Powder Coating as an Environmentally Acceptable Alternate to the System of MIL-P and MIL-PRF-22750

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Powder Coating as an Environmentally Acceptable Alternate to the System of MIL-P-53022 and MIL-PRF-22750 by Jeffrey L. Duncan ARL-TR-2965 May 2003 Approved for public release; distribution is unlimited.

NOTICES Disclaimers The findings in this report are not to be construed as an official Department of the Army position unless so designated by other authorized documents. Citation of manufacturer s or trade names does not constitute an official endorsement or approval of the use thereof. Destroy this report when it is no longer needed. Do not return it to the originator.

Army Research Laboratory Aberdeen Proving Ground, MD 21005-5069 ARL-TR-2965 May 2003 Powder Coating as an Environmentally Acceptable Alternate to the System of MIL-P-53022 and MIL-PRF-22750 Jeffrey L. Duncan Weapons and Materials Research Directorate, ARL Approved for public release; distribution is unlimited.

Report Documentation Page Form Approved OMB No. 0704-0188 Public reporting burden for this collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection information. Send comments regarding this burden estimate or any other aspect of this collection of information, including suggestions for reducing the burden, to Department of Defense, Washington Headquarters Services, Directorate for Information Operations and Reports (0704-0188), 1215 Jefferson Davis Highway, Suite 1204, Arlington, VA 22202-4302. Respondents should be aware that notwithstanding any other provision of law, no person shall be subject to any penalty for failing to comply with a collection of information if it does not display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. 1. REPORT DATE (DD-MM-YYYY) May 2003 2. REPORT TYPE Final 4. TITLE AND SUBTITLE Powder Coating as an Environmentally Acceptable Alternate to the System of MIL-P-53022 and MIL-PRF-22750 3. DATES COVERED (From - To) May 2001 - January 2002 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Jeffrey L. Duncan 5d. PROJECT NUMBER AH84 5e. TASK NUMBER 5f. WORK UNIT NUMBER 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) U.S. Army Research Laboratory ATTN: AMSRL-WM-MA Aberdeen Proving Ground, MD 21005-5069 9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES) Albany Marine Corps Logistics Base, Maintenance Center ATTN: Engineering Dept., Code 882 (Mr. Steve Allen) 814 Radford Blvd., Ste. 20325 Albany, GA 31704-0325 12. DISTRIBUTION/AVAILABILITY STATEMENT Approved for public release; distribution is unlimited. 8. PERFORMING ORGANIZATION REPORT NUMBER ARL-TR-2965 10. SPONSOR/MONITOR'S ACRONYM(S) 11. SPONSOR/MONITOR'S REPORT NUMBER(S) 13. SUPPLEMENTARY NOTES 14. ABSTRACT Powder coatings offer potential performance and environmental benefits over conventional, solvent-based protective coatings. At the request of the Albany Marine Corps Logistics Base (MCLB), three powder coatings were evaluated as performancebased alternatives to the military specification coatings normally used on combat vehicles. Specimen panels, to which the powder coatings had been applied, were subjected to a selection of performance tests from MIL-P-53022, an epoxy primer specification, and from MIL-PRF-22750, an epoxy topcoat specification. These products are part of the U.S. Army s Chemical Agent Resistant Coating (CARC) system and are applied to all Army and Marine Corps tactical equipment. These substrates, 1020 steel with zinc phosphate pretreatment, bare aluminum, and aluminum with chromate conversion coating, were submitted, representing the materials from which vehicles are constructed. Coupled with the three powder coatings, that led to nine possible combinations of substrate and powder coating. With the exception of one minor problem, probably associated with substrate pretreatment rather than coating performance, all three powder coatings performed well, and the U.S. Army Research Laboratory believes they are acceptable for use at Albany MCLB as alternatives to the CARC specifications normally used. 15. SUBJECT TERMS CARC, powder coating, Albany MCLB, experimental products program, EPP 16. SECURITY CLASSIFICATION OF: a. REPORT UNCLASSIFIED b. ABSTRACT UNCLASSIFIED c. THIS PAGE UNCLASSIFIED 17. LIMITATION OF ABSTRACT UL 18. NUMBER OF PAGES 16 19a. NAME OF RESPONSIBLE PERSON Jeffrey L. Duncan 19b. TELEPHONE NUMBER (Include area code) 410-306-0690 Standard Form 298 (Rev. 8/98) Prescribed by ANSI Std. Z39.18 ii

