface roughness. Results show that increasing current density adversely affects the surface morphology and metallization processes enhance the surface conductivity of the foam.

Keywords

Aerospace engineering electroless plating foam surface metallization nickel coating tool materials

Introduction

Composite manufacturing is significant for the aerospace industry because of preferred characteristics like enhanced strength/weight ratio, high durability limit under cyclic stresses and minimized corrosion issues of composites [1–10]. Composite parts are manufactured by several methods while the hand lay-up process is still used commonly. Thermoset resin impregnated carbon fibres (prepregs) are layed on each other by concerning symmetry and balance rules of composite manufacturing. Afterwards, the thermoset matrix is cured under high temperature and pressures in autoclaves. The aerospace industry uses low tolerances for composite part dimensions. Therefore, several composite lay-up tool materials exist related with the complexity of the parts. Thus, manufactured structures can follow limits of design tolerances. However, the most important problem for composite manufacturing is the thermal expansion coefficient difference between manufactured part and composite lay-up tool material [11]. This problem may result in delamination, spring-backs and distortion problems after the curing process. Related with these concerns, carbon-fibre reinforced composite, aluminium and invar (FeNi36/64FeNi) are recently used lay-up tool materials for composites in aeronautics [12]. Major drawbacks of these composites are low life-cycles, high coefficients of thermal expansion (CTE), high costs and waste occurence [13]. Thus, researchers are focused on the development of Ni lay-up tools via electrochemical methods since Ni has a rather mediocre CTE and is reliable under harsh environmental conditions [14]. Additionally, other important concerns about the tooling material are the thermal cycle durability and wear resistance [15]. Several studies related with the experimental investigation of the tool/part interface were conducted to determine durability and perform life cycle assessment [15–18]. Corresponding studies showed that Ni electroplating with sulphamate solution reveals lower damage to human health than four well-known different thermal spraying processes (wire-arc, plasma, high velocity oxygen fuel (HVOF) and cold spray) which is of signifance for manufacturers of aerospace platforms. Additionally, part production with nickel sulphamate ions contributes to low internal stress characteristics [16]. In the light of these information, the major aim of this study is to set up the fabrication of Ni lay-up tools for composites by virtue of electroforming on ABS surfaces. To the best of our knowledge, almost the complete literature focuses on the metallic substrate for electroplating processes for all applications due to the conductivity requirement of the electroplating process. Since there is a conductivity barrier between anode and cathode surfaces as well as a double layer formation of nickel ions, the electric field is changed directly. Within this regard, Shourije et al. [19] investigated and analysed the distribution of the electric field in a nickel-induced electrolytic cell within different electroplating conditions via COMSOL Multiphysics [20]. Major drawbacks of metallic substrates for aerospace tooling are the cost-effectiveness and manufacturing limitations. Moreover, purchase and manufacturing dimension limits for complex shaped metallic substrates for the electroplating process exist. Thus, the most effective solution is surface metallization of easily machined, transported, and cost-effective polymeric substrates [21].

The originality of this study is that it is the first study for the application of surface sensitization, activation, and electrolytic Ni plating on the surface of ABS for the aerospace industry. The covering metallization was performed stepwise by degreasing, etching, sensitization, activation as well as electroless nickel plating. In the case of sensitization by tin (Sn), complex colloids of an Sn sensitization blend contain mainly ${Sn}^{4 +}$ cores which were stabilized by the ${Sn}^{2 +}$ exterior sheet. Diameters of these colloids were approximately 25 to 100 Å. After sensitization, the surface was metallized with palladium (Pd) by oxidizing ${Sn}^{2 +}$ to ${Sn}^{4 +}$ and reducing ${Pd}^{2 +}$ ions to Pd atoms using an activation solution since Ni tools have superior properties such as resistance to corrosion and minor scratches [22–26]. Additionally, Ni tools may be fabricated with micrometer level sensitivity and very low residual stresses via electroforming [14, 27–33].

Another important property of surface metallization of ABS is that it is also applicable for additively manufactured parts to improve relevant surface properties and especially the surface roughness [34–36]. Butadienes of the ABS structure are removed by chromic acid. ${Cr}^{6 +}$ oxidizes ABS by disjoining C=C double bonds of the butadiene structure [37]. After surface metallization processes, the effect of electroless and electrolytic plating on the surface roughness of the as-built ABS substrates are shown in Figure 1. Reduction of the surface roughness is an important issue for improving surface properties of additively manufactured materials [38]. This study introduces knowledge of improving surface properties and enables hollowed structures of metallized structures with the removal of polymeric parts with strong solvents of ABS.

