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Abstract
This article delves into the use of waterborne thin organic coatings (TOCs) as base coats for color coatings in the construction industry, focusing on the effects of various zinc alloy coatings on the properties of coated panels. The study explores the advantages of TOCs, such as simplified coil coating processes and reduced solvent use, and examines the performance of different galvanized coatings, including standard zinc, zinc-aluminum, zinc-iron, and zinc-aluminum-magnesium alloys. Mechanical testing, including T-bend and impact resistance tests, showed excellent performance across all samples. However, short-term water condensation tests revealed microscopic cracks and corrosion product formation, highlighting the importance of understanding these degradation mechanisms. The article employs advanced techniques like ion beam milling and high-resolution SEM-EDS imaging to visualize interfaces within the coating matrices, providing a comprehensive analysis of the interactions between metallic and organic layers. The findings underscore the significance of tailoring coating systems to enhance corrosion resistance and accelerate the development cycle for new coating technologies.
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Abstract
Steels with four different galvanizing coatings (zinc, zinc–aluminum–magnesium, zinc–iron, and zinc–aluminum) were coated with an acrylic thin organic coating and a solventborne polyurethane topcoat, followed by mechanical and water condensation testing. All the coatings passed the standardized mechanical testing (T-bend and impact resistance) and water condensation testing on flat panels (100% RH, 40°C for 1500 h). However, a combined deformation (T-bend at 0 T) and water condensation test (100% RH, 60°C for 48 h) showed differences between the samples. Below the seemingly intact organic coating, zinc and zinc–aluminum coatings showed thinning during deformation, and good early-stage resistance to humidity-induced metal oxidization. Zinc–aluminum–magnesium coating was more brittle, exposing steel, and initiating the galvanic protection process, which, because of Al and Mg content, was less pronounced than for the zinc–iron coating. Ion beam milling combined with high-resolution SEM-EDS provides an unparalleled technique to assess the early-stage degradation mechanisms and facilitates tailoring of more resistant coating systems.
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Introduction
Prepainted steel is a common raw material used in the construction industry. This hybrid material, composed of galvanized steel with an organic protective coating, can be tailored to meet the requirements of many end use environments. Cost efficiency, environmental legislation, and embedding of functionality within organic coatings are some of the factors that continue to drive the development of new pretreatments, corrosion inhibitors, and functional coatings in the color coating industry.1‐4 Combining traditional pretreatment and primer layers into a single waterborne thin organic coating (TOC), preferably applied at the end of the galvanizing process, is not a new concept,5,6 but has not yet replaced traditional solventborne primers or basecoats in high-performance color-coated products. The concept of a waterborne thin organic coating as the first layer in multilayer organic coatings offers several advantages. For instance, the coil coating process could be simplified, the amount of process waste and the use of solvents could be reduced, and three-layer coatings could be easily applied in typical coil coating lines consisting of two paint application steps.5 A three-layer structure opens numerous possibilities to tailor both the performance of the coil coated products and the esthetical properties of the coating.
In a full coating system, the nature of the galvanized coating plays an important role for the overall properties. Various galvanized coatings are commercially available. The most common is the standard zinc coating (with ~ 0.2% of aluminum), which is known for its good formability and all-around corrosion resistance. Zinc–aluminum coatings with lamellar microstructure derived from the 5% Al content have further improved formability and corrosion resistance.2,7 Zinc–iron alloys have excellent weldability and paint adhesion, and zinc–aluminum–magnesium coatings are claimed to have improved corrosion resistance at a lower coating film thickness than the other alloys.8‐10 Galvanizing is a much older method of protecting steel against weathering than continuous color coating,11‐13 and the degradation mechanisms related to specific alloy compositions are fairly well understood. However, the synergistic protective effects of specific galvanized coatings and novel organic coatings represent more complex degradation processes that cannot be fully comprehended by simply considering protective properties of singular layers.