Contents List of Figures List of Tables iv iv 1. Background 1 2. Objective 1 3. Approach 1 4. Results 4 5. Discussion 6 6. Conclusions 7 7. References 7 Appendix. Photographs of Test Panels 9 iii

List of Figures Figure 1. Test panel locations where film thickness was measured....3 Figure A-1. Salt fog steel substrate...9 Figure A-2. Recoatability...10 Figure A-3. Flexibility green no. 24533 on steel...10 Figure A-4. Flexibility all coatings on aluminum...10 List of Tables Table 1. Coatings and substrates...2 Table 2. Summary of tests and corresponding performance requirements...3 Table 3. Results for white no. 17925....4 Table 4. Results for green no. 24533....5 Table 5. Results for black no. 17038....5 iv

1. Background In late 2000, Albany Marine Corps Logistics Base (MCLB) personnel contacted the Coatings Technology Team, Weapons and Materials Research Directorate, U.S. Army Research Laboratory (ARL) about a test program designed to approve the use of epoxy powder coatings as replacements for the standard chemical agent resistant coating (CARC) system used on tactical equipment, because ARL is the CARC Commodity Manager and the CARC approving authority for the Department of Defense. The powder coatings were to be used on a variety of equipment to replace the military specification MIL-P-53022 (1) epoxy primer and MIL-PRF-22750 (2) epoxy topcoat as applied to bare and pretreated aluminum and zinc phosphate pretreated steel. Normally, substitutions are for cases where those specifications do not meet volatile organic compounds (VOC) regulations in force or where new technology will provide more general benefits in the future or a more environmentally acceptable process for the user. Although these specification coatings are available in low-voc formulations, the environmental benefits (zero VOC) and performance enhancements of powder coatings are well documented. The proposed test program and approval process fell under the auspices of ARL s Experimental Products Program (EPP), which is set up to evaluate performance alternatives to military specification finishing systems. After discussions to set the number and type of panels required, panels were submitted for three powder coatings on three different substrates. 2. Objective The test program was designed to evaluate epoxy powder coatings as performance-based alternatives to the system of epoxy primer MIL-P-53022 and epoxy topcoat MIL-PRF-22750 on the substrates noted in section 1. As part of a military tactical system, the parts must have CARC as the finishing system, and for interior components this typically includes a requirement for the previously mentioned specifications. For exterior use, the powder would replace only the primer. The powder coating needed to perform as well as or better than the system it was to replace. 3. Approach A set of laboratory tests was assembled to evaluate the performance of the epoxy powders as a primer or as a combination of the primer and epoxy topcoat CARC system. While the corrosion resistance test requirement for salt fog exposure in MIL-P-53022 is 336 hr, the standard used in 1

the EPP is 1000 hr, the same as for MIL-P-53084 (3), a lead and chromate free electrodeposition epoxy primer developed by the Coatings Technology Team. That material and its thermal curing process provide a much more appropriate performance standard for the powder coating process under consideration in this case. The supplied test panels represented the nine possible substrate/pretreatment/powder coating combinations envisioned by Albany MCLB and included the three substrates in combination with three powder coatings from the Sherwin-Williams Co. (Sherwin-Williams) as noted in Table 1. The white color is typical of epoxy primers in the CARC system, and the green and black colors are commonly used on interior surfaces of tactical equipment. Table 1. Coatings and substrates. Powder Coatings Sherwin-Williams EWS8-9004 white no. 17925 Sherwin-Williams EGS2-9007 green no. 24533 Sherwin-Williams EBS8-9003 black no. 17038 Substrates 1020 steel with zinc phosphate pretreatment Bare aluminum Aluminum with chromate conversion coating The tests normally performed in a powder coating EPP study such as this one are extracted from the primer and topcoat specifications as appropriate. They are selected as laboratory simulations of conditions that the tactical equipment is anticipated to encounter in the field, such as exposure to rain, gasoline, acid rain, oil, and hydraulic fluid. However, the ultimate (and military unique) tests are the chemical agent resistance and resistance of the coating to Decontaminating Solution No. 2 (DS2). Tests run in this program and their corresponding performance requirements are summarized in Table 2. The topcoating test was modified slightly from that specified in no. 12 in Table 2, in that the panels were topcoated with MIL-C-53039 (4) and MIL-DTL-64159 (5), Type II. After curing, they were tested by crosshatch adhesion (American Society for Testing and Materials [ASTM] Standard D 3359 (6), Method B) and by wet tape adhesion after immersion for 24 hr in deionized water (FED-STD-141 (7), Method 6301). Due to the thickness of the supplied test panels, the mandrel flexibility test could not be performed, so the conical mandrel test in accordance with ASTM D 522 (8), Method A was used instead to evaluate adhesion of the powder coatings to the substrates. Prior to any testing, the dry film thickness of the powder coatings was measured. The six steel panels provided for the salt fog test were used, and eight measurements were made on each, following the pattern on Figure 1 and making a total of 48 test points for each color. The electronic film thickness gauge calculated the film thickness as follows: for the white no. 17925, the low reading was 2.05 mil, the high reading was 3.41 mil, and the average was 2.52 ± 0.25 mil; for the green no. 24533, the low reading was 1.85 mil, the high reading was 3.20 mil, and the average was 2.54 ± 0.29 mil; and for the black no. 17038, the low reading was 1.91 mil, the high reading was 3.20 mil, and the average was 2.44 ± 0.29 mil. 2

