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SCIENTIFIC AND TECHNICAL INFORMATION
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Final Report
Army Ordnance Contract DA-ll-022-509-ORD-3070
ORD Project TB4-006D
Development of a Finishing System
for Lightweight Metals
"by Richard W. ClopeHarold M. Blairn
James M. Williard
Milton A. Glaser
L.%dt1,,strial Finishes Company
Illinois
Ail1/, 1.963
List of Figures
Page
1. Mounting of Bimetallic Corrosion Test Panels. 135
2. Bimetallic Corrosion Test Cell. 136
3. Panels Not Tested Due to Cracking of Topcoat. 138
4. Typical Galvanic Corrosion Failures. 140
5. Galvanic Corrosion Testing of Primers Containing 141Extender Pigments.
6. Typical 5% Salt Spray Test Results. 150
7. Examples of Good and Poor Adhesion. 157
8. Effect of Pigment Content on Galvanic Corrosion Resistance 188of a Silicone-Epoxy: Polyamid Primer.
9. Galvanic Corrosion Testing of Coating Systems Using 234Specification Primers.
10. Effect of Addition of Inert Pigment to Primers of 254Preferred Coating Systems.
11. 5% Salt Spray Results (on Magnesium-Steel Coupled Panels) 323of Olive Drab Coating System without and with Protectionof Lapped Area.
12. 5% Salt Spray Results (on Magnesium-Steel Coupled Panels) 324of White Coating System without and with Protection ofLapped Area.
List of Tables
page
1. Key to Numerical Ratings and Symbols in Vehicle 8
Screening Tables.
2. Half Second RS Nitrocellulose Modification of Silicone 11-13
Resins.
3. Half Second SS Nitrocellulose Modification of Silicone 15-17
Resins.
4. Half Second Cellulose Acetate Butyrate Modification of 20-22
Silicone Resins.
5. Acrylic (Acryloid A-101) Modification of Silicone Resins. 24-26
6. Polyvinyl Butyral (Bakelite XYHL) Modification of 29-31
Silicone Resins.
7. Styrene Butadiene (Goodyear Pliolite S-5) Modification of 33-35
Silicone Resins.
8. Triazine Formaldehyde (Rohm and Haas Uformite M-311) 38-40
Modification of Silicone Resins.
9. Polyvinyl Formal (Shawinigan Formvar 7/70) Modification 42-44
of Silicone Resins.
10. Modified Alkyd (Hercules Petrex SS) Modification of 47-49
Silicone Resins.
11. Epoxy Ester (Midland R-55) Modification of Silicone Resins. 51-54
12. Oxidizing Alkyd (Midland R-9) Modification of Silicone 57-59
Resins.
13. Oxidizing Alkyd (Midland R-50) Modification of Silicone 61-63
Resins.
14. phenolic (Bakelite BRS-2600) Modification of Silicone 66-68
Resins.
page
15. Butadiene Acrylonitrile (Naugatuck Paracril CV) 70-72
Modification of Silicone Resins.
16. Natural Fossil Resin (RDH 510) Modification of Silicone 75-77
Resins.
17. Epoxy-Polyamide (General Hills Versamid 100) Resin Systems. 8114
18. Epoxy-Polyamide (General Mills Versamid 115) Resin Systems. 83
19. Epoxy-Polyamide (General Hills Versamid 125) Resin Systems. 85
20. Epoxy-Polyamide (General Mills Versamid 140) Resin Systems. 87
21. Epoxy-Polyamide (General Mills Genamid 250) Resin Systems. 89
22. Epoxy-Polyamide (General Hills Genamid 310) Resina System~s. 91
23. Epoxy-Polyamide (Ciba Lancast A) Resin Systems. 93
24. Epoxy-Amino Silane (Dow Corning Z-6020) Resin Systems. 95
25. Epoxy Novolac (Dow Chemical 2638.1 and 2638.3) Resin 97-98
Systems.
26. Epoxy-Moisture Activated Catalyst (Shell H-1 and H-2) 100-101
Systems.
27. Experimental Silazane (#2311) Catalyzed Silicone Resins. 104-106
28. Amino Silane (Dow Corning Z-6020) Catalyzed Silicone 108-109
Resins.
29. Half Second RS Nitrocellulose Modification of Fluorinated 112
Hydrocarbon Resins.
30. Polyvinyl Butyral (Bakelite XYHL) Modification of 114
Fluorinated Hydrocarbon Resins.
31. Acrylic (Acryloid A-101) Modification of Fluorinated 117
Hydrocarbon Resins.
32. Styrene Butadiene (Goodyear Pliolite S-5) Modification 119
of Fluorinated Hydrocarbon Resins.
page
33. Triazine Formaldehyde (Rohn and Haas Uformite M-311) 122
Modification d Fluorinated Hydrocarbon Resins.
34. Polyvinyl Formal (Shawinigan Foravar 7/70) Modification 124
of Fluorinated Hydrocarbon Resins.
35. Miscellaneous Resin Systems. 127-129
36. Bimetallic Corrosion Rating System. 137
37. Bimetallic Corrosion Testing of Primers. 142-144
38. Bimetallic Corrosion Testing of Primers Containing 146-147
Extender Pigments.
39. 5% Salt Spray Testing of Primers. 151-153
40. 5% Salt Spray Testing of Primers Containing Extender 154
Pigments.
41. Adhesion Rating System. 158
42. Bimetallic Corrosion Testingof Olive Drab Coating Systems. 159-161
43. 57. Salt Spray Testing of Olive Drab Coating Systems. 163-165
44. Bimetallic Corrosion Testing of White Coating Systems. 169-170
45. 57. Salt Spray Testing of White Coating Systems. 172-173
46. Screening Epoxy Ester Resins. 178-183
47. Effect of Pigment Content in Midland R-55: Plaskon ST-847 185
Primer on Bimetallic Corrosion Resistance.
48. Effect of Pigment Content in Midland R-55: Plaskon ST-847 187
Primer on 5% Salt Spray Performance.
49. Bimetallic Corrosion Testing of Epoxy Ester Primers. 191-192
50. 5. Salt Spray Testing of Epoxy Ester Primers. 194-196
51. Bimetallic Corrosion Testing of Epoxy Ester Olive Drab 198-199
Topcoats.
EL IIiIIIi
w
Page
52. 5% Salt Spray Testing of Epoxy Ester Olive Drab Topcoats. 201-202
53. Bimetallic Corrosion Testing of Epoxy Ester White 205
Topcoats.
54. 5% Salt Spray Testing of Epoxy Ester White Topcoats. 207
55. Screening Silicone-Epoxy Copolymer Systems. 210-211
56. Bimetallic Corrosion Testing of Epoxy and Silicone-Epoxy 213-214
Primers.
57. 5% Salt Spray Testing of Epoxy and Silicone-Epoxy Primers. 216-217
58. Bimetallic Corrosion Testing of Epoxy and Silicone-Epoxy 219
Olive Drab Topcoats.
59. 5% Sait Spray Testing of Epoxy and Silicone-Epoxy Olive 221-222
Drab Topcoats.
60. Bimetallic Corrosion Testing of Epoxy and Silicone-Epoxy 224
White Topcoats.
61. 5% Salt Spray Testing of Epoxy and Silicone-Epoxy White 226-227
Topcoats.
62. Bimetallic Corrosion Testing of Olive Drab Coating Systems 230
Using Conventional Primers.
63. 5% Salt Spray Testing of Olive Drab Coating Systems 232
Using Conventional Primers.
64. Bimetallic Corrosion Testing of Molybdate Primers. 236-237
65. 5% Salt Spray Testing of Molybdate Primers. 239-240
66. Bimetallic Corrosion Testing of Coating Systems Using 243
Molybdate Primers.
67. 5% Salt Spray Testing of Coating Systems Using Molybdate 245
Primers.
J L i l i I I I I I
68. Bimetallic Corrosion Ttsting of Coating Systems Using 248-249
Primers Containing Extender Pigments.
69. 5% Salt Spray Testing of Coating Systems Using Primers 251-252
Containing Extender Pigments.
70. Effect of Tributyl Tin Oxide on Bimetallic Corrosion. 255
71. 5% Salt Spray Testing of Primers Containing Tributyl 257
Tin Oxide.
72. Bimetallic Corrosion Testing of Coating Systems Using 260-262
Previously Eliminated Primers.
73. 5% Salt Spray Testing of Coating Systems Using Previously 264-266
Eliminated Primers.
74. Bimetallic Coirosion Testing of Primers Using Miscellaneous 270
Vehicles.
75. 5% Salt Spray Testing of Primers Using Miscellaneous 272
Vehicles.
76. Bimetallic Corrosion Testing of Reformulated Olive Drab 276-277
Topcoats.
77. Bimetallic Corrosion Testing of Miscellaneous Olive Drab 283
Topcoats.
78. Symbols Representing Pigments. 286
79. Bimetallic Corrosion Testing of Topcoats Containing 288-291
Various White Pigments.