Figure 1

Change of the surface roughness of the as-build sample after electroless and electrolytic Ni plating.

Within the concept of this study, the surface of the ABS substrate was metalized and plated with an electroless Ni electrolyte to bring the metallic layer on top of the surface of ABS for the preparation of the surface to electrolytic Ni plating. In addition, the final step is the electrolytic Ni plating. In this study, the effect of each metallization technique was examined before and after each metallization and plating procedure. By this route, the mechanism of metallization was examined with microstructural characterization such as; surface morphology, crystallography, elemental spectroscopy methods and electrical characterization via the Hall effect measurement method. Finally, the composite lay-up tool manufactured from the electrolytic Ni plating procedure was obtained. Additionally, this study broadens the horizon of improving surface properties of additively manufactured polymeric parts and manufacturing hollowed structures of metallic parts from polymer additive manufacturing approaches like Fused Deposition Modelling (FDM).

Material and methods

Materials

An ABS substrate manufactured by injection molding with a minced surface roughness of 0.9–1 μm was used. The surface of neat ABS was cleaned and degreased with alkaline (sodium hydroxide (NaOH)) and acidic (chromium(III) oxide ( ${Cr}_{2} O_{3}$ ) as well as sulphuric acid ( $H_{2} S O_{4}$ )) solutions [39]. Surface sensitization was applied by a tin ions containing solution (tin(II) chloride ( ${SnCl}_{2}$ )) while activation was achieved via the palladium(II) chloride ( ${PdCl}_{2}$ ) containing solution. The neutralization as well as acceleration procedures were applied in the sodium sulphite ( ${Na}_{2} {SO}_{3}$ ) and NaOH, copper(I) sulphate ( ${Cu}_{2} {SO}_{4}$ ), ethylenedinitrilotetraacetic acid disodium salt (EDTA $- {Na}_{2}$ ) solutions, respectively. Electroless Ni plating was applied in a hypophosphate reducing agent containing sodium hypophosphite ( ${NaPH}_{2} O_{2}$ ), acidic nickel(II) chloride hexahydrate ( ${NiCl}_{2} \cdot 6 H_{2} O$ ) and basic nickel(II) sulphate hexahydrate ( ${NiSO}_{4} \cdot 6 H_{2} O$ ).

Experimental procedure

Metallization of the ABS surface is a multistep process. Since the main purpose of the present manuscript is to grasp effects of acceleration and neutralization processes on the metallization mechanism, characterization was also applied on intermediate steps.

After the alkaline and acidic cleaning processes, the surface of ABS was available for neutralization and the subsequent acceleration process before sensitization and activation steps. The neutralization stage involved removal of residual chromium from the etching solution by sodium sulphite which is a reducing agent in the solution. Surface sensitization was conducted by submerging the foam into a blend consisting of 50 $\frac{g}{L}$ ${SnCl}_{2}$ and 1 $\frac{mol}{L}$ hydrochloric acid ( $HCl$ ) at 30 ∘C for 5 min.

The effect of the activation approach was conducted in the mixture of both Pd and Sn solutions. The main reason for this process is the intentional constitution of butadiene removal of the acidic etching process with chromium and sulphuric acid solutions. Remarkably, there were microporous regions of removed butadiene positions [40]. The final step was acceleration. The mixture of sodium hydroxide, copper(I) sulphate and EDTA was used as dissolution of ${SnCl}_{2}$ and reduction of Pd onto the surface of ABS, i.e.

{Sn}^{2 +} + {Pd}^{2 +} ⟶ {Sn}^{4 +} + Pd . (1)

After surface activation, the surface was plated by an acidic electrolyte. The aimed plating thickness after each process was 20 μm since the building of a conductive area on the surface of the activated ABS was aimed for. Ni ions inside the alkaline and acidic electroless Ni plating electrolyte were reduced on the exterior of the activated surface. These reduction reactions denoted in Equations (2) and (3) occur with the help of the phosphate reducing agent, i.e.

{Ni}^{2 +} + H_{2} {PO}_{2}^{-} + 3 {OH}^{-} ⟶ {HPO}_{3}^{2 -} + 2 H_{2} O + Ni, (2)

{Ni}^{2 +} + 2 H_{2} {PO}_{2}^{-} + 2 H_{2} O ⟶ Ni + 2 H_{2} {PO}_{3}^{-} + 2 H^{+} + H_{2} . (3)

After these multistep processes electrolytic Ni plating was conducted on the surface and current efficiencies were measured. Within this regard, the plating was performed in a nickel sulphamate (Ni(SO₃NH₂)₂) electrolyte with four varying current densities, i.e. 2, 3, 4 and 5

\frac{A}{d m^{2}}

. The required coating thickness for the determination of tooling specification for the aerospace industry is at least 50 μm. Therefore, because of the coating limit for the characterization and analysis of the samples, four different current densities were applied on each sample.