Table 2. Summary of tests and corresponding performance requirements. Test No. Test Reference Procedure Requirement 1 Chemical agent resistance MIL-C-46168 (9), para 4.3.25 expose 5-cm 2 area for 1/2 hr 40 µg of nerve agent GD and 180 µg of mustard agent HD desorbed 2 Water resistance 3 Hydrocarbon resistance 4 Lube oil resistance 5 Hydraulic fluid resistance MIL-P-53022, para 4.14 MIL-P-53022, para 4.15 MIL-PRF-22750, para 4.6.3 MIL-PRF-22750, para 4.6.3 6 DS2 resistance MIL-C-46168, para 4.3.24 7 Acid MIL-C-46168, resistance para 4.3.21 8 Color FED-STD-595 (10) 9 Gloss ASTM D 523 (60 and 85 ) (11) immerse in water at 23 ± 1 C (77 ± 1 F) for 168 hr immerse in hydrocarbon fluid at 23 ± 1 C (77 ± 1 F) for 168 hr immerse in lube oil at 121 ± 3 C (250 ± 5 F) for 168 hr immerse in hydraulic fluid at 65.5 ± 3 C (150 ± 5 F) for 168 hr expose to DS2 for 1/2 hr expose to 10% acetic acid for 1 hr compare to standard color chip instrumental measurement initial defects, indistinguishable after 2 hr from unexposed film minor initial defects, indistinguishable after 24 hr from unexposed film no defects after 4-hr recovery no defects after 4-hr recovery no blistering, wrinkling, or film softening, E NBS 2.5 units no blistering and no change from the original color visual match color dependent 10 Crosshatch ASTM D 3359 see ASTM 3359 rating 4B or better adhesion 11 Flexibility MIL-P-53022, 1/4-in mandrel bend no cracking or flaking para 4.13 12 Intercoat adhesion MIL-P-53022, para 4.17 apply CARC topcoat no attack on primer, difficult to remove 13 Salt fog resistance ASTM B 117 (12) 1000-hr exposure to ASTM B 117 method no more than 5 scattered blisters 1 mm in diameter Figure 1. Test panel locations where film thickness was measured. 3

While most measurements fell within a typical range of 2 3.5 mil, several had either thinner or thicker films. Where film thickness was an important factor in a test (i.e., flexibility), every effort was made to use a panel with the typical (assumed to be production) film thickness. Where film thickness was not as important (e.g., DS2 or acid resistance), the most appropriate panel was selected. 4. Results Test results are summarized in Tables 3 5. In general, the resistance testing was satisfactory, but there were minor problems with flexibility. Photographs of some of the test panels are included in the Appendix. Table 3. Results for white no. 17925. Test Substrate Pretreated Steel Bare Aluminum Pretreated Aluminum Color no. 17925 Pass a Gloss (60 /85 ) 97.5 / 96.4 b Flexibility Pass Pass Pass Crosshatch adhesion Pass (5B) Pass (4B) Pass (5B) Acid resistance Pass Pass Pass Water resistance Pass Pass Pass Hydrocarbon resistance Pass Pass Pass Lube oil resistance Pass Pass Pass Hydraulic fluid resistance Pass Pass Pass DS2 resistance Pass Pass Pass Chemical agent resistance Pass Intercoat dry adhesion (53039) Pass (5B) Intercoat dry adhesion (64159) Pass (4B) Intercoat wet adhesion (53039) Pass Intercoat wet adhesion (64159) Pass Salt fog scored Pass Pass Pass Salt fog unscored Pass Pass Pass a Customer decision on acceptability; however, good visual match, and instrumentally determined as E NBS ~0.5 units when compared to the FED-STD-595, color no. 17925 chip. b Customer decision on acceptability. 4