80. Bimetallic Corrosion Testing of White Topcoats Containing 293
Same Vehicles as Best Olive Drab Topcoats.
Page81. 5% Salt Spray Testing of White Topcoats Containing Same 295
Vehicles as Best Olive Drab Topcoats.
82. Bimetallic Corrosion Testing of White Topcoats Containing 298-299
Various Extender Pigments.
83. 5. Salt Spray Testing of 4hite Topcoats Containing Various 301
Extender Pigments.
84. Bimetallic Corrosion Testing of White Topcoats Containing 304
Chromate and Aluminum Pigments.
85. Bimetallic Corrosion Testing of White Topcoats with Same 307
PVC as Olive Drab Topcoats.
86. Bimetallic Corrosion Testing of Previously Eliminated 309-313
White Topcoats.
87. Bimetallic Corrosion Testing of White Topcoats Using 316
Miscellaneous Vehicles.
88. Final Testing of Preferred Coating Systems. 326
89. Screening of Vinyl Resin Systems. 329
90. Screening of Epoxy-Polyurethane Systems. 331-332
91. Screening of Silicone-Polyesters Catalyzed with 335-336
Polyurethane.
92. Screening of Miscellaneous Materials. 339-341
93. Bimetallic Corrosion Testing of Primers and Clear 343-346
Coatings.
94. 5% Salt Spray Testing of Primers and Clear Coatings. 349
95. Bimetallic Corrosion Testing of Miscellaneous Primers. 350
Page
96. Bimetallic Cor:osion Testing of O.1ive Drab Topcoats. 353
97. Bimetallic Corrosion Testing of White Topcoats. 355
98. Bimetallic Salt Spray Testing of White Coating Systems. 357
i
Table of Contents
Pae
Section I Introduction 1
Section II Initial Screening of Clear Films. 3
Section III Results of Screening Clear Coatings. 10
A. Half Second Nitrocellulose Modification of Silicone 10
Resins.
B. Half Second Cellulose Acetate Butyrate Modification 19
of Silicone Resins.
C. Acrylic (Rohm and Haas Acryloid A-101) Modification 19
of Silicone Resins.
D. Polyvinyl Butyral (Bakelite XYHL) Modification of 28
Silicone Resins.
E. Styrene Butadiene (Goodyear Pliolite 5-5) 28
Modification of Silicone Resins.
F. Triazine Formaldehyde (Robin and Haas Uformite M-311) 37
Modification of Silicone Resins.
G. Polyvinyl Formal (Shawinigan Formvar 7/70) 37
Modification of Silicone Resins.
H. Modified Alkyd (Hercules Petrex SS) Modification of 46
Silicone Resins.
I. Epoxy Ester (Midland R-55) Modification of Silicone 46
Resins.
j. Oxidizing Alkyd (Midland R-9) Modification of 56
Silicone Resins.
ii
page
K. Oxidizing Alkyd (Midland R-50) Modification of 56
Silicone Resins.
L. Phenolic (Bakelite BRS-2600) Modification of 65
Silicone Resins.
M. Butadiene Acrylonitrile (Naugatuck Paracril CV) 65
Modification of Silicone Resins.
N. Natural Fossil Resin (RBH 510) Modification of 74
Silicone Resins.
0. Epoxy Resin Systems. 79
P. Silicone Resins Cured with #2311 Experimental Silazane. 103
Q. Silicone Resins Cured with Dow Corning Z-6020 Amino 103
Silane.
1. Half Second RS Nitrocellulose Modification of 111
Fluorinated Hydrocarbon Resins.
S. Polyvinyl Butyral (Bakelite XYHL) Modification of 111
Fluorinated Hydrocarbon Resins.
T. Acrylic (Rohm and Bass Acryloid A-101) Modification 116
of Fluorinated Hydrocarbon Resins.
U. Styrene Butadiene (Goodyear Pliolite S-5) Modification 116
of Fluorinated Hydrocarbon Resins.
V. Triazine Formaldehyde (Rohm and Haas Uformite M-311) 121
Modification of Fluorinated Hydrocarbon Resins.
W. Polyvinyl Formal (Shawinigan Formvar 7/70) 121
Modification of Fluorinated Hydrocarbon Resins.
X. Miscellaneous Resins Sytems. 126
iii
Page
Section IV Development of Primer
A. Initial Vehicles Used. 131
B. Pigments Used. 133
C. Bimetallic Corrosion Testing. 134
D. Results of Bimetallic Corrosion Testing. 139
E. Addition of Inert Pigments to Primers. 139
F. Salt Spray Exposure of Primers. 149
Section V Development of Olive Drab Topcoat
A. Initial Vehicles Used. 155
B. Pigmentation 155
C. Preparation of Panels. 156
D. Bimetallic Corrosion and Salt Spray Testing. 156
Section VI Development of White Topcoat
A. Initial Vehicles Used. 167
B. Pigmentation 167
C. Preparation of Panels. 167
D. Bimetallic Corrosion and Salt Spray Testing. 167
Section VII Epoxy Ester and Silicone-Epoxy Ester Coatings
A. 301-103-A Primer 175
B. Preparation and Testing of New Vehicles. 176
C. Screening Clear Resins. 177
D. Epoxy Ester Primers. 177
E. Epoxy Ester Olive Drab Topcoats. 197
F. Epoxy Ester White Topcoats. 204
Page
Section VIII Epoxy and Silicone-Epoxy Copolymer Coatings
A. Preparation and Testing of New Vehicles. 209
B. Screening of Clear Resins. 209
C. Epoxy and Silicone-Epoxy Primers. 209
D. Epoxy and Silicone-Epoxy Olive Drab Topcoats. 218
E. Epoxy and Silicone-Epoxy Wt~ite Topcoats. 216
Section IX Miscellaneous Primer Work
A. Conventional Primers. 229
B. Primers Containing Molybdate Pigments. 235
C. Comparison of Zinc Chromate Pigments from Various 241
Suppliers.
D. Effect of Extender Pigments on Primer Performance. 246
E. Effect of Tributyl Tin Oxide on Galvanic Cortosion 247
Resistance.
F. Evaluation of Previously Eliminated Primers. 258
G. Primers Containing Miscellaneous Vehicles. 268
H. Reformulation of 301-131-B Primer. 268
Section X Miscellaneous Olive Drab Topcoat Work
A. Reformulation of Olive Drab Topcoats to Match 273
Color #X-24087.
B. Corrosion Resistance of Reformulated Olive Drab 273
Topcoats.
C. Alternate Olive Drab Pigmentation. 279
D. Addition of Wax to Olive Drab Topcoats. 279
E. Silane Treatment of Olive Drab Pigments. 280
F. Flexibility Study of 301-284-D Topcoat. 282
G. Olive Drab Topcoats Containing Miscellaneous Vehicles. 282
v
Section XI Miscellaneous White Topcoat Work
A. Effect of Various White Pigments on Corrosion 285
Resistance.
B. White Topcoats Containing Same Vehicles as Best 267
S Olive Drab Topcoats.
C. Effect of Various Extender Pigments on Corrosion 297.
Resistance.
D. Addition of Chromate and Alumimm Pigmonts to White 303
Topcoats.
i. White Topcoats Containing Same PVC as Olive Drab 306
Topcoats.
F. Previously Eliminated White Topcoats. 308
G. Silane Treatment of White Pigments. 315
H. White Topcoats Made from Miscelleneous Vehicles. 315
Section XII Miscellaneous Testing
A. Optimum Thickness of Primer and Topcoat. 318
B. Exterior Exposure Panels. 318
C. Evaluation of Clear Coatings. 320
D. Riveted Bimetallic Panels. 320
E. Baked Coatings. 321
F. Final Testing of Preferred Systems. 325
Section XIII Additional Research
A. Vinyl Coatings. 328
B. Epoxy Coatings. 328
C. Silicone-Polyester Coatings Catalyzed with 334
Isocyanates and Amines.
vi
D. Miscellaneous Materials 334
E. Bimetallic Corrosion and Salt Spray Testing of 338
Primers and Clear Coatings.
F. Bimetallic Corrosion Testing of Olive Drab and 352
White Topcoats.
G. Bimetallic Salt Spray Testing of White Coating 352
Systems.
Section XIV A.Summary 358B. Acknowledgement 359
Section XV Appendix
A. Bibliography 361
B. Formulations of Preferred Coatings. 362
Section I
Introduction
The object of this contract was to develop finishing systems
for lightweight metals in both olive drab and white colors.
The ultimate use of these systems would be on aircraft,
missiles and rockets, ground transportation equipment, and
related items. The substrate of primary concern was to be
Dlow 17 treated H1K-31 magnesium alloy. Aluminum and steel
were to be given secondary consideration. It was understood
that any new magnesium alloys developed during the term of
the contract would also be used as substrates.
The major requirements of the system are:
1. Applicable by spray.
2. Air dry, preferably quick dry type.
3. Ability to withstand temperatures up to 500 0 F. for
short periods of time without losing film integrity.