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Some of the bottlenecks related to introducing novel coating formulations to the market are related to relatively long testing and verification procedures. Currently, quality control during development of prepainted steel is carried out with accelerated exposures, UV-weathering, and corrosion testing, followed by gloss and color measurements, and assessment of blister density, delamination, and paint adhesion. One of the reasons behind the slow pace of approval is that the evaluations rely heavily on visual inspection of changes in macroscopic coating properties. For a long time, molecular-level coating deterioration can remain invisible to the naked eye and undetectable by commonly used evaluation techniques.8,14,15 Formation of any visual signs of degradation may take many several years even at highly corrosive sites.16 A significant improvement would be to be able to observe and understand the microscopic degradation mechanisms and interactions between different coating layers, both metallic and organic, at an earlier stage, where extensive corrosion product formation or external pollutions do not yet render the interpretation of the degradation processes difficult.15,17‐20
In this paper, results of a project to develop a waterborne TOC that could be used as a base for multilayer coil coatings are presented, with emphasis on the effect of galvanizing coating composition on overall properties. The goal of this paper was to address the hidden degradation mechanisms, induced by deformation and water condensation, on a selected set of metallic coatings, on top of which a thin organic coating and a polyurethane topcoat were applied. In order to visualize the interfaces within the coating matrices, modern cross-sectional preparation by ion beam milling, followed by high-resolution SEM-EDS imaging and mapping, was employed.
Materials and methods
Substrates
List of the studied hot-dip galvanized coatings and their compositions is shown in Table 1.
Table 1
Details of the studied galvanized coatings on steel
Zinc coating
Abbreviations
Coating composition (weight-%)
Coating thickness (μm)
Overall thickness (mm)
Al
Zn
Mg
Fe
Zinc
Z
0.2
99.8
–
–
20
0.5
Zinc–Al–Mg
ZM
1.5
97.0
1.5
–
12
0.6
Zinc–Fe
ZF
0.2
~ 90
–
~ 10
20
0.7
Zinc–Al
ZA
5.0
95.0
–
–
20
0.5
Coating process
An alkaline cleaning agent (Gardoclean 338, Chemetall), based on sodium hydroxide and fatty alcohol polyglycol ether, was used to clean the galvanized panels before color coating. An acrylic thin organic coating (TOC, BRUGAL® PRETREAT 030) was applied on the cleaned substrates. The wet formulation had a pH of ~ 11.5. The formulation contained silica (for corrosion protection) and TiO2 (for opacity). The target dry film thickness was 1–2 µm. The peak metal temperature for thermal curing was 80–100°C. A solventborne polyamide-structured polyurethane topcoat was applied on the TOC-coated panels. The peak metal temperature for the coating was 249–252°C, and the target dry film thickness was 27–29 µm. The Tg of the coating was about 35°C.
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Test protocols
Standardized impact resistance and T-bend evaluation of the samples were performed according to SFS EN 13523-5 and 13523-7. Water condensation resistance test (SFS EN 13523-35, ISO 4628-2) was run on flat panels of 10x15 cm size. The samples were held in a chamber with 100% relative humidity at 40°C for 1500 h, and the degree of blistering (blister density and size) was visually assessed during the test. Gloss retention was calculated by measuring gloss at 60º after the test with an Erichsen Picogloss instrument.
The coating performance was further evaluated by first subjecting the samples to mechanical deformation (T-bend at 0 T) and then performing a short-term condensation test placing the bent samples in a humidity chamber at 100% relative humidity and 60°C for 48 hours. Cross-sectional characterization was performed from the tip of the T-bending (Fig. 1).
Figure 1
Schematic view of the cross-sectioning area of the exposed samples
Preparation of cross sections was carried out with an Ilion + Advantage Precision Cross-Sectional System (model 693, Gatan, Inc., USA). The samples were first cut to about 5x5 mm size and manually prepolished, followed by attaching the samples with silver glue (Agar silver paint G3691) to masking blade.21 The ion guns operated with argon ionizing gas. The accelerating voltage was 6 kV. Scanning electron microscopy (SEM) characterization was performed using a Zeiss Gemini 450 microscope equipped with a Bruker QUANTAX FlatQUAD EDS detector.
Results
T-bend and impact resistance
Mechanical testing of coatings showed very good performance (Table 2). All the samples passed the maximum height of impact and the most severe T-bend without adhesion problems. The standardized T-bend evaluation (Table 2) was done visually according to the standard and was based on the eventual increase in exposed area of bare metal. Figure 2 shows cross-sectional SEM images of the samples before and after T-bend. The SEM images were recorded at a 25º angle, showing both the cross-sectional area and some of the sample surface. From the SEM images, it can be confirmed that the metal coating remained unexposed even after bending. However, the coating was for all samples locally disrupted around polyamide structuring agent particles. Additive particles like polyamides are not chemically bonded to the coating matrix and were easily retracted from the coating during deformation as the organic coating was stretched.22 In the following, cross-sectional characterization of individual T-bend samples is discussed more in detail.
Table 2
Impact resistance and T-bend test results
Coating
Impact resistance
T-bend
[Ibf in]
Adhesion
T-bend (T)
Adhesion (T)
Z
160
160
0,0
0,00
ZM
160
160
0,0
0,00
ZF
160
160
0,0
0,00
ZA
160
160
0,0
0,00
Figure 2
SEM images showing the effect of T-bend on coated panels. The image widths are 230 µm (left) and 420 µm (right). The T-bend cross sections were prepared from the outermost tip of the samples (Fig. 1)
Figure 3 shows close-up SEM images and EDS element maps of the sample with zinc (Z) coating. A continuous but locally thinning zinc coating was seen beneath the organic coating (Fig. 3). Some deformation-induced air pockets were observed at the metal/organic coating interface. In a close-up, these cavities were seen to correspond to the zinc layer deformation/thinning caused by the deformation. The adhesion was subsequentially locally lost between the metallic coating and the thin organic coating, although good coating properties were manifested by thin residual threads of the organic coating sticking to the metal surface. In the EDS maps, carbon (blue) is the trace element for the polyurethane topcoat, and silicon (green) for the thin organic coating. Finally, minor cavities and stretch marks were observed around the TiO2 particles in the topcoat. The zinc–aluminum–magnesium (ZM) coating was more brittle than the standard zinc (Z) coating, and cracking of the galvanized coating took place in addition to thinning (Fig. 4). This behavior was only seen in the cross-sectional images, since the polyurethane topcoat was flexible enough to cover the cracks in metallic coating layer. The cracks in the ZM coating were not phase- or grain boundary-specific. The zinc–aluminum coating (ZA) behaved similar to the zinc (Z) coating (Fig. 5). The galvanized coating took up the deformation forces by thinning, and there were local cavities within the thin organic coating layer as a result of coating stretching, and local adhesion losses to the metallic coating. Zinc–iron (ZF) coating was the most brittle: The galvanizing layer was fragmented into small pieces and there were adhesion losses between the steel and the ZF coating (Fig. 6).
Figure 3
Elemental mapping of the cross section of zinc (Z) sample after T-bend
The standardized condensation resistance test on flat panels showed excellent results for all samples (Table 3). No blisters were observed in any of the samples, there were no post-exposure adhesion problems (neither in dry or wet state), and the gloss retention was in line with normal variations for laboratory-applied specimens. Finally, a short-term water condensation test (100% RH, 60ºC, 48 h) was run on T-bend samples at 0 T. The samples were evaluated by electron microscopy, since no standard is available for this test.
Table 3
Humidity resistance test results
Coating
Blister density/size (ISO 4628-2)
Adhesion
Gloss
250 h
500 h
750 h
1000 h
1250 h
1500 h
Wet
Dry
Start
End
Z
0
0
0
0
0
0
0
0
31,4
29,4
ZM
0
0
0
0
0
0
0
0
33,8
29,9
ZF
0
0
0
0
0
0
0
0
34,7
31,4
ZA
0
0
0
0
0
0
0
0
33,7
31,0
Figure 7 shows cross-sectional SEM images of the sample with metallic zinc (Z) coating after short-term humidity exposure of the T-bend sample. The humidity and the elevated temperature induced large-scale cracking of the organic coating. The short-term humidity exposure released the residual stresses within the stretched organic coating. As noted in the literature, the crack formation was initiated at the structural weak interface that was the metal/coating interface.22,23 Deformation combined with humidity exposed the embedded weak adhesion between the metal coating and the organic coating. It should also be noted that the water condensation temperature exceeded the Tg of the coating system.24 While the large cracks in the coating overshadowed the deformation-induced cavities around the polyamide particles, the humidity may further promote their extraction due to different water absorption properties of the main polyurethane matrix and the polyamide particles.25,26 The surface of unprotected zinc is easily deteriorated in humid conditions, with simple zinc oxides, hydroxides, and carbonates appearing as the early-stage corrosion products in pollution-free environments.27‐31 In line with these reports, minor zinc corrosion product formation on the exposed metallic zinc surface was observed by backscattering electron imaging (Fig. 7).
Figure 7
Cross-sectional SEM images of zinc (Z) coating sample after T-bend (0T) and short-term humidity exposure
The ZM sample showed similar cracks in the organic coating as the Z sample. A damaged galvanizing coating renders the metallic coating very prone to electrochemical activity due to oxidation of less noble zinc in favor of more noble iron. Early-stage zinc corrosion was initiated both around the exposed galvanized coating and on the adjacent steel surface (Fig. 8, lower left). Furthermore, sites where the damaged galvanizing coating had been hidden beneath the intact organic coating before cross-sectioning also showed an abundance of zinc corrosion products (Fig. 8, right-hand side). The organic coating is a semipermeable membrane that allows migration of humidity through it,19 attacking the weak or exposed interfaces. The microphases in the ZM coating were a primary zinc phase, a binary Mg-containing phase (MgZn2-Zn), and a ternary eutectic phase with high finely structured Al content.32,33 The Zn-Mg eutectic phase is predominantly dissolved in contact with humidity, as Zn phases are more noble than Zn-Mg phases, which in the beginning of the electrochemical activity may even boost Zn dissolution and simple corrosion product precipitation.32,34,35 This may be ultimately beneficial, since the initial simple corrosion product layer develops into a protective passivating corrosion product layer.
Figure 8
Cross-sectional SEM images of zinc–aluminum–magnesium (ZM) coating sample after T-bend (0T) and short-term humidity exposure
Zinc–iron (ZF) coating was the most brittle of the studied coatings, resulting in an extensive open volume beneath the organic coating, and by far the largest exposed steel surface. Similar to ZM coating that was also somewhat brittle, exposure of iron sped up the oxidation processes even during the very short humidity exposure. All metal surfaces, regardless of whether they were located by the wide cracks in the organic coating, or hidden beneath it, were oxidized (Fig. 9). The layers of oxidized precipitates were uniform and dense, allowing their mapping with the EDS system. The zinc–iron coating is chemically somewhat different to the other alloys, since the coating is produced by heat treatment forming several phases that have different zinc/iron ratios in z-direction.36‐38 The absence of less reactive aluminum and magnesium phases and the presence of multiple intermetallic phases promote the function of zinc as a sacrificial anode toward steel that acts as a cathode.31 With prolonged humidity exposure of the deformed ZF system, full coating delamination would be expected. Overall performance of a color coating systems is derived from understanding the behavior and interactions of individual layers (metal substrate, primer, topcoat), since the surrounding layers are affected differently by deformation and weathering.39,40 In the construction industry, some prepainted materials are deformed before mounting, and testing of flat panels may not reliably reflect the final properties of deformed parts.
Figure 9
Cross-sectional SEM images of zinc–iron (ZF) coating sample after T-bend (0T) and short-term humidity exposure
The zinc–aluminum (ZA) coating performance showed resemblance to the zinc (Z) coating. As the galvanizing coating was thinning rather than cracking, no steel was exposed and electrochemical activity on the metal coating surface was minimal (Fig. 10). Eventually, of course, zinc oxidization on the open cracks in the organic coating is inevitable, but zinc efficiently passivates itself by forming a thin patina layer, preventing further dissolution and maintaining the steel interface intact for a long time. Early-stage corrosion behavior of ZA coating has been reported to be comparable with Z coating also in the literature.41
Figure 10
Cross-sectional SEM images of zinc–aluminum (ZA) coating sample after T-bend (0T) and short-term humidity exposure
Various galvanized coatings (Zn, Zn-Al-Mg, Zn-Fe, Zn-Al) were coated with an acrylic thin organic coating and a polyurethane topcoat, followed by standardized mechanical and humidity exposure tests. All the samples passed the mechanical tests and the water condensation test of flat panels. T-bend samples were further exposed to short-term (48 h) water condensation test, which brought up microscale cracks and corrosion product formation that were not reflected in the standardized testing. Delicate cross-sectional preparation by ion beam milling, followed by high-resolution SEM/EDS characterization, was successfully employed to illustrate the microscale degradation phenomena within coating systems. Mechanical deformation induced fractures and tensions in both metallic and organic matrices, which may be manifested in different ways when the product is weathered in eventual end use environment. The zinc–iron coating was the most brittle, taking up the mechanical load and providing relaxation of the organic coating matrix. However, exposure of iron to humidity resulted in extensive sacrificial oxidization of metallic zinc, resulting in thick oxidized layers on all metal surfaces after humidity exposure, even within regions sheltered beneath intact coating. This initial electrochemical activity, even though not yet macroscopically detectable, would result in earlier full-scale coating delamination than for the standard zinc and zinc–aluminum coating that showed thinning rather than cracking of the galvanized coating, and very minor zinc oxidization only at sites where the organic coating had cracked. Zinc–aluminum–magnesium coating showed both thinning and cracking, but the mixed alloy composition suppressed the early corrosion product formation more than in the case of zinc–iron coating. In summary, the residual tensions within organic coatings were released with increased temperature and humidity after deformation. Being able to observe and understand these mechanisms enables tailoring of more corrosion-resistant coatings and speeding up the laboratory-to-market cycle for new coating and product development.
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