Table 4. Results for green no. 24533. Test Substrate Pretreated Steel Bare Aluminum Pretreated Aluminum Color no. 24533 Pass a Gloss (60 /85 ) 21.6/49.6 b Flexibility Pass c Pass Pass Crosshatch adhesion Pass (5B) Pass (5B) Pass (5B) Acid resistance Pass Pass Pass Water resistance Pass Pass Pass Hydrocarbon resistance Pass Pass Pass Lube oil resistance Pass Pass Pass Hydraulic fluid resistance Pass Pass Pass DS2 resistance Pass Pass Pass Chemical agent resistance Pass Intercoat dry adhesion (53039) Pass (5B) Intercoat dry adhesion (64159) Pass (4B) Intercoat wet adhesion (53039) Pass Intercoat wet adhesion (64159) Pass Salt fog scored Pass Pass Pass Salt fog unscored Pass Pass Pass a Customer decision on acceptability; however, good visual match, and instrumentally determined as E NBS ~1.75 units when compared to the FED-STD-595, color no. 24533 chip. b Customer decision on acceptability. c Some delamination at small radius bend (see section 5; Figure A-3). Table 5. Results for black no. 17038. Test Substrate Pretreated Steel Bare Aluminum Pretreated Aluminum Color no. 17038 Pass a Gloss (60 /85 ) 97.3/96.2 b Flexibility Pass Pass Pass Crosshatch adhesion Pass (5B) Pass (4B) Pass (5B) Acid resistance Pass Pass Pass Water resistance Pass Pass Pass Hydrocarbon resistance Pass Pass Pass Lube oil resistance Pass Pass Pass Hydraulic fluid resistance Pass Pass Pass DS2 resistance Pass Pass Pass Chemical agent resistance Pass Intercoat dry adhesion (53039) Pass (5B) Intercoat dry adhesion (64159) Pass (4B) Intercoat wet adhesion (53039) Pass Intercoat wet adhesion (64159) Pass Salt fog scored Pass Pass Pass Salt fog unscored Pass Pass Pass a Customer decision on acceptability; however, good visual match, and instrumentally determined as E NBS ~1.79 units when compared to the FED-STD-595, color no. 17038 chip. b Customer decision on acceptability. 5

5. Discussion The ultimate criterion for a CARC substitute is its chemical agent resistance, and the results from the U.S. Army Edgewood Chemical and Biological Center for all three powder coatings were excellent with readings of less than 10-µg HD (mustard agent) on each test panel. The test for GD (nerve agent) is under revision and was not run. All three also showed acceptable resistance to DS2 exposure, with minimal color changes and no softening, indicating that decontamination of surfaces exposed to chemical warfare agents would not adversely affect the materials. Adhesion of each powder coating to the three substrates was excellent. The purpose of the topcoating (intercoat adhesion) test, with the subsequent crosshatch and wet tape adhesion tests, was to validate the ability to topcoat the powder used as a primer or to repair or rework powder coated items later. Even at the high gloss levels obtained for the white and black submissions, the results were excellent. Resistance to exposure to water, acid, hydrocarbon fluid, hydraulic fluid, and lubricating oil was excellent, typical of a quality epoxy coating. All three of the powder coatings performed very well in the corrosion resistance (salt fog) test. The aluminum substrate had little score corrosion and only a few defects elsewhere after 1008-hr exposure. The steel exhibited some score corrosion, but with minimal undercutting, and also had few defects elsewhere. As previously indicated, the thickness of the test panels precluded using the mandrel flexibility test method specified in MIL-P-53022 and normally used in powder coating EPP testing. Instead, the conical mandrel flexibility test (ASTM D 522, Method A) was used. The only defect noted was for the sea foam green color on the pretreated steel substrate. There, delamination was noted for a diameter up to ~1/2 in. The test was performed on three different panels with dry film thicknesses of ~1.53, 2.25, and 3.09 mil. Since the flexibility was acceptable for the other two substrates, the problem likely lies with the surface preparation and not with the powder coating. However, this would indicate that the pretreatment process and the dry film thickness must be closely monitored until satisfactory flexibility is obtained. Visual appearance and instrumental determination of color difference between the samples and the FED-STD-595 samples were acceptable, but color acceptability is usually a customer decision. Also, as previously indicated, while all three colors performed well in the corrosion resistance test and would therefore perform acceptably as primers, when a CARC topcoat is applied, the infrared reflectance of the system could be affected and the camouflage properties compromised by the black or sea foam green colors, and solar heat loading could be increased. 6

6. Conclusions The only problem noted in this study was the delamination noted during the flexibility test for the sea foam green color on the pretreated steel substrate. Since this is likely a pretreatment problem rather than a problem with the powder coating, ARL believes that all three Sherwin- Williams products tested in this project are acceptable for use as substitutes in the CARC system. It is, of course, the user s responsibility to monitor the surface preparation, application, and curing processes to ensure satisfactory results in a production environment. The three powder coatings are Sherwin-Williams product EWS8-9004 white no. 17925, EGS2-9007 sea foam green no. 24533, and EBS8-9003 black no. 17038. 7. References 1. MIL-P-53022. Primer, Epoxy Coating, Corrosion Inhibiting, Lead and Chromate Free 1988. 2. MIL-PRF-22750. Coating, Epoxy, High-Solids 1994. 3. MIL-P-53084. Primer, Cathodic Electrodeposition, Chemical Agent Resistant 1994. 4. MIL-C-53039. Coating, Aliphatic Polyurethane, Single Component, Chemical Agent Resistant 1993. 5. MIL-DTL-64159. Coating, Water Dispersible Aliphatic Polyurethane, Chemical Agent Resistant 2002. 6. ASTM D 3359. Standard Test Methods for Measuring Adhesion by Tape Test. Annu. Book ASTM Stand. 2002. 7. FED-STD-141. Paint, Varnish, Lacquer, and Related Materials: Methods of Inspection, Sampling, and Testing 2001. 8. ASTM D 522. Standard Test Methods for Mandrel Bend Test of Attached Organic Coatings. Annu. Book ASTM Stand. 2001. 9. MIL-C-46168. Coating, Aliphatic Polyurethane, Chemical Agent Resistant 1993. 10. FED-STD-595. Colors Used in Government Procurement 1994. 11. ASTM D 523. Standard Test Method for Specular Gloss. Annu. Book ASTM Stand. 1999. 7

12. ASTM B 117. Standard Practice for Operating Salt Spray (Fog) Apparatus. Annu. Book ASTM Stand. 2002. 8

Appendix. Photographs of Test Panels Figure A-1. Salt fog steel substrate. 9

Figure A-2. Recoatability. Figure A-3. Flexibility green no. 24533 on steel. Figure A-4. Flexibility all coatings on aluminum. 10

NO. OF NO. OF COPIES ORGANIZATION COPIES ORGANIZATION 2 DEFENSE TECHNICAL INFORMATION CENTER DTIC OCA 8725 JOHN J KINGMAN RD STE 0944 FT BELVOIR VA 22060-6218 ABERDEEN PROVING GROUND 2 DIR USARL AMSRL CI LP (BLDG 305) 1 COMMANDING GENERAL US ARMY MATERIEL CMD AMCRDA TF 5001 EISENHOWER AVE ALEXANDRIA VA 22333-0001 1 INST FOR ADVNCD TCHNLGY THE UNIV OF TEXAS AT AUSTIN 3925 W BRAKER LN STE 400 AUSTIN TX 78759-5316 1 US MILITARY ACADEMY MATH SCI CTR EXCELLENCE MADN MATH THAYER HALL WEST POINT NY 10996-1786 1 DIRECTOR US ARMY RESEARCH LAB AMSRL D DR D SMITH 2800 POWDER MILL RD ADELPHI MD 20783-1197 1 DIRECTOR US ARMY RESEARCH LAB AMSRL CS IS R 2800 POWDER MILL RD ADELPHI MD 20783-1197 3 DIRECTOR US ARMY RESEARCH LAB AMSRL CI OK TL 2800 POWDER MILL RD ADELPHI MD 20783-1197 3 DIRECTOR US ARMY RESEARCH LAB AMSRL CS IS T 2800 POWDER MILL RD ADELPHI MD 20783-1197 1

NO. OF COPIES ORGANIZATION ABERDEEN PROVING GROUND 10 DIR USARL AMSRL WM MA J DUNCAN 2