4. Good film properties, such as hardness, toughness,
adhesion, flexibility, durability, and corrosion
resistance.
5. Resistance to aviation gasoline, and, if feasible,
diester lubricant.
6. Good salt spray resistance, 2,000 hours alone, and
500 hours bimetallic coupling.
7. Quality control performed by general analytical and
performance tests.
-2-
In addition, discussion with Army Ordnance Coating and
Chemical Department personnel prior to the start of work
on the contract brought out the following items:
1. A two coat system, primer plus topcoat, was
preferable to a one coat system.
2. #2430 olive drab and untinted white were tiie
desired colors for the topcoats. It was under-
stood tiat the olive drab was of primary importance.
3. The gloss of tae complete system was to be 15o-25o
as measured at 600.
4. The desired length of time for the coating to retain
film integrity at 5000 F. was 30 minutes minimum. If
the coating could withstand 5000 F. for 2 hours, this
would be more desirable. The ability of the coating
systems to withstand more than 500 0 F. was also to be
evaluated.
5. The aviation gasoline to be used for test purposes
was type III high aromatic content conforming to
MIL-S-3136 while the diester lubricant was purified
tricresyl phosphate as described in specification
MIL-H-19457.
"- 3 "
Section II
Initial Screening of Clear Films
Since a relatively high temperature was involved in this
contract, it was believed a silicone was in order. These
organic modified inorganic polymers are well known for
their excellent heat resistance. The following silicones
and silicone copolymers were chosen for initial screening:
1. General Electric SR-17
2. General Electric SR-28
3. General Electric SR-32
4. General Electric SR-82
5. General Electric SR-98 (now CR-116)
6. General Electric SR-111
7. General Electric SR-119
8. General Electric SR-120
9. Dow Corning DC-802
10. Dow Corning DC-803
11. Dow Corning DC-805
12. Dow Corning DC-806A
13. Dow Corning DC-840
14. Dow Corning XR-261
15. Dow Corning R-4471
16. Dow Corning R-6-0031
17. Dow Corning XR-856
18. Union Carbide R-64
19. Union Carbide R-630
20. Plaskon ST-847
21. Plaskon ST-856
-4-
It was realized that while silicones possess desirable high
temperature properties, they are lacking in other respects
such as ability to air dry and resistance to solvents.
Accordingly, it was decided to modify them with a variety
of organic materials to form composite resins which would
have most of the properties needed. Clear resin blends
were made containing 90, 75. and 50% silicone resin solids
(in a few cases, 25% silicene content materiels were also
evaluated) while the remainder of the vehicle nonvolatile
matter consisted of the following organic resins:
1. 1/2 second IS nitrocellulose
2. 1/2 second SS nitrocellulose
3. 1/2 second cellulose acetate butyrete
4. Polyvinyl butyral - Bakelite XYHL
5. Acrylic - Rohm and Haas Acryloid A-101
6. Styrene butadiene - Goodyear Pliolite S-5
7. Trieaine formaldehyde - Rohm and Haas Uformite M-311
8. Polyvinyl formal - Shawinigan Formvar 7/70
9. modified alkyd - Hercules Petrex SS
10. Epoxy ester - Midland Industrial Finishes Company R-55
11. Oxidizing alkyd - Midland Industrial Finishes Company R-9
12. Oxidizing alkyd - Midland Industrial Finishes Company R-50
13. Phenolic - Bakelite BRS-2600
14. Butadiene acrylonitrile - Naugatuck Paracril CV
15. Fossil resin - RBH 510
Since fluorinated hydrocarbon resins are also noted for their
resistance to thermal degradation, some of these materials
were modified in the same manner as the silicones. The
following resins were used:
1. DuPont Viton A
2. Firestone Exon 461
3. Minnesota Mining and Manufacturing Fluorel
4. hinnesota Mining and Manufacturing Kel-F 800
The best finishing system for magnesium alloys prior to
this contract was based on a polyamide cured epoxy. Con-
sequently, the entire range of conventional bisphenol A-
epichlorhydrin resins was catalyzed with various curing
agents. TWo silicone epoxy copolymers, Dow Corning XR-6-0000,
and Midland X-4209, were investigated at the same time. The
curing agents used were:
1. Vereamid 100
2. Versamid 115
3. Versamid 125
4. Versamid 140
5. Genamid 250
6. Genamid 310
7. Lancast A
8. Dow Corning Z-6020 and XZ-2-2023, amino
functional silanes
9. Diethylene triamine
10. Snell curing agents H-1 and H-2
-6 -
Other film formers which were screened include:
1. Midland R-62, a heat resistant non-oxidizing alkyd.
2. Spencer Kellogg XP-1078 high temperature polyurethane
3. Roskydol 500 polyester
4. Reichhold Polylite 8702 and 8703 polyesters
5. Rohm and Haas Paraplex P-444 polyester
6. Isocyanate cured Dow Corning R-6-0031
7. Silicones cured with experimental silazane #2311
8. Food, Machinery, and Cnemicel Company's Oxiron
resins cured with PMDA adduct
9. Dow Chemical Company's epoxy novolac resins cured
with PMDA adduct
10. Midland X-3928 silicone copolymer
11. Midland X-4415 silicone copolymer
12. Midland X-4323 silicone copolymer
13. Midland X-3934 urethane prepolymer
14. Archer Daniels Midland Aroflint 202-XAI-60 catalyzed
resin
15. Shell Eponol H-55.1 - B-40 linear thermoplastic
epoxy.
It was decided to perform relatively simple tests on these
resin systems to eliminate as many of them as possible and
therefore, make the more detailed evaluation much smaller
in scope. After samples were prepared, the coatings were
applied to 30 gauge steel with a 0.003" Bird applicator.
The coatings were allowed to air dry for 24 hours after
which they were tested as follows:
- 7-
1. Air dry film properties such as dry, compatibility
in the film, and adhesion were noted. See Table I
for key to numbers used in rating film properties.
2. Panels were subjected to 500 0 F. for periods of 30
minutes and 2 hours. Any ciiange in adhesion or loss
of film integrity resulting from the heat exposure
was noted. All coatings tested became dark in color
after the heat test. See Table 1 for key to symbols
used in rating heat resistance.
3. After allowing the coated panels to age for 96 nours,
solvent resistance of the coatings was determined.
Two small strips of each panel were cut, one strip
being immersed for 4 hours in MIL-S-3136 fluid and
the other being immersed for the same period in the
lubricant. Any coating which softened was allowed to
dry for 24 hours after which it was checked to see if
it had regained its original hardness. See Table 1
for ratings used.
4. The wet samples of each coating were checked for
storage stability after 1 montih. Any gelation,
stratification, or otaer ill effects were noted.
See Table 1 for key to stability ratings.
-8-
Table 1
Keyto Numerial Ratings and Symnbols in Vehicle Screening Tables
Ra tin. Dry Adhesion
0 Hard Excellent
1 Tack-free but Very goodslightly soft
2 Tack-free but Goodsoft
3 Slightly Tacky Fair
4 Tacky Poor
5 Very Tacky Extremely Poor
Compatibillt2
C - Compatible
H - Hazy
I - Incompatible
Stality
C - Compatible
H - Hazy
S - Stratified
Film Integrity
O.K. - No perceptible change except for darkening.
B - Blistered
N.G. - Extensive flaking or other loss of film integrity.
Gasoline and Lubricant Immersion
U - Unaffected
S - Softened
D - Dissolved
24 Hour Recovery
Yes - Recovered original properties
No - Did not recover original properties
- 10 -
Section III
Results of Screening Clear S2oins
A. Half Second Nitrocellulose Modification of Silicone Resins
1. The compatibility of unmodified silicones end nitro-
cellulose was poor while the compatibility of some of
the silicone copolymers and nitrocellulose was good.
Since most unmodified silicones are supplied with
aromatic hydrocarbon solvents, a few of the commer-
cially available 100% NVM silicones were dissolved
in methyl isobutyl ketone and blended with nitro-
cellulose. Compatibility was still poor.
2. Compatibility and resistance to MIL-S-3136 fluid and
diester lubricant were best at the 50% level of
nitrocellulose.
3. After the heat exposures, systems with borderline
compatibility often displayed blistering.
4. For the most part, the RS and SS grades of nitro-
cellulose were equivalent in performance.
5. For details of nitrocellulose modifications of
silicone resins, see Tables 2 and 3.
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- 19 -
B. Half Second Cellulose Acetate Butyrate Modification of
Silicone Resins
1. The compatibility of silicones and half second cellulose
acetate butyrate was better than the nitrocellulose
modified silicones but was still quite poor.
2. Again, compatibility and resistance to the test fluids
were best at the 50% level of modifier.
3. Coatings which were subjected to the 5000F. heat test
performed quite well in general.
4. For details of cellulose acetate butyrate modifications
of silicone resins, see Table 4.
C. Acryloid A-101 Modification of Silicone Resins
1. The compatibility of silicones and Acryloid A-101 was
quite good.
2. Resistance to the test fluids was poor with many of the
coatings being completely soluble in the fluids.