Characterizations

Surface microviews of the substrate at each step were observed by a Scanning Electron Microscope (SEM) with the brand FEI 430 Nova NanoSEM. Electrical surface conductivity analyses were performed by a Hall Effect Measurement System NanoMagnetics Instruments ezHEMs. Elemental spectroscopy on the top of the surface (approximately 10 nm) was done by a PHI 5000 X-ray photoelectron spectroscope (XPS). Crystallography analyses were performed by the PANanalytical X'Pert Pro X-ray Diffractometer (XRD). Surface tribology analyses and wear rate measurements of electroless Ni plated, non-activated and activated samples were determined with the Tribotechnic Pin-on-Disc & Oscillating Tribometer device. Samples were prepared and analysed according to ASTM C1624 and G171 standards. The effect of the acceleration process on the surface metallization process was examined. After subsequent metallization procedures, electroless and electrolytic Ni-plated samples were analysed with the pin-on-disc method, and surface hardness measurements were conducted with the Zwick Micro Vickers tester under 0.3 N load. Nickel-plated samples mounted on a rotating disc and an aluminium oxide ( ${Al}_{2} O_{3}$ ) ceramic ball having a 6 mm diameter were used under a 2 N load and dry ambient environmental condition. The linear speed of the disc was 5 $\frac{mm}{s}$ with 95 m sliding distance and 5040 cycles.

Results and discussion

Microviews, grain sizes, elemental spectroscopy analysis and morphologies of the coatings were analysed by SEM. ${Sn}^{2 +}$ ions stay on ABS subsequent to the surface sensitization application. After Pd immersion, ${Sn}^{2 +}$ ions are oxidized and ${Pd}^{2 +}$ ions are reduced on the surface as presented in Figure 2. Connected to this observation, the sensitized thickness was examined in detail in Cohen's study [41,42]. Accordingly, the sub-micrometer thickness of the sensitized surface and identification of the oxidation procedure of Sn and its stability was determined by Mössbauer spectroscopy which is based on the Mössbauer effect depicted in Figure 2. As a result, corresponding spectra imply that all ${Sn}^{2 +}$ oxidize to ${Sn}^{4 +}$ succeeding the submersion to an activation blend [41] which is analogue to our observation. The electroless Ni plating was applied with a ${NaPH}_{2} O_{2}$ reduction agent. ${PH}_{2} O_{2}^{-}$ reduces Ni while also dihydrogen reduction was detected on the surface.

Figure 2

Effect of Pd activation on a sensitized surface; (a) Stable state of Sn after Pd immersion as well as (b) Mössbauer spectroscopy results after Pd immersion and stability of ${Sn}^{4 +}$ on the surface [41,42] (reprinted with permission).

The surface of ABS was metallized after electroless Ni plating. Thus, the subsequent plating process was applied on the Ni surface. Current efficiency values after each metallization process were calculated from Faraday's law for electrochemistry [31].

The pH of the commercial alkaline electroless plating electrolytes decreases during the plating procedure. Therefore, alkaline electrolytes loose their stability in time [43]. This unstable condition results in suppression of the stability of the approach and all Ni ions inside the electrolyte are reduced suddenly [43, 44]. However, in the chosen acidic electrolyte, the reduction of Ni ions is continuous and homogeneous in comparison to commercial alkaline electrolytes.

After each surface metallization process SEM analysis was performed. Surface quality and grain size of Ni atoms after the electroless Ni plating process are given as Figure 3. The uttermost adequate surface was measured for the electroless Ni plated surface after neutralization and activation. Grain size and surface morphologies of the surface of ABS is decreased. NAA (Nucleated Activated and Accelerated samples) in Figure 3(e–g) show finer grain sizes in comparison to NA samples. However, the corresponding current efficiency is lower. Thus, usage in industrial applications is not preferable in this case.

Figure 3

SEM images of electrolytic Ni plated surfaces of ABS substrates. ABS substrates were subjected to neutralization and activation with current density values at (a) 2, (b) 3, (c) 4, (d) 5 $\frac{A}{d m^{2}}$ and neutralized, activated and accelerated at current densities of (e) 2, (f) 3, (g) 4, (h) 5 $\frac{A}{d m^{2}}$ .

Furthermore, this study investigates the outcome of the acceleration process on surface metallization and coating efficiency performance of the coatings. Surface finish and current density related efficiency calculations determined by thickness measurements from cross-sectional SEM images can be seen as Figure 4. The theoretical thickness of the sample is 250 μm. The theoretical value and average data of the experimental results are being compared while current efficiencies were calculated in detail. Results indicate that neutralization and activation processes are fairly enough and can be easily seen in Figure 5. Additionally, the acceleration process does not affect current efficiency as expected due to the expectation of improvement in the electrical conductivity values which is explained below in detail. As a result, the optimum processing parameters are 3 $\frac{A}{d m^{2}}$ current density, acidic electroless Ni plated, neutralized and activated conditions. Therefore, the additional process of EDTA and copper (Cu) added acceleration does not fulfil the requirement of efficiency for mass production for the aerospace industry.

Figure 4

Cross sectional SEM analysis of the neutralized, activated and accelerated sample with a current density of 3 $\frac{A}{d m^{2}}$ .

Figure 5

Effect of current density with/without acceleration process after neutralization and activation.

The tribological behaviour of electroless and electrolytic Ni plated samples was determined by wear analyses, surface hardness measurements and surface roughness analyses. Adhesion behaviour and surface integrity of Ni on the surface of ABS were measured to analyse the performance of the Ni lay-up tool under variable environmental conditions depending on the reutilization of the tool after each curing procedure. Pin-on-disc measurements were conducted on neutralized, activated, accelerated, electroless and electrolytic Ni plated samples coated with 2, 3, 4 and 5 $\frac{A}{d m^{2}}$ current densities and on the neutralized, activated and with 3 $\frac{A}{d m^{2}}$ current density coated sample which was the most efficient specimen. The electroless Ni plated sample was also analysed. A corresponding bar chart is provided in Figure 6. Results indicate that the acceleration process and most efficient current density improve the surface resistance. Additionally, absence of an acceleration process on the surface metallization procedure decreases the wear resistance more than the electroless Ni plated sample. On the other hand, surface roughness analyses show that the acceleration process increases the surface roughness. After immersion of the Pd and Sn catalyst containing activation solution, Pd clusters stay still on the surface of the substrate and accelerator particles into the electrolyte dissolve excess of activator and remove them from the surface in order to interfere with the absorbed catalytic action [40]. Thus, the surface roughness is changed because of this removal. Since the subsequent process was electroless Ni plating, the roughness remained lower than the electrolytic Ni coated samples. Comparison of the current densities reveals that the lowest surface roughness was observed at 3 $\frac{A}{d m^{2}}$ which can be seen in Figure 7. In order to analyse the surface integrity hardness measurements were applied several times to obtain repeatability and stability on the surface hardness values. A load of 0.3 N gave stable results for approximately 250 μm thicknesses. The surface of the indented sample (by HV 0.3) and results from the electrolytic Ni plated sample are provided in Figure 8(a,b), respectively.

Figure 6

Effect of acceleration process on electrolytic Ni plating with 2, 3, 4, 5 $\frac{A}{d m^{2}}$ current density and the behaviour of electroless Ni plated samples were examined in detail.

Figure 7

Surface roughness analysis for the activated and Ni plated specimen; activated, accelerated and Ni plated samples with 2, 3, 4, 5 $\frac{A}{d m^{2}}$ current density and electroless Ni plated specimen.

Figure 8

(a) Optical image of the surface hardness measurement with a standard deviation obtained for 5 different hardness values and (b) results of activated, accelerated and electrolytic Ni plated samples with current densities of 2, 3, 4 and 5 $\frac{A}{d m^{2}}$ .

Additionally, XRD was conducted for electrolytic Ni plated specimens at 2, 3, 4, 5 $\frac{A}{d m^{2}}$ current density applied to acidic electroless Ni plated samples as shown in Figure 9. The preferred orientation of face-centred cubic structure varies related to the applied current density and processing parameters. NAA samples always exhibit a regular face-centred cubic pattern due to the crystal structure of Ni. However, remarkably the electrochemical behaviour is affected by the crystallographic orientational plane and the ratio of (111) as well as (002) peaks oriented parallel to the surface since the atomic density varies with these [45] as can be seen in Figure 9. Additionally, surface energies are affected by the observed change in crystal orientation which in turn varies with the acceleration process.

Figure 9

Effect of current density on crystallographic orientation with/without an acceleration process after neutralization and activation.

Results subsequent to the electrolytic Ni plating after each metallization step can be seen in Figure 9. Examination and optimization of process parameters reveal the influence of acceleration on crystallographic arrangements. The strongest reason for the acceleration process is to dissolve excess Sn from the surface to remove adsorbed Pd. Yet this problem is overcome by dissociating Pd and Sn into the activation bath and firstly sensitizing with Sn ions and activating only with Pd. With the help of this procedure almost all of the ${Sn}^{2 +}$ oxidize to ${Sn}^{4 +}$ . Current efficiencies are more efficient in the neutralized and activated case and most intense peaks appear for the (220) plane in comparison to (111).

XPS analyses were conducted for each sample after the electroless Ni plating procedure. Results can be seen in Figure 10. P2p and Ni2p peaks occur due to the use of hypophosphate as reducing agent and electroless Ni plating, respectively. Sn and Pd are not observed since the surface was fully dense in contrast to the literature [14], where foam substrates were examined after the final plating step. However, XPS measurements of this study where performed after acceleration and electroless Ni plating. Thus, presented graphs in Figure 10 display intermediate process results which explains the absence of any Cu peaks while the literature contains results after the final step for foam substrates [14].

Figure 10

Examination of the effect of acceleration process on the electroless Ni coating by XPS.

BET analyses were conducted for electroless as well as electrolytic Ni plated samples and as received ABS as can be seen in Figure 11. The specific surface area was measured by analysing the cross section area of nitrogen molecule. Nitrogen adsorption is the key parameter for the measurement of specific surface area. Results show that application of electroless Ni plating increases the specific surface area of the sample. This result can be explained by the butadiene removal process after the etching while the corresponding space was not filled by Pd ions and thus Ni atoms after electroless Ni plating. In addition, the specific surface area of electrolytic Ni plated surface is decreased as expected since the corresponding pore density is reduced.

Figure 11

Specific surface area of bare ABS, electroless and electrolytic Ni plated surfaces.

Measurement of surface resistivity values of every level of metallization is crucial for the observation of surface resistivity after each process. Hall effect measurements were applied on the metalized surface while charge carrier mobility, surface resistivity and carrier concentration were also determined by this approach. The difference between neat ABS and after the electroless Ni plating procedure with/without acceleration revealed that the surface resistivity decreased after the acceleration process. The most important parameter for improving the surface conductivity of the acceleration process is the solution containing Cu ions. These ions stay still after electroless Ni plating. Thus, the resistivity is decreased in connection with the very high conduction behaviour of Cu under an electric field. Therefore, improvement of the sheet resistance with the acceleration process within high orders of magnitude can be seen in Table 1.

Table 1

Effect of electrical characterization of Ni plating after each electroless plating process.

Sample name	Resistivity $[Ω m]$	Sheet resistance $[\frac{Ω}{sq}]$
Neat ABS	$3.16 \cdot 10^{14}$	$3.16 \cdot 10^{21}$
NA2	$3.69 \cdot 10^{2}$	$1.12 \cdot 10^{5}$
NA3	$2.49 \cdot 10^{2}$	$7.98 \cdot 10^{5}$
NA4	$3.68 \cdot 10^{2}$	$1.12 \cdot 10^{5}$
NA5	$5.07 \cdot 10^{2}$	$1.58 \cdot 10^{5}$
NAA2	$7.54 \cdot 10^{1}$	$2.23 \cdot 10^{4}$
NAA3	$1.22 \cdot 10^{1}$	$3.68 \cdot 10^{4}$
NAA4	$2.13 \cdot 10^{1}$	$6.68 \cdot 10^{4}$
NAA5	$5.75 \cdot 10^{0}$	$1.69 \cdot 10^{3}$

Note: NA2−NA5 are neutralized and activated surfaces with current densities of 2–5 $\frac{A}{d m^{2}}$ while neutralized, accelerated and activated surfaces with corresponding current densities are abbreviated as NAA2−NAA5.

Conclusion

The major objective of this presented manuscript was to define the metallization mechanism of ABS and grasp the behaviour of the coating parameters at each step. Several characterization techniques were applied for the analysis of surface metallization. The effect of activation after sensitization process, pH on the electroless Ni plating behaviour and also affects of current density values on the electroless Ni plated samples were analysed. An efficient surface quality was obtained by the neutralized surface without acceleration process. The highest electrical conductivity was obtained with the electroless Ni plated specimen in the acidic electrolyte with higher Pd amount. Moreover, Sn sensitization, Pd activation as well as electroless Ni plating in the acidic electrolyte are necessary steps before the electrolytic Ni plating for lay-up tool manufacturing.

Footnotes

Disclosure statement

No potential conflict of interest was reported by the author(s).

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