The Shop-Coated Pipeline That Cracked

From JPCL, September 2011 | Free Product Information

More items for Coating Materials

The Shop-Coated Pipeline That Cracked Valerie D. Sherbondy

Senior Chemist, KTA-Tator, Inc. Valerie Sherbondy is a senior chemist for KTA-Tator, Inc., a consulting and engineering firm specializing in industrial protective coatings. Ms. Sherbondy has been employed by KTA since 1990 and has provided laboratory support for the investigation of hundreds of coating failures and coating testing programs. In addition, Ms. Sherbondy serves as the Laboratory Quality Assurance Officer, overseeing the A2LA and NELEC accreditations of the laboratory. She holds a BS in chemistry and a BS in business from the University of Pittsburgh and is an SSPC Certified Protective Coating Specialist (no. 467-921-0326), a member of the American Chemical Society (ACS), and a committee chair for NACE International. Richard A. Burgess Series Editor, KTA-Tator, Inc. Gas transmission pipelines are often coated in a shop using fusion bonded epoxy (FBE) coating systems. These coatings are chosen for their resistance to chemicals in soil and excellent impact resistance, which means less damage during the transportation and installation of the pipe sections and less mechanical damage during backfilling. Shop operations for abrasive blast cleaning and coating application are automated, and the resulting applied films are generally uniform. One drawback is that the weld areas and joints that connect pipe sections must be prepared and coated in the field are generally not as uniform and consistent from joint to joint as are the stick to stick shopapplied coatings. A second drawback with the same FBE coating materials applied in the shop is that they are more difficult to apply in the field due to widely variable environmental conditions.

In This Article Background Laboratory Investigation Conclusions Recommendations

Valerie D. Sherbondy, Senior Chemist, KTA-Tator, Inc

Additional resources must be devoted to inspection of the field-applied coating. In this case from the F-Files, the added field inspection resources paid off when unexpected defects in the shopapplied coatings were discovered. Inspection of the joint areas indirectly extended to the neighboring FBE coated pipe, which revealed occasional cracking and blistering. A failure investigation was initiated, and several pipe sections were removed for examination and laboratory analysis of the coating.

Background
The specification provided for coating the pipe sections required that the steel surfaces be prepared in accordance with SSPC-SP 10, Near-White Blast Cleaning, and that the resultant profile be angular with a depth of 1.5 to 3.5 mils. Once prepared for coating, the pipe sections were to be heated to between 460 F and 500 F, not exceed 500 F. A two-coat FBE coating system was specified. The primer was specified to be applied to achieve a dry film thickness (DFT) of 1620 mils, with an average of 18 mils. The topcoat, or outer jacket, was to be applied immediately after the first coat. The topcoat was to be applied to achieve a DFT of 3036 mils. The total system DFT was specified to be in the range of 4656 mils. The primer was green, and the topcoat was brown. The pipes were prepared and coated in a shop and then shipped to a single location for installation. The field observations included isolated blisters in the coating on the exterior of the pipe and cracks in the FBE coating film at the field bend locations. It was reported that only four or five initial blisters were observed in the field before the pipe sections were installed and welded. Additional blisters were observed on the pipe sections after field installation. The blisters were repaired in the field, with the exception of those on a blistered pipe section sent to the laboratory for examination. In addition, cracks at field bend locations were holiday tested and repaired in the field shortly after the bending procedure. It had been noted that in some instances cracks were not apparent after bending and had appeared the following day. The total FBE thickness around defective areas was measured using a nondestructive electronic coating thickness gage. The thickness readings were obtained in a minimum of six areas on each pipe sample. The average coating system thickness measurements revealed a range of 54.860.6 mils. The nondestructive measurements were consistent with the overall thickness determined by microscopy and confirmed that the total system thickness exceeded the specified range of 4656 mils.

Laboratory Investigation
Coated samples were cut from larger pipe sections at the field site by the contractor and submitted to the laboratory. The samples were to be representative of the typical FBE coating defects observed in the field and included a section of the cracking that was reportedly occurring at the installation site and a pipe section containing blisters observed during installation. Properly heated and cured control samples of the specified primer and topcoat materials were provided by the coating manufacturer. High voltage holiday testing was performed on the pipe sections received by the laboratory prior to sectioning for laboratory testing. This testing was performed to determine if the cracks in the coating sample extended through the FBE coating film to the substrate. It was confirmed that the cracks did extend through the coating, or at least sufficiently deep enough to result in detection of the discontinuity. The laboratory used a plasma cutter to section the pipe samples and isolate the areas exhibiting defects for examination. During the plasma cutting process, additional blisters formed in the FBE coating in the heat-affected zone. The blistering occurred when the coating surface temperature adjacent to the cut line was in the range of 210 F to 220 F. As the surface cooled, most of the
2

A High Performance, Damage Tolerant Fusion Bonded Epoxy Coating

D.G. Enos, J.A. Kehr, C.R. Guilbert 3M Company Corrosion Protection Products Dept. 3M Austin Technical Center 6801 River Place Blvd. Austin, TX 78726 USA ABSTRACT A novel technique has been developed which significantly improves the damage tolerance of epoxy coated components in a variety of corrosive environments. Characterization of these coatings via an array of AC and DC electrochemical techniques has revealed considerable improvements in the overall corrosion performance as a result of this technology. The quality of the protective coating is thereby maintained, despite minor damage, which may occur on the job site. Furthermore, this improved corrosion performance enhances cathodic disbondment (CD) performance while the impact resistance and flexibility of the fusion-bonded epoxy (FBE) coating are unaffected. INTRODUCTION Corrosion is a global problem, consuming three to four percent of gross national product in the developed countries of the world.[1] Selecting economical and effective techniques for minimizing the effects of corrosion is a critical design decision for pipeline systems. Corrosion protection is essential to prevent leaks, environmental disasters, fire and explosion, personal injury, service disruption and costly maintenance. Thus, in addition to effectively dictating the lifetime of the pipeline, the corrosion prevention system also significantly influences the pipelines operational costs such as general maintenance, pumping energy, and capacity upgrades. Although these protective measures are critical, they represent only a small fraction of the overall long-term cost of a pipeline system. Today, higher operating temperatures and a host of hostile environmental conditions that pipeline materials encounter during installation and use require a new generation of coatings [2] to protect both the interior and exterior of the pipe. Hydrogen sulfide (H2S), increased levels of carbon dioxide (CO2) and other factors contribute to a pipeline environment that increases levels of internal corrosion. There are many possible solutions to these problems including use of corrosion resistant alloys, inhibitors, and corrosion protective linings and coatings. FBE coatings have offered an effective solution to these problems for nearly 40 years. As the times and exposure conditions have changed, FBE coatings have evolved as well. More demanding transportation, storage, installation, and pipeline operating conditions require the use of advanced FBE-based worldclass coatings to protect the pipe exterior. In addition, improved field application technology provides comparablequality same-system coatings for the girth weld. FBEs have been formulated to operate in these very harsh service environments. Background, History, and Advantages of FBE Linings and Coatings An FBE is a one part, heat curable, thermosetting epoxy resin powder. It is a material that utilizes heat to melt and adhere to a metal substrate. It provides a coating with no trapped solvents, excellent adhesion, and a tough, smooth finish resistant to abrasion and chemicals. FBE coatings have been in use since 1960 to protect pipelines from corrosion. It is estimated that over sixty thousand miles (ninety-five thousand kilometers) of FBE coated pipelines are installed around the world.

FBE is currently specified in the oil, gas, and water pipeline industries. It has been used as an internal lining in desalination plants in Australia and the Middle East and on gas [5] and oil transmission lines It has been in use protecting downhole tubing for over twenty years. More recently, it has been used in sour crude pipelines [4]. In addition to its use as a stand-alone exterior coating, FBE is the favored primary coating for three-layer polyolefin corrosion coatings, where it has been in use since 1979. In the water industry, FBE provides a thinner lining than competing materials such as concrete, enabling smaller pipe sizes and reduced bulk and weight during handling and installation of pipe. The smooth, hard FBE coating provides reduced friction compared to uncoated or concrete-lined pipe. This results in more efficient flow, reduced energy costs, and lower-installed pump or compressor investment. It has been used on valves, pumps, and fittings in water districts for both water and sewer systems in California for nearly thirty years. It is in use protecting brine-pit piping systems, solving both erosion-corrosion problems as well as general corrosion [5]. FBE has been used in high-sand-content seawater cooling pipework for ten years and is still in excellent condition. It has been applied to valves and pipework handling seawater for the US Trident Submarine program and has a twenty-year history in the pump manufacturing industry effectively protecting against cavitation and slurry damage. In the UK, it has protected drinking water pipework since 1978, with coating on over two hundred thousand square meters [6]. Specific formulations meet the drinking-water requirements in many countries. There are reports of six to eighteen percent flow efficiency improvements in gas transportation when using FBE internally lined pipe as opposed to bare steel pipe []. Using the six percent figure on an eight-hundred mile (thirteen-hundred kilometer), DN 750 (NPS 30) pipeline with a discharge pressure of 140 kPa (960 psig) and a compressor station every eighty miles (one-hundred-thirty kilometers), the potential savings are over four million dollars in compressor equipment cost and an annual energy savings of about a million dollars. Damage Tolerant FBE Coatings Although FBE coatings are extremely effective corrosion protection materials in a wide variety of environments, their overall effectiveness is still closely tied to the quality of the applied coating. As with nearly all barrier coatings, defects caused by mishandling or misuse of the coated pipe significantly reduce its ability to provide the superior corrosion protection required for many applications. Coating damage frequently occurs during the handling and installation of a pipeline, or is the result of rock damage occurring during backfill [7]. The solution to this problem is seemingly quite simple: if the FBE coated pipe is treated properly, and the coating remains structurally sound, the pipeline should readily meet or exceed its design life. Unfortunately, the type of damage which is causing the problems discussed above is nearly impossible to avoid. Policing jobsites and preventing the use of questionable construction practices is problematic at best. Similarly, preventing rock damage during backfill is nearly impossible, and even more difficult to verify. Nevertheless, irrespective of the pipe coating condition, or the abuse level, it still needs to get the job donepreventing the onset of corrosion and subsequent structural problems. It is better to assume that damage to the coating is inevitable, and, instead of trying to prevent it, design the coating to survive it with much of its corrosion-preventive properties intact. In this study, such a coating is pursued. Through the addition of microencapsulated materials, a self-healing FBE coating has been designed. As illustrated below, this coating is considerably more damage tolerant than traditional FBE coatings. The mechanical damage which weakens conventional coatings instead ruptures the microcapsules which in turn heal the FBE coating, preserving its barrier properties. What follows is a brief description of the coating technology under evaluation, along with promising preliminary results. Microencapsulation is a technique through which liquid materials, such as oils, are encapsulated within a seamless, solid shell. An example of microencapsulated oil is presented in Figure 1. A wide variety of shell wall materials are available the appropriate choice is determined by a combination of the application, the material to be encapsulated, and the desired stimulus to rupture the capsule (e.g., impact, pH, or solution chemistry). In general, microcapsules are between 5 m to 200 m (0.2 mils to 8 mils) in size with wall thicknesses on the order of 1 m to 2 m (0.04 mils to 0.08 mils). Fill materials may be either aqueous or non-aqueous in nature. What is important to note is that, once encapsulated, liquid-based fill materials behave as a solid. As a result, considerably larger quantities of the fill material may be added to a coating without adversely affecting its properties.

As an example, suppose a liquid inhibitor has been demonstrated to effectively halt corrosion of the metal to be coated. The coating formulator then makes the decision that the inhibitor should be added to the current coating formulation. However, in the case of a powder coating such as an FBE, only very limited concentrations of a liquid additive may be added before the powder begins to clump and hinder application. If that same liquid is encapsulated prior to addition to the powder, large concentrations of the inhibitor may be added with little or no detrimental effect on the handling or application of the coating material. A similar scenario holds for liquid-based coatings, where large additions of an inhibitor may hinder cure of the coating or degrade physical properties. In this study, a series of modified coatings were formulated and produced, as illustrated in Figure 2. As can be seen in the figure, the coating consists of two layers. The first layer is a primer layer containing the microcapsules. The microcapsules contain approximately 80% active fill, and are approximately 50 m (2 mils) in size. The epoxy matrix of the primer layer is an unmodified, flexible FBE. The second layer of the coating, or the topcoat, is composed entirely of an unmodified FBE. More details on the actual formulation may be found below in the Experimental Methods section. Also illustrated in Figure 2 is the manner in which the coating is designed to function. The coating will behave the same as a traditional FBE until it has been subjected to mechanical damage. This damage may be the result of an impact to the coating, microcracking of the coating during bending on the job site, etc. Once damaged, the microcapsules release their protective fill. By placing the microcapsules close to the steel surface in the primer layer, they are able to deliver their protective fill directly to the regions near the metal surface where they are needed. A variety of fill materials have been investigated, consisting essentially of combinations of corrosion inhibiting materials and sealants. Once released, the fill material reseals the coating and prevents the onset of corrosion, preserving the protective benefits of the FBE. Although placing the microcapsules in the primer layer is the simplest embodiment of this coating concept, it is not the only one. Figure 3 illustrates a coating that has microencapsulated additions in both the topcoat and the primer layer. In this example, a series of different microcapsules could be envisioned, each serving a different purpose. Microcapsules containing corrosion inhibiting materials could be placed in the primer layer, ensuring their delivery directly to the metal surface. In the topcoat, capsules containing sealants could be used, their purpose being to reseal the damage site and hold in place the inhibitive materials released from the primer layer. In addition, microcapsules containing a dye could also be incorporated into the topcoat. Upon damage, the dye capsules would rupture, releasing their fill and locally discoloring the coating (e.g., turn a green coating red), easing the identification of damage sites along the pipe for later repair with appropriate patch materials. EXPERIMENTAL METHODS Coating Composition and Preparation Prior to coating, mild steel bars were degreased in 2-butanone (MEK) and isopropanol, then grit blasted to a near-white metal finish in accordance with NACE No.2/SSPC-SP 10. Each bar was preheated for 45 minutes to a temperature of 400F (205C), after which they were coated via a fluidized bed system. A two-step coating was accomplished by first dipping the sample into the primer bed, after which the sample was immediately transferred to, and coated in the topcoat bed. Samples were left in each fluidized bed for sufficient time to allow the coating to build to the desired thickness. Coating thickness was verified using a magnetic thickness gauge. The FBE coatings investigated in this study were based on a flexible fusion bonded epoxy resin. Control samples were coated with 400 m (16 mils) in a single coating operation. Microcapsule containing coatings were produced by first depositing a primer layer 150 m (6 mils) in thickness which consisted of 85% unmodified FBE + 15% microcapsules, followed by a 250 m (10 mils) top coat of unmodified FBE. The two layers were applied sequentially (i.e., no additional preheating). Electrochemical Testing

Solution Preparation. All solutions were prepared using distilled water and reagent grade chemicals. The cathodic delamination testing solution was made in accordance with ASTM G8 [8] and contained 1% each of sodium chloride, sodium carbonate, and sodium sulfate. Corrosion initiation tests were conducted in mildly acidic, 3.5 wt% sodium chloride solutions. The sodium chloride solutions were first made to the desired concentration after which the pH was adjusted (via HCl) to 5. Cathodic Delamination (CD). Samples were prepared by machining a 6 mm (0.25 inch) defect in the center of a 11.4 cm x 11.4 cm (4.5 inch x 4.5 inch) coated panel. The samples were then placed in the cell pictured in Figure 4. Next, the solution was added and the samples polarized for 30 days at 1.44 V vs. a saturated calomel reference electrode. Periodic electrochemical impedance spectroscopy (EIS) spectra were taken from each sample throughout the 30 days. Upon completion of the test, the coating around the intentional holiday was removed with a knife and the delamination radius measured in accordance with ASTM G8. Four replicates of both the control and the capsule containing samples were investigated. Impact Corrosion Testing. Following coating, samples were subjected to an impact of 80 in-lbs (9 Nm) with a 0.625-inch (15.9-mm) diameter tup. A holiday detector was utilized to verify that the coating had been disrupted and that bare metal was exposed. Next, the samples were placed into a pH 5, 3.5% NaCl solution for 30 days. Throughout the testing, periodic electrochemical impedance spectra were taken from each sample. Four replicates of both the control and microcapsule containing coatings were investigated. Electrochemical Impedance Spectroscopy. EIS testing was performed utilizing a PAR Model 273A Potentiostat in combination with a Solartron 1255 FRA and two PAR Model 314 Multiplexers. All experiments were conducted under software control via ZPlot (Scribner Associates, Inc.). Experiments were performed about a DC bias of 1.44 VSCE for the CD experiments, and about the open circuit potential for the impact-damaged samples. The perturbation frequency was scanned between 106 Hz and 1 mHz. A waveform of 25 mVRMS was used in all cases. RESULTS Cathodic Delamination Testing Cathodic delamination testing was performed for traditional FBE coated samples as well as for the microcapsule loaded coating. Four replicates of each coating were evaluated. Figure 5 illustrates the typical results for the two coatings. As can be seen in the figure, the delamination radius was reduced by 60% from 9.8mm (0.38 inches) for the traditional FBE to 4.2mm (0.17 inches) for the capsule loaded coating. There was very little variation among the four replicates of each coating. On an area basis, the delaminated area was reduced by 68%. Neither coating was discolored, blistered, or observably swelled after the 30-day experiment. Corrosion Initiation from a Damage Site To determine if the microencapsulated additions actually prevent the onset of corrosion, coated samples were damaged as discussed above and placed into a mildly acidic, high chloride solution. While in the bath, electrochemical impedance spectroscopy was used to qualitatively evaluate changes occurring at the damage site. Figures 6 and 7 present a comparison of impedance data for the conventional and modified FBE coatings. As is clearly evident in the figures, a second time constant is present in the case of the modified coating. This second time constant represents the newly sealed layer resulting from the ruptured microcapsules. Throughout the time of the test it can be seen that the polarization resistance of the modified FBE coating remained significantly higher than that of the conventional FBE coating. Based on this information, it may be inferred that the modified coating is providing increased protection compared to the standard FBE coating. To further demonstrate the ability of the modified coating to provide increased protection, samples were prepared as described above, then placed into a pH 5, aerated, 3.5 wt% NaCl solution at 60C (140F). Within a matter of hours, rust blooms were observed within the damage site for all conventional FBE coated samples. In the case of the modified FBE coated samples, no corrosion initiation was observed within the defect for two weeks. This is illustrated in Figures 8a and 8b. Note the minor attack visible on the modified FBE coating as compared to the severe attack visible on the conventional coating. After 6 weeks, more significant corrosion was visible on the

modified FBE coated sample. However, the corrosion of the conventionally coated sample was again more severe then the microcapsule containing, modified FBE coating. DISCUSSION/SUMMARY To summarize, a modified FBE coating has been presented which possesses an extraordinary self-healing ability. This self-healing characteristic is achieved through the use of microencapsulated additions that are positioned close to the metal/coating interface. In the particular example presented in this paper, the microcapsules are designed to rupture and release their protective fill when the FBE coating is subjected to mechanical damage. These protective fill materials may include corrosion inhibiting materials as well as sealants for the coating. As a result, a protective material is delivered to and held in place at the steel surface within a damage site. In addition, the damaged coating is sealed, and the protective nature of the coating is preserved. Experiments were conducted on coatings containing a wide variety of microcapsule types and fill materials. Preliminary results for one of the more promising combinations were presented above. As was discussed previously, electrochemical testing to determine if the microcapsules increase the corrosion resistance of a damaged coating revealed that the onset of corrosion was delayed considerably. In addition, in an industry standard cathodic disbondment test, a significant improvement in performance was observed. Other advantages of this technology revolve about the self-healing capability of these coatings in combination with other features that may be attained through the use of microencapsulated additions. For example, through the use of dye capsules, a coating could be produced that, in addition to possessing the self-healing capabilities described above, would positively indicate where damage occurred. This indicator would enable more efficient repair of damage areas via an appropriate patch material. In addition to aiding the patch process, the newly sealed layer formed by the ruptured microcapsules further enhances the performance of the patch, providing a more effective barrier to the external environment. Perhaps most important, though, is that the modified FBE coating will be able to effectively handle the abuse which current FBE experiences en route to and at the job site. The microcapsule containing coating also provides additional benefits when used in conjunction with a cathodic protection system. When such a system is utilized, one of the primary factors dictating operational cost and overall effectiveness is the total defect area present in the coating. As the total defect area increases, the amount of cathodic protection current required to protect those areas increases thus increasing the cost of operation. In addition, as the overall cathodic protection current increases, the effective throwing power of the CP system decreases, due to IR drop. In other words, a larger portion of the applied potential will be comprised of IR drop unless compensated, insufficient cathodic protection will be applied. Since the overall effect of the coating described above is to minimize the amount of damage experienced by the pipe, such a coating will also reduce the cost and help maintain the effectiveness of a cathodic protection system as well. In addition to the benefits described above, the modified FBE coating offers a number of advantages over similar corrosion prevention technologies. Although this approach appears to be simply the addition of corrosion inhibitors to a coating, it is much more than that. Corrosion inhibitors are added in such a way that very large concentrations (considerably more than could be added to a coating via conventional means) are delivered to the damage site, while very little of the material is wasted. This is in contrast to the typical procedures followed when using inhibitors. When protecting the internals of a pipe system, the use of chemical corrosion inhibitors requires that large quantities of inhibitor be added to the process stream to protect a relatively small amount of material (i.e., the entire stream must be treated, even though only that portion which is in contact with the steel needs to have inhibitor present the remainder is waste). In the case of external protection of the pipe, the use of inhibitors is typically not possible due to environmental concerns. The system above alleviates many of the problems of using inhibitors so, protection of the external surface of a pipe is possible, since the inhibitor is confined to the coating. By sealing the inhibitive materials in place at the damage site, there is no need to continuously augment the system with additional inhibitor. Another advantage of a modified FBE coating as presented above is its similarity in performance and handling to traditional FBE coatings. By maintaining a form that is handled in the same manner as conventional FBE coatings, no new technologies must be invested in and learned by applicators. The modified FBE coating may be applied via electrostatic spray or through a fluidized bed. The only change required is the addition of another

series of spray guns in the existing equipment (this assumes, of course, that a multi-layer coating is applied). Since the coating behaves identically to a conventional FBE coating, no new pipeline construction practices or procedures need be adopted.

CONCLUSIONS In conclusion, in this study a robust FBE coating has been designed through the application of microencapsulated additions. Upon being damaged in a manner that would compromise a conventional FBE, the microcapsules are ruptured, releasing their protective chemistry. As a result, the damaged FBE coating is healed, retaining much of the protective properties that it possessed prior to damage. The list below summarizes the benefits of this technology and its advantages: The modified FBE coating presented in this study possesses superior resistance to corrosion initiation in the damaged state compared to conventional FBE coatings. The modified FBE coating presented in this study possesses superior resistance to cathodic delamination compared to conventional FBE coatings. Unlike cathodic protection, increased maintenance requirements or expensive equipment that is subject to failure in the field does not accompany this increased resistance to corrosion. The overall effect of this coating is the reduction of defect area on a coated pipe. Since the cost to operate a CP system is a direct function of the defect area, this coating reduces operation costs associated with the use of a CP system. Implementation of this technology will be facilitated by the fact that the same technologies are used in its application. No new technologies must be mastered by coating applicators the modified FBE can be readily applied with existing equipment and methods.

ACKNOWLEDGEMENTS The authors gratefully acknowledge the technical support provided by Susan Weiland and Stephen Daniell in the 3M Corrosion Protection Products Department. REFERENCES 1. 2. 3. 4. 5. 6. 7. 8. Islam, Moavin, Condition Evaluation of Reinforced Concrete Structures: A Case Study, Paper No. 521, NACE National Corrosion Conference, Corrosion 95. Strobel, Rupert F., Fusion-Bonded Epoxy Coatings for Pipeline Corrosion Protection, 1981, 3M Company publication. Corrosion Control Report: Internal Pipe Coatings are a Wise Investment, Pipeline and Gas Journal, March 1993, pp. 67-69. Read, Thomas, Yates Field Crude Line Coated Internally, Externally, Pipeline and Gas Journal, February 1982. Carlson, Ron E., Jr., Internal Pipeline Corrosion Coatings Case Studies and Solutions Implemented, Paper No. 27, NACE 1992 Annual Corrosion Conference. Langford, Paul, Dr., New Developments in Coatings for the Internal Protection of Water Industry Line Pipe, unpublished, 1993. Norman, D., Gray, D., Fusion-Bonded Epoxy Pipe Coatings 10 Years Experience, Materials Performance, Vol. 32, No. 3 (1993), p.36. Standard test Methods for Cathodic Disbonding of Pipeline Coatings, ASTM Standard G8-96.

10

Figure 1: Micrograph of typical microcapsules containing a protective fill.

FBE

Damage
Steel

Self Healing

Newly Sealed Layer

Figure 2: Schematic illustrating the function of a single primer layer containing corrosion-preventative microencapsulated additions.

11

Damage
Steel

Damage Indicator

Self Healing, Indicating

Newly Sealed Layers

Figure 3: Schematic illustrating the function of a coating in which both the primer and top layer contain microencapsulated additions. By careful selection of the fill materials, the function of the top and bottom layers may be tailored (e.g., primer provides corrosion inhibiting materials, while the top layer provides materials which seal the damage site and possibly provide a visual indication of the damaged area. Figure 4: Schematic of electrochemical cell used for the testing and evaluation of the FBE coated plates (i.e., CD testing, impact testing, etc.).
CE RE Clamping System

Acrylic Cell Body

WE

Defect

O-Ring Seal Coated Sample

12

Figure 5: Typical cathodic disbondment results after 30 days in 1% sodium chloride + 1% sodium sulfate +1% sodium carbonate at room temperature with an applied potential of 1.44 VSCE for (a) unmodified FBE (9.2 mm) and (b) unmodified FBE with a 150 m (6 mil) primer layer containing 15 wt% microencapsulated additions (4.7 mm). Coating thickness was 350 m (14 mils) in both cases.

13

-70000

105

Magnitude

24 Hours pH 5, 3.5% NaCl

Scotchkote 413SG Modified FBE

104 103 102 10-3

Imaginary Impedance (Capacitive)

-55000

-40000

10-2

10-1

100

101

102

103

104

105

Frequency (Hz)
-25000 -90

Phase Angle

-65 -40 -15 10-3 10-2 10-1 100 101 102

Additional Time Constant

-10000

15000

30000

45000

60000

103

104

105

Real Impedance (Resistive)

Frequency (Hz)

Figure 6: Typical EIS spectra for an unmodified FBE and the microcapsule containing material after 24 hours. Note the presence of an additional time constant indicative of the inhibitor film in the case of the microcapsule containing material.

Scotchkote 413SG Modified FBE

-17500

105

Magnitude

Imaginary Impedance (Capacitive)

-15000

360 Hours pH 5, 3.5% NaCl

Scotchkote 413SG Modified FBE

104 103 102 101 10-3 10-2 10-1 100 101 102 103 104 105

-12500

-10000

Frequency (Hz)
-7500 -90 -5000

Phase Angle

-75 -60 -45 -30 -15 0 10-3 10-2 10-1 100 101 102 103 104 105

-2500

Additional Time Constant

2500

5000

7500

10000

12500

15000

17500

Real Impedance (Resistive)

Frequency (Hz)

Scotchkote 413SG Figure 7: Typical EIS spectra for an unmodified FBE and the microcapsule containing material after 360 hours. Modified FBE Note that the additional time constant is still present for the microcapsule containing material, illustrating its persistence.

14

Figure 8: Typical results for impact damaged coatings exposed in 60C (140F), pH 5, 3.5% NaCl solution for (a) an unmodified FBE and (b) a coating containing the microencapsulated materials. The microcapsules dramatically increased the time to corrosion initiation in this qualitative test (from 4 hours to nearly two weeks).

Severe corrosion initiation

Minor corrosion initiation

15