3. The Acryloid A-101 modified silicone coatings withstood
5000F. very well.
4. For details of Acryloid A-101 modifications of silicone
resins, see Table 5.
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- 28 -
D. Polyvinyl Butyral Modification of Silicone Resins
1. The compatibility of Bakelite XYHL and silicone
resins was very poor.
2. Resistance to MIL-S-3136 fluid and diester lubricant
was extremely poor.
3. The film integrity of these coatings was good after
the 500 0 F. heat exposure.
4. For details of Bakelite XYHL modifications of silicone
resins, see Table 6.
E. Styrene Butadiene Modification of Silicone Resins
1. The compatibility of Pliolite S-5 and silicone resins
was excellent.
2. These coatings did not air dry as well as most of the
other systems which were ev,,aluated.
3. Almost all the coatings were completely soluble in
the test fluids.
4. Film properties after the heat exposure were good.
5. For details of Pliolite S-5 modifications of silicone
resins, see Table 7.
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- 37 -
F. Triazine Formaldehyde Modification of Silicone Resins.
1. The compatibility of silicones and Uformite M-311 was
fairly good.
2. Many of the coatings were still quite tacky after a
24-hour air dry period.
3. Resistance to the test fluids, particularly to the
diester lubricant, was very poor.
4. Heat resistance was good.
5. For details of Uformite M-331 modifications of silicone
resins, see Table 8.
G. Polyvinyl Formal Modification of Silicone Resins
1. The compatibility of silicones and Formvar 7/70 was
very poor.
2. The best resistance to the test fluids was obtained
with coatings containing 50% Formvar 7/70.
3. The film integrity of the coatings after the 5000F.
heat exposure was good.
4. For details of Formvar 7/70 modifications of silicone
resins, see Table 9.
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- 46 -
H. Modified Alkyd (Petrex SS) Modification of Silicone Resins
I. The compatibility of Petrex SS and silicone resins was
good.
2. Coatings containing Petrex SS did not air dry well.
3. All coatings were dissolved by the test fluids.
4. Heat resistance of coatings containing Petrex SS
was good.
5. For details of Petrex SS modifications of silicone
resins, see Table 10.
I. Epoxy Ester Modification of Silicone Resins
1. The compatibility of silicone resins and Midland R-55
was generally good.
2. Only coatings containing 75. epoxy ester air dried
satisfactorily.
3. Resistance to MIL-S-3136 fluid and diester lubricant
was fair.
4. Heat resistance of coatings containing Midland R-55
was good.
5. For details of Midland R-55 modifications of silicone
resins, see Table 11.
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- 56 -
J. Oxidizing Alkyd (Midland R-9) Modification of Silicone Resins
1. The compatibility of silicone resins and Midland R-9
was limited.
2. It was generally necessary to have 75. R-9 in a coating
to obtain satisfactory dry.
3. Resistance to the test fluids was poor.
4. Heat resistance was good.
5. For details of Midland R-9 modifications of silicone
resins, see Table 12.
K. Oxidizing Alkyd (Midland R-50) Modification of Silicone Resins
1. The compatibility of silicone resins and Midland R-50
was limited.
2. Resistance to the test fluids was slightly better than
coatings containing Midland R-9, but was still
unsatisfactory.
3. Heat resistance was good.
4. For details of Midland R-50 modification of silicone
resins, see Table 13.
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- 65 -
L. Phenolic (Bakelite BRS-2600) Modification of Silicone Resins
1. The compatibility of BRS-2600 and silicone resins was
poor.
2. Coatings containing 75% BRS-2600 had excellent
resistance to the test fluids.
3. Most of these coatings blistered when tested at 5000F.
4. For details of Bakelite BRS-2600 modifications of
silicone resins, see Table 14.
M. Butadiene Acrylonitrile Modification of Silicone Resins
1. The compatibility of Paracril CV and silicone resins
was limited.
2. Resistance to the test fluids was poor.
3. Some of the coatings containing 75. Paracril CV
decomposed at 5000 F.
4. For details of Paracril CV modifications of silicone
resins, see Table 15.
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- 74 -
N. Natural Fossil Resin (RBH 510) Modification of
Silicone Resins
1. The compatibility of RBH 510 and silicone resins
was fairly good.
2. Resistance to the diester lubricant was quite good
but resistance to MIL-S-3136 fluid was poor.
3. Heat resistance of coatings containing RBH 510 was
poor. Flaking, blistering, and decomposition were
all noted.
4. For details of RBH 510 modifications of silicone
resins, see Table 16.
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- 79 -
O. EPoxy Resin Systems
1. Coatings containing Epon 828 were generally unsatis-
factory. Many Epon 828 coatings would not properly
cure and many others had a tendency to "crawl" and
create an appearance of incompatibility.
2. With the exception of Versamid 100, the polyamides
successfully cured the epoxies and were judged to
be about equivalent in performance. Coatings con-
taining Versamid 100 were sensitive to the MIL-S-3136
fluid but this was probably because Versamid 100 is
the slowest reacting polyamide.
3. Coatings containing 10% and 25% polyamide (depending
on the epoxy used) had the best resistance to the
test fluids and had the best over-all film properties.
4. The solid epoxies (Epons 1001, 1004, 1007, and 1009)
seemed to be about equal in performance with Epon 1009
possibly having slightly superior heat resistance.
5. The silicone epoxy copolymers (Dow Corning XR-6-0000
and Midland X-4209) had no better heat resistance than
the unmodified epoxies and were slightly poorer than
the unmodified epoxies in resistance to the test fluids.
6. Dow Corning Z-6020 amino silane appeared to be an
effective curing agent for epoxies but had little
effect on the high temperature properties of the
epoxies which were quite good to begin with.
- 80 -
7. The epoxy novolacs (Dow 2638.1 and Dow 2638.3) were
all extremely brittle, regardless of the curing agent
used.
8. Shell H-1 and H1-2 curing agents seemed to be worthwhile
catalysts with Epon 1001 and the silicone-epoxy
copolymers. With Epon 1007 and Epon 1009, however,
a large number of eyeholes appear in the coatings
after the 5000 F. heat exposure. These eyeholes were
not present before the heat test. H-1 seemed to be
slightly superior in performance to H-2.
9. Details of epoxy resin systems may be found in
Tables 17-26.
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- 103 -
P. Silicone Resins Cured with #2311 Experimental Silazane
1. Many of the systems in this series gelled immediately
after the addition of the silazane and were of no
use.
2. Resistance to the test fluids was very poor.
3. Heat resistance was excellent.
4. For details of silicone resins cured with #2311
experimental silazane, see Table 27.
Q. Silicone Resins Cured with Z-6020 Amino Silane
1. Some silicones do not react (or react very slowly)
with Z-6020. All systems had a usable pot life.
2. Resistance to the test fluids was poor.
3. Heat resistance was good.
4. For details of silicone resins cured with Z-6020,
see Table 28.
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- ill -
R. Half Second RS Nitrocellulose Modification of
Fluorinated Hydrocarbon Resins
1. Compatibility of nitrocellulose and the fluorinated
resins was good.
2. The test fluid resistance of some of these systems
was good.
3. A few of these coatings decomposed during the heat
test but most were satisfactory.
4. Details of nitrocellulose modification of fluorinated
resins can be found in Table 29.
S. Polyvinyl Butyral Modification of Fluorinated Hydrocarbon
Resins
1. Compatibility of Bakelite XYHL and the fluorinated
resins was poor.
2o Resistance to the test fluids was poor.
3. Heat Resistance was good.
4. For details of Bakelite XYHL modification of
fluorinated hydrocarbon resins, see Table 30.
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- 116 -
T. Acryloid A-10 Modification of Fluorinated
Hydrocarbon Resins
1. Compatibility of Acryloid A-101 and the fluorinated
resins was fairly good.
2. Resistance to lubricant and MIL-S-3136 fluid was
generally good.
3. Heat resistance was good.
4. For details of Acryloid A-101 modification of
fluorinated hydrocarbon resins, see Table 31.
U. Styrene Butadiene Modification of Fluorinated
Hydrocarbon Resins
I. Compatibility of Pliolite S-5 and the fluorinated
resins was fair.
2. Resistance to the test fluids was poor.
3. Except for two systems, neat resistance was good.
4. For details of Pliolite S-5 modifications of
fluorinated resins, see Table 32.
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- 121
V. Triazine Formaldehyde Modification of Fluorinated
Hydrocarbon Resins
1. Compatibility of Uformite M-311 and the fluorinated
hydrocarbon resins was fair.
2. Resistance to the test fluids was poor.
3. Heat resistance was good.
4. For details of Uformite M-311 modification of
fluorinated resins, see Table 33.
W. Polyvinyl Formal Modification of Fluorinated Hydrocarbon
Resins
1. Compatibility of Formvar 7/70 and the fluorinated
resins was fair.
2. Resistance to the test fluids was poor.
3. Heat resistance was good.
4. Details of Formvar 7/70 modifications of fluorinated
hydrocarbon resins may be found in Table 34.
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- 126 -
X. Miscellaneous Resin Systems
1. Many of the miscellaneous resin systems tested
showed great promise in the initial screening
tests. Most of the better coatings were based
on epoxies, polyurethanes, or polyesters.
2. For results of testing the miscellaneous resin
systems, see Table 35.
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- 131-
Section IV
Development of Primer
A. Initial Vehicles Used
After the screening tests had been completed on the
clear resin systems, the test results were reviewed
and the following vehicles were chosen for use in
primers:
1. 507. Midland R-62
507. Half Second RS Nitrocellulose
2. 50%. Dow Corning R-6-0031
50%. Half Second RS Nitrocellulose
3. 50%. Plaskon ST-856
50%. Half Second RS Nitrocellulose
4. 50%. Dow Corning DC-803
50%. Half Second Cellulose Acetate Butyrate
5. 507. Dow Corning DC-805
507. Half Second Cellulose Acetate Butyrate
6. 507. General Electric SR-82
507. Formvar 7/70
7. 507 Kel F 800
507 Acryloid A-101
8. 75% Kel F Fluorel
25% Acryloid A-l01
- 132 -
9. 50% Dow Corning R-6-0031
50% Bakelite BRS-2600
10. 25% Plaskon ST-847
75M Midland R-55
11. Roskydol 500 Catalyzed Polyester
12. 73% Dow Corning R-6-0031
5% Mobay Multron R-16
22% Mobay Mondur CB-75
13. 90% Epon 1009
10% Versamid 115
14. 90% Epon 1009
10% Dow Corning Z-6020
15. Epon 1009 catalyzed witii diethylene
triamine (DET).
16. 75% Epon 1001
25% Versamid 115
17. 907. Epon 1001
107. Dow Corning Z-6020
18. Epon 1001 catalyzed with diethylene
triamine (DET).
19. 75% Dow Corning XR-6-0000
25% Versamid 115
- 133 -
20. 75% Midland X-4209
257. Versamid 115
21. 757. Dow Corning XR-6-0000
25% Dow Corning Z-6020
22. 75% Midland X-4209
257 Dow Corning Z-6020
It will be noted that several vehicles which appear in
Table 35 and seem to nave some promise are not included
in tois list. These materials were evaluated later in
th-e contract and will be mentioned later in the report.
B. Pigments Used
Previous work lto develop a coating system for magnesium
included an extensive evaluation of corrosion inhibiting
pigments. It was determined that the chromates of
calcium and strontium were among the most effective for
protection of magnesium. These pigments were selected
for the primers. Zinc chromate was believed worthy of
testing and was also included.
The same previous work found a pigment content of 357. by
weight to provide tiie optimum protection of magnesium.
This pigment content was cnosen for the initial pigment
study. No extender pigments were used.
1. The reference may be found in the bibliography section of theappendix.
2. Ibid.
- 134 -
C. bimetallic Corrosion Testing
It was decided to form a bimetallic couple between the
coated magnesium panel and Ui-7PH stainless steel to
test the effectiveness of tote coatings in preventing
galvanic corrosion. The coated magnesium panel and the
stainless steel strip were mounted approximately I inch
apart in a wooden mounting, block and were then connected
witr. a copper wire and clips. The magnesium panel was
scraped witti a knife to bare metal where the clip was
attactied. (See fig. 1)
Initially, some panels t.ad :)eei, coated witL. 0.0005, J.0010,
and 0.0015 inches of two of Lhe primers. The panels were
connected to the stainless steel and immersed in I and 5%
NaCI solutions which were contained in 1 gallon glass jars.
Th'e panels were immersed to a depth of 4 inches and the
immersed anode: cati,ode area ratio was 4:1 (See fig. 2).
A n-,i.';ber of materials were used to cover the uncoated edges
of te panels. It was found that black electrical tape
put on the edges of the panel and coated with a layer of
paraffin afforded the best protection. It was also
determined tftat a coating thickness of 0.0015 inches and
an electrolyte concentration of 1% NaCl produced the most
consistent results. All coatings were tested for bimetallic
corrosion resistance in this manner. Table 36 explains
the symbols used in rating bimetallic corrosion.
- 137 -
Table 36
Bimetallic Corrosion Rating System
The following ratings are used in all bimetallic
corrosion tables:
HoursRating Exposed Condition of Panel
0 500 Perfect.
1 500 Very few very small blistersor slight discoloration.
2 500 Many small blisters and fewmedium blisters. Very slightcorrosion.
3 500 Many small and medium blisters.Few large blisters and slightcorrosion.
4 Less than Many blisters and considerable500 corrosion.
5 Less than Many blisters and severe corrosion.500
The following symbols may also be found:
N.T. - The coating was not tested due to some film failure
such as cracking. (See fig. 3)
G - The coating gelled during preparation and could not
be tested.
4.
00
EXAMPLES OF PANELS WHICH HAVE CRACKED UPON DRYING
Fig. 3
PANELS NOT TESTED DUE TO CRACKING OF TOPCOAT
- 139 -
D. Results of Bimetallic Corrosion Testing
As a result of tite galvanic corrosion tests, the following
primers were selected for further testing:
1. 301-103-A
2. 301-101-D
3. 301-131-B
Tne results of galvanic corrosion testing of the primers
may be found in Table 37.
E. Addition of Inert Pigments to Primers
Most of the faiiLres which occurred during the galvanic
corrosion testing of the primers were due to blistering
and/or corrosion. (See fig. 4) It was decided to
evaluate the addition of extender pigments to these
coatings in an attempt to reduce the blistering. The
inert pigments used were talc and clay. The total
pigment content was kept at 35% by weigat.
It was found tnat no improvement was made in the perform-
ance of the topcoats tested but rather the galvanic
corrosion resistance of tie coatings containing tne
extender pigments was worse than that of the original
coatings. (See fig. 5) For results of galvanic corrosion
testing of primers containing extender pigments, see
Table 38.
- 140 -
FIG. 4
EXAMPLES OF POOR GALVANIC CORROSION RESISTANCEALL FAILED IN LESS THAN 500 HOURS
Fig. 4
TYPICAL GALVANIC CORROSION FAILURES
. 141,.
FIG. 5
1/a e ia'u ,
j 9,
RESULTS OF ADDING INERT PIGMENTS TO PRIMERS ALONE124G, H, K-INERTS 300 HRS. IN CELL, 103A-NONE 500 HRS.
Fig. 5
GALVANIC CORROSION TESTING OF PRIMERS
CONTAINING EXTENDER PIGMENTS
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- 149 -
F. Salt Spray Exposure of Primers
Panels coated with the initial primers were tested in
57. salt spray at the same time they were being evaluated
for galvanic corrosion resistance. Throughout most of
the contract, t~iis simultaneous exposure was conducted.
The coating thickness on the salt spray panels was the
same as tne bimetallic corrosion panels. All salt
spray panels were scribed to the bare metal down the
center of the panel. For results of salt spray
exposure of the primers, see Tables 39 and 40.
(See fig. 6)
It should be noted that all salt spray results, unless
otherwise stated, represent the entire panel, not only
the scribed portion of the panel. Wnen different
results occur on the panel and on the scribe, a
semicolon is used. For example:
Many small blisters; many small blisters,
slight corrosion on scribe.
indicates the following were present:
(1) many small blisters on panel.
(2) many small blisters on scribe.
(3) slight corrosion on scribe.
kt
- 150 -
FIG. 6
VARYING RESULTS IN 5% SALT SPRAY. PERFECT INUPPER LEFT, TO MANY BLISTERS LOWER RIGHT
Fig. 6
TYPICAL 5% SALT SPRAY TEST RESULTS
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- 155 -
Section V
Development of Olive Drab Topcoat
A. Initial Vehicles Used
The vehicles used for preparation of olive drab topcoats
were the same as those used for the primers. The complete
list can be found in part A of the primer section.
B. Pigmentation
The following pigmentation was used to obtain the #2430
olive drab color and 15-250 gloss:
Pigment .by weight
Medium chrome yellow 31.6
Red lead 16.7
Zinc oxide 9.1
Red iron oxide 12.3
Lampblack 6-0
Titanium dioxide 10.9
Clay 2.7
Diatomaceous earth 10.7
100.0%
Coatings containing unmodified silicone resins did not
include the red lead because of the reactivity of those
resins with lead. A pigment content of 65% by weight
was used. No attempt was made to shade tnese coatings
to match the #2430 color chip nor was the gloss of any
coating adjusted.
156 -
C. Preparation of Panels
The Dow 17 treated HK-31 magnesium panels were primed
with 0.0015 inches of primer and allowed to age a
minimum of / days. The same t-ickness of topcoat was
applied and the panels were aged for 7 more daysbefore
9 testing. Each coating was crosshatched with a stylus
and the adhesion tested with cellulose tape. The tape
was firmly applied to the crosshatched section and then
removed from the panel in one rapid motion. See Table 41
for adhesion rating key. (See fig. 7)
D. Bimetallic Corrosion and Salt Spray Testing
The bimetallic corrosion and salt spray testing of the
complete coating systems were conducted in the same
manner as those tests were performed on the primers alone.
The following systems were judged to be the best coatings
at this point in the work:
Primer Topcoat
1. 301-103-A 301-115-A
2. 301-131-B 301-115-A
3. 301-131-B 301-114-C
4. 301-103-A 301-134-A
5. 301-103-A 301-134-C
6. 301-131-B 301-134-C
7. 301-131-B 301-118-F
For results of salt spray and bimetallic corrosion testing
of the olive drab coating systems, see Tables 42 and 43.
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- 167 -
Section VI
Development of White Topcoat
A. Initial Vehicles Used
4 The vehicles found in Part A of the primer section were
used to prepare white topcoats. One resin system, the
combination of Dow Corning R-6-0031 and Bakelite
BRS-2600, was not used because of its dark color.
B. Pigmentation
The pigment chosen for the white topcoats was sulfate-
process rutile titanium dioxide. The coatings were
flatted to the approximate gloss required with talc.
A 53% pigment content by weight was used.
C. Preparation of Panels
The same procedure used for preparation of olive drab
coating systems was followed with the white systems.
Only the 301-103-A and 301-131-B primers were used.
D. Bimetallic Corrosion and Salt spray Testing
Bimetallic corrosion and salt spray tests were conducted
in the usual manner.
Although the white coating systems were generally
inferior in performance to the olive drab systems, the
following were considered to have performed well enough
to merit additional testing:
- 168-
Primer Topcoat
1. 301-103-A 301-164-D
2. 301-131-B 301-163-F
3. 301-131-B 301-183-B
4. 301-103-A 301-183-D
5. 301-103-A 301-210-A
For results of salt spray and bimetallic corrosion
testing of white coating systems, see Tables 44 and
45.
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- 175 -
Section VII
EFpoxy Ester and Silicone Epoxy Ester Coatings
A. 301-103-A Primer
This primer, containing a blend of Midland R-55 epoxy
ester and Plaskon ST-847 silicone-epoxy ester copolymer
was one of the two best primers for inhibiting galvanic
corrosion. However, it did not provide good adhesion
for most topcoats. The following were tried in an
attempt to improve this property:
1. The drier content was increased and decreased.
2. The time between applying the primer and applying
tne topcoat was varied.
3. The topcoats were reduced with methyl isobutyl
ketone to try to soften tuie primer just enougn
to provide better adhesion.
4. The pigment volume concentration of the topcoats
was increased and decreased.
None of the above was successful with the exception of
topcoating witnin 24 hours after applying the primer.
This was believed to be too impractical to merit further
consideration.
- 176 -
3. Preparation and Testing of New Vehicles
Since primer 301-103-A was a blend of an epoxy ester
and a silicone-epoxy eater copolymer, it was thought
that a silicone-epoxy ester copolymer approximately
equal to the blend in composition might have some
properties superior to the blend. For this reason,
the following resins were prepared:
Code EpFatty Acid Silicone
X-4235 40% Upon 1001 30% Linseed 30% Dow Corning5-6018
X-4237 49% Epon 1001 36% Tall 15% Dow Corning5-6018
X-4238 49% Epon 1001 36% Linseed 15% Dow Corning5-6018
X-4240 49% Upon 1001 36% DCO 15% Dow Corning5-6018
X-4241 51% Epon 1001 39% Linseed 10% Dow Corning5-6018
X-4243 51% Epon 1001 39% Tall 10% Dow Corning5-6018
X-4245 51% Upon 1001 39% DCO 10% Dow Corning5-6018
X-4253 49% Upon 1001 36% DCO 15% Dow CorningSylkyd 50
X-4255 51% Epon 1001 39% DCO 10% Dow CorningSylkyd 50
X-4257 49% Upon 1001 36% DCO 15% Dow CorningXS-6088
X-4263 49% Upon 1001 36% Safflower 15% Dow CorningZ-6018
X-4266 51% Upon 1001 39% Safflower 10% Dow Corning5-6018
X-4271 49% D.E.R. 661 36% Safflower 15% Dow Corning5-6018
X-4278 49% Upon 1001 36% Soya 15% Dow Corning5-6018
X-4282 49% D.A.R. 661 36% DCO 15% Dow Corning5-6018
X-4283 49% Axaldite 6071 36% DCO 15% DowCorning5-6018
X-4295 49% Upon 1001 36% DCO 15% Dow Corning5-6018
X-4296 49% Upon 1007 36% DCO 15% Dow Corning5-6018
X-4300 49% Spon 1001 36% DCO 15% Union CarbidexM-820
- 176a -
The silicone-epoxy eater copolymers were prepared in
the following manners
1. The fatty acid was heated to approximately the
melting point of the epoxy resin. For epoxy resins
with epoxide equivalent weights of 500, the temperature
was 210-250OF. For epoxies with epoxide equivalent
weights of 900-1,000 and 2,000-2,500, the temperatures
to which the fatty acids were heated were 300 F and
350 F, respectively. In some cases, a catalytic quan-
tity of triphenyl phosphite was added after the fatty
acids reached the desired temperature. A blow of inert
gas was used throughout the cook.
2. The epoxy resin was added and the mixture was
blown at 520°F for 1 hour. The acid number would be
in the range of 1-5 after this time.
3. The temperature was lowered to 400OF and the
silicone intermediate and a portion of the solvent
was added. Some octoic acid was added as a catalyst
when Dow Corning Sylkyd 50 and Union Carbide XR-620
were used. The material was refluxed about 10 hours
or until viscous. The remainder of the solvent was
added.
In addition some counterparts of Midland R-55 were
prepared to determine the effect of different oils
on the performance of this resin. Midland X-3540,
4 X-3548, and X-4334 contained linseed, DCO, and soya
fatty acids, respectively. The following commercial
epoxy esters were also evaluated:
1. Reichhold Epotuf 6401
2. Jones-Dabney Bpitex 120
3. Jones-Dabney Epitex 1241
4. Jones-Dabney Spitex 1486
5. Midland R-2
- 177 -
C. Screening of Clear Resins
The epoxy esters and the silicone-epoxy ester copolymers
mentioned above were screened in clear coatings by them-
selves and, when indicated, in combination with each other.
The results of this testing can be found in Table 46. All
9coatings made from the same resin differ only in drier
content. The following ratio of driers (based on metal
content by weight) was used throughout.
3 parts cobalt
4 parts calcium
2 parts rare earth
D. Epoxy Ester Primers
Since the pigment level chosen for evaluation of the
primers was set at 35% by weight only on the basis of
previous work in this field, a study of the effect of
pigment concentration on corrosion resistance was under-
taken. The Midland R-55: Plaskon ST-847 vehicle was
chosen for this work and the pigment content was varied
from 0 to 65% by weight. It was found that the 35%
pigment level was as good a choice as could be made.
For bimetallic corrosion and salt spray testing of
these coatings, see Tables 47 and 48. (See fig. 8)
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- 188 -
FIG. 8
.35:1 .15:1
EFFECT OF PIGMENT-TOTAL SOLIDS RATIO
Fig. 8
EFFECT OF PIGMENT CONTENT ON GALVANIC CORROSION
RESISTANCE OF A SILICONE-EPOXY: POLYAMIDE PRIMER
-189 -
The following resin systems were believed worthy of
testing based on results of screening tests on the
$ clear resins:
1. Midland X-4240
2. 75% Midland R-5525% Midland X-4235
3. Midland R-55
4. Midland X-4245
5. Midland X-4263
6. Midland X-4271
7. Midland X-4282
8. Midland X-4283
9. Midland X-4300
10. 507 Midland X-428350% Midland R-55
11. 50% Midland X-424050% Midland R-55
12. 507 Midland X-426350% Midland R-55
13. Midland X-3548
14. 75% Midland X-3548257 Plaskon ST-856
15. Midland X-4334
16. Midland X-3540
17. 75% Midland X-3540257 Plaskon ST-847
18. Reichhold Epotuf 6401
19. g5% Reichhold Epotuf 6401257 Plaskon ST-847
20. Jones-Dabney Epitex 120
- 190 -
21. 75% Jones-Dabney Epitex 12025% Plaskon ST-847
9 22. Jones-Dabney Epitex 1341
23. 50% Jones-Dabney Epitex 134150% Plaskon ST-847
24. 75. Jones-Dabney Epitex 148625% Plaskon ST-847
25. 50% Jones-Dabney Epitex 148650% Plaskon ST-847
To expedite testing of these vehicles in primers, many
of the primers were made using only zinc or calcium
chromate as pigment. Earlier testing of primers had
shown the strontium chromate to be an ineffective
corrosion inhibitor. In some of the primers the
calcium chromate also was not used since the zinc
chromate appeared to be the best pigment in epoxy
ester coatings.
As a result of the bimetallic corrosion and salt spray
testing, the following primers were included in future
testing:
1. 301-158-C
2. 301-158-L
3. 301-159-D
4. 301-159-G
5. 301-202-A
For results of galvanic corrosion and salt spray
testing of epoxy ester primers, see Tables 49 and
50.
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- 197 -
E. Epoxy Ester Olive Drab Topcoats
Some of the epoxy ester vehicles which were used in
the primers were also used in olive drab topcoats.
Most of these coatings did not perform any better
tnan the original coating systems but the following
were selected for further testing:
Primer Topcoat
1. 301-103-A 301-174-B
2. 301-131-B 301-174-B
3. 301-131-B 301-174-C
4. 301-103-A 301-175-A
5. 301-103-A 301-175-B
6. 301-131-B 301-175-B
The results of bimetallic corrosion and salt spray
testing of epoxy ester olive drab topcoats can be
found in Tables 51 and 52.
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- 204 -
F. Epoxy Ester White Topcoats
The same vehicles used in the olive drab topcoats were
4 used for the white coatings. The original pigmentation
was used for these coatings. None of these materials
performed well enough to merit future work. Galvanic
corrosion and salt spray test results can be found in
Tables 53 and 54.
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- 209 -
Section VIII
Epoxy and Silicone-Epoxy Copolymer Coatings
A. Preparation and Testing of New Vehicles
Since epoxies and silicone-epoxy copolymers had performed
fairly well in the intial testing, it was decided to pre-
pare some copolymers with different silicone contents for
evaluation. The following materials were synthesized:
Code Silicone Epoxy
X-4311 25% Dow Corning R-861 75% Epon 1001
X-4313 (12.5% Dow Corning Z-6018 75% Epon 1001(12.5% Dow Corning QZ-8-0031
X-4315 25% Dow Corning Z-6018 75% Epon 1001
X-4316 15% Dow Corning Z-6018 85% Epon 1001
X-4317 35% Dow Corning Z-6018 65% Epon 1001
X-4209 50% Dow Corning Z-6018 50% Epon 1001
B. Screening of Clear Resins
The silicone-epoxy copolymers were screened in the usual
manner. Versamid 115, Dow Corning Z-6020, and diethylene
triamine were used as catalysts. Almost all of these
materials were excellent when tested in the clear film
as can be seen from Table 55.
C. Epoxy and Silicone-Epoxy Primers
Primers were prepared from a number of epoxy and silicone-
epoxy resins. Only two of them, 301-188-C and 301-232-E,
were included in future work. Results of bimetallic
corrosion and salt spray testing of the epoxy and silicone-
epoxy primers can be found in Tables 56 and 57.
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- 218 -
D. Epoxy and Silicone-Epoxy Olive Drab Topcoats
None of the olive drab topcoats made from the epoxy
and silicone-epoxy resins performed as well as expected
and all were eliminated from future testing. Bimetallic
corrosion and salt spray results can be found in Tables
58 and 59.
E. Epoxy and Silicone-Epoxy White Topcoats
Of the white systems tested, only the following was
considered satisfactory:
Primer Topcoat
301-131-B 301-211-C
Results of galvanic corrosion and salt spray testing
can be found in Tables 60 and 61.
!.
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- 229 -
Section IX
Miscellaneous Primer Work
A. Conventional Primers
It was decided to evaluate some conventional corrosion
inhibiting primers under some of the better topcoats.
The following materials were chosen for evaluation:
Primer Code Type
1. 407 MIL-P-15328
2. 621 TT-E-485d Olive Drab
3. 408 MIL-P-7962
4. 503 MIL-P-11414A
The wash primer, 40W, was catalyzed with half the normal
acid.
The following olive drab topcoats were used over the
conventional primers:
I. 301-114-C
2. 301-115-A
3. 301-134-A
4. 301-134-C
5. 301-118-F
In general, the performance of coating systems using
conventional primers was poor. In the few cases where
performance in the bimetallic coupling test was fairly
good, the salt spray results were not as good as those
obtained when the experimental primers were used. The
conventional primers were, therefore, eliminated from
additional testing. Bimetallic corrosion and salt
spray results are in Tables 62 and 63. (See fig. 9)
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- 234-
FIG. 9
$e
407 503
Fig. 9
GALVANIC CORROSION TESTING OF COATING SYSTEMS USING
SPECIFICATION PRIMERS.
- 235 -
B. Primers Containing Molybdate Pigments
During the course of the contract, a new series of
corrosion inhibiting pigments became commercially
available. These materials, made by Mineral Pigments
Corporation, are calcium, strontium, and zinc molybdate.
$ While they supposedly do an excellent job in the protection
of ferrous substrates, no information was available regard-
ing their effectiveness over magnesium. The following
pigments were used:
1. 0820 calcium molybdate
2. 0830 zinc molybdate
3. 0838 strontium molybdate
4. 0821 calcium molybdate extended withcalcium carbonate
5. 0831 zinc molybdate extended withcalcium carbonate
6. 0839 strontium molybdate extended withcalcium carbonate
The vehicles used were:
1. Midland R-55: Plaskon ST-847
2. Dow Corning XR-6-0000: Versamid 115
Pigment content was varied from 20 to 65% by weight.
It was found that several of these primers, particularly
at low pigment loadings, performed well in the bimetallic
corrosion test. The salt spray performance of these coat-
ings, however, was extremely poor. The molybdate pigments,
rather than having an inhibitory effect on corrosion,
actually seemed to promote corrosion. Galvanic corrosion
and salt spray testing results of molybdate primers can
be found in Tables 64 and 65.
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- 241 -
Although the salt spray performance of the molybdate
primers was poor, it was decided to try a few of th~em
under some of the better topcoats. The following were
chosen:
9 1. 301-252-F
2. 301-253-B
3. 301-253-G
Topcoats used for this program were:
1. 301-118-F
2. 301-175-B
3. 301-114-C
4. 301-134-A
5. 301-204-A
b. 301-163-B (white)
The coating systems using the molybdate primers were
fair in the bimetallic corrosion test but performed
poorly in the salt spray. These primers were eliminated
from further testing. Galvanic corrosion and salt spray
results can be found in Tables 66 and 67.
C. Comparison of Zinc Chromate Pigments from Various Suppliers
Midland R-55: Plaskon ST-847 primers were made from zinc
chromate pigments obtained from the following suppliers:
1. Imperical Color, Chemical & Paper Corp.
2. Reichhold Chemicals, Inc.
3. Western Dry Color Company
- 242 -
4. Kentucky Color & Chemical Company
5. DuPont
Bimetallic corrosion tests performed on panels coated
with these primers indicated no substantial differences
in tuese pigments as far as tikeir performance in this
coating was concerned.
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- 246 -
D. Effect of Extender Pigments on Primer Performance
Earlier in the contract, small amounts of extender
pigments were added to some primers to determine the
effect of the inerts on bimetallic corrosion resist-
ance. No topcoats were used. The primers contain-
ing tne inert pigments were far inferior in performance
to the same coatings without the inerts.
It was believed worthwhile testing the two best
primers, with and without extender pigments, under
some of the better topcoats. The following primers
were used:
1. 301-103-A zinc chromate primer
2. 301-124-H zinc cnromate primer withextender pigments
3. 301-131-B calcium chromate primer
4. 301-232-H calcium chromate primer withextender pigments
The first two primers above nave Midland R-55:
Plaskon ST-847 as the vehicle while the other
remaining two coatings contain a Dow Corning XR-6-0000:
Versamid 115 vehicle. Thie following topcoats were
used over each primer:
1. 301-115-A
2. 301-134-A
3. 301-175-A
4. 301-175-C
5. 301-222-A
6. 301-183-B (white)
- 247 -
The results of the testing of this series are very
similar to those obtained when only the primers were
tested, namely, systems using primers containing no
extender pigments performed much better than systems
using primers with inert pigments. Results of salt
spray and bimetallic corrosion testing can be found
in Tables 6b and b9. (See fig. 10)
E° Effect of Tri-butyl Tin Oxide on Galvanic Corrosion
Resistance
Tri-butyl tin oxide supposedly has an inhibitory
effect on the corrosion of magnesium. Small amounts
of TBTO were, therefore, added to the 301-131-B
calcium chromate primer. Similar additions of TBTO
to tile 301-103-A zinc chromate primer produced
incompatibility and gelation. The results of the
testing of coatings containing TBTO seem to indicate
that for this particular coating, the addition of
TBTO accelerates rather than inhibits corrosion.
Salt spray and bimetallic corrosion results are
listed in Tables 70 and 71.
41
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- Z51 -
Table 69
576 Salt Spray Testing of Coating SystemsUsing Primers Containing Extender Pigments
Primer Topcoat Hour s
Code Code Adhesion Results Tested
301-103-A 301-115-A 5 Slight corrosion and one medium blister 2000on scribe.
Y#01-124-H 301-115-A 3 One medium and few small blisters, slight 2000
lifting and moderate corrosion, all on scribe.
301-131-B 301-115-A 2 Very slight lifting on scribe. 2000
301-232-H 301 -115-A 0 Few small and one medium blister, slight 2000
lifting and corrosion, all on scribe.
301-103-A 301-134-A 0 Few small blisters and slight lifting on scribe. 2000
301-124-H 301-134-A 0 Some very small blisters; one medium blister, 2000moderate corrosion and slight lifting onscribe.
301-131-B 301-134-A 0 Very slight lifting and few very small blisters 2000on scribe.
301-232-H 301-134-A 0 Some very small blisters; two medium blis- 2000
ters, slight corrosion and lifting on scribe.
301-103-A 301-175-A 5 Slight corrosion on scribe. 2000
301-124-H 301-175-A 0 Many small blisters, slight corrosion and 2000
lifting, all on scribe.
301-131-B 301-175-A 1 Few veiv small blisters and slight corrosion 2000
on scribe.
301-232-H 301-175-A 0 Few small and one medium blister, slight 2000corrosion and lifting, all on scribe.
301-103-A 301-175-C 5 Slight lifting and corrosion on scribe. 2000
301-124-H 301-175-C 3 Two medium blisters; few small blisters, 2000
slight corrosion and lifting on scribe.
301-131-B 301-175-C 5 Two small blisters, very slight lifting and 2000
corrosion, all on scribe.
301-232-H 301-175-C 0 Many very small blisters; few small blisters, 2000
slight corrosion and lifting on scribe.
301-103-A 301-222-A 5 Very few small blisters and slight corrosion 2000
on scribe.
301-124-H 301-222-A 1 Slight corrosion and lifting on scribe. 2000
301-131-B 301-222-A 5 Few small and one medium blister, slight 2000
lifting and corrosion, all on scribe.
301-232-H 301-222-A 0 Few small blisters, slight lifting and 2000
corrosion, all on scribe.
- 252 -
Table 69 (continued)
5% Salt Spray Testing of Coating SystemsUsing Primers Containing Extender Pigments
Primer Topcoat HoursCode Code Adhesion Results Testcd
301-103-A 301-183-B 1 Completely unaffected. 2000
301-124-H 301-183-B 0 Few small blisters; slight lifting and very 2000
# slight corrosion on scribe.
301-131-B 301-183-B 0 Very slight corrosion on scribe. 2000301-232-H 301-183-B 0 Few very small blisters; many very small 2000
blisters and slight corrosion on scribe.
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- 254 -
FIG. 10
I
RESULTS OF ADDING INERT PIGMENTS TO PRIMERSC = INERTS ADDED A = WITHOUT
Fig. 10
EFFECT OF ADDITION OF INERT PIGMENT TO PRIMERS OF
PREFERRED COATING SYSTEMS
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-258 -
F. Evaluation of Previously Eliminated Primers
Since all evaluation of complete coating systems had
been conducted using only two primers, it was decided
to test some of the better topcoats over some previously
eliminated primers. It was also decided to include
some of the primers which were developed later in the
contract and never tested under topcoats. The primers
chosen for this study were:
Primer Code Vehicle Pigment
1. 301-106-A Epon 1001: Versamid 115 ZnCr04
2. 301-106-G Epon 1001: Versamid 115 CaCr04
3. 301-106-K Epon 1001: Diethylene Triamine CaCr04
4. 301-107-A Epon 1009: Versamid 115 ZnCr04
5. 301-102-D Kel F Fluorel: Acryloid A-101 ZnCr04
6. 301-156-L Midland X-4245 ZnCr04
7. 301-159-D Midland X-4271 ZnCr04
8. 301-188-C Epon 1001: Snell H-1 CaCr04
9. 301-202-A Midland X-4283 ZnCr04
10. 301-158-C Midland X-4240 CaCr04
11. 301-159-G Midland X-4282 ZnCr04
12. 301-232-E Midland X-4316: Versamid 115 CaCr04
The topcoats used were:
1. 301-175-B Olive Drab
2. 301-118-F Olive Drab
3. 301-114-C Olive Drab
4. 301-134-A Olive Drab
5. 301-134-C Olive Drab
6. 301-163-B White
- 259 -
As usual, both bimetallic corrosion and salt spray
resistance of these coating systems was determined.
All of these systems, as can be seen from Tables 72
and 73, were inferior to tne best coating systems and
were eliminated from furtLier consideration.
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-268-
G. Primers Containing Miscellaneous Vehicles
During the course of the contract, a number of
miscellaneous vehicles were tested. Some of these
materials passed initial screening tests in clear
films and were incorporated into primers. These
resin systems were:
1. Midland X-3928 - a silicone copolymer.
2. Dow Corning R-6-0031: Mondur CB-75 - This
vehicle is the same as one of the better vehicles
but the Multron R-16 polyester was eliminated.
3. Midland X-4415 - a silicone copolymer.
4. Midland X-4323 - a silicone copolymer.
5. ADM Aroflint 202-XAl-60: 303-X-90.
6. Cargill 1459 Polyurethane Oil.
7. Midland X-3934 - a urethane prepolymer.
None of these primers were considered good enough to
warrant further investigation. Bimetallic corrosion
and salt spray results can be found in Tables 74 and
75.
H. Reformulation of 301-131-B Primer
One of the problems with the 301-131-B primer was the
extremely hard settling of the pigment. A small amount
of Bentone 27 was added to correct this condition. The
code for the reformulated primer was 301-271-D.
- 269 -
It was then discovered that the General Electric $K-82
which was added as a flow control agent was absorbed
by the pigment, eventually causing a flow problem.
This was corrected by putting the SR-82 into the
catalyst system. The code for the final revised
formula is 301-275-E. No change in performance of
the primer was noticed as these changes were made.
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- 273 -
Section X
Miscellaneous Olive Drab Topcoat Work
A. Reformulation of Olive Drab Topcoats to Match
Color #X-24087.
During the course of the contract, it was decided the
color of the olive drab topcoat should match color
chip #X-24087 rather than #2430. This color was
obtained by deleting the titanium dioxide from the
original pigmentation and shading the resulting
color. The formula codes for the shaded systems
are as follows:
#2430 #X-24087
301-114-C 301-264-B
301-175-B 301-270-C
301-118-F 301-284-D
301-134-A 301-278-E
301-134-C 301-278-C
In addition to matching the new color, these formu-
lations were corrected to the proper gloss.
B. Corrosion Resistance of Reformulated Olive Drab Topcoats
It was decided to compare the reformulated topcoats
with the original coatings. In addition, the effect
of some variations in pigment volume concentration were
evaluated. The coatings tested and their variables
were:
Vr- 2i5 -
R-6-0031
Multron R-16 Midland R-6-0031Mondur CB-75 R-55 BRS-2600
1. Original PVC, color #2430 301-116-F 301-175-B 301-114-C
2. Orieinal PVC, color #X-240b7 301-312-D 301-314-A 301-315-A
3. Original PVC, color #X-2406?, 301-313-B 301-314-B 301-315-Bwitnout inert pigments
4. New PVC, color #2430 301-312-B 301-313-C 301-314-C
D. New PVC, color #X-24087 301-2b4-D 301-270-C 301-264-B
It can be seen from Table 76 that there was very
little change in galvanic corrosion resistance
wnen ttie olive drab coatings were reformulated.
At the time of tnis test, it was noted that there
was considerable variation in the appearance of the
Dow 17 treated panels. Some of the panels had a
uniform appearance while others looked spotty.
Each of these coatings was tested on both types
of substrate. Neither substrate was consistently
better than the otner. No salt spray tests were
performed.
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-279-
C. Alternate Olive Drab Pigmentation
An alternate form of pigmentation was tried using the
Midland R-55: Plaskon ST-847 vehicle. The following
pigment system was used:
Graphite 17.4%
Mapico #20 17.77.
Cadmium lithopone 24.7%
Talc 40.27%
100.07.
Coatings with pigment contents of 40 and 607. were
evaluated. Since no improvements were gained using
this pigmentation, the original pigment system was
used for the remainder of the contract.
D. Addition of Wax to Olive Drab Topcoats
Since wax had been so effective in preventing corro-
sion of the edges of tLe panels, it was decided to
add some wax to the olive drab topcoats. Petrolatum
and spermaceti were the waxes used. The coatings
containing the waxes were no better in corrosion
resistance, and in most cases worse, than the coat-
ings without wax. A coating of wax was applied
over some of the coating systems, also. Unless the
wax was applied in a very heavy coat, no improvements
were seen.
- 280 -
S. Silane Treatment of Olive Drab Pigments
Since most of the problems encountered during the
duration of this contract were galvanic corrosion
failures, it was decided to try to stop the electro-
lyte from connecting the anode and cathode electrically.
If this could be accomplished, the galvanic cell would
be short circuited and no galvanic corrosion could
occur. It was believed the electrolyte either pene-
trated the paint film by wick action directly through
pigment particles or penetrated through the pigment-
resin interface. The latter was probably a weak link
since the organophobic nature of most pigments prevents
their surfaces from being properly wetted by resins.
If either of these conditions was responsible for the
generally poor galvanic corrosion resistance shown by
most coating systems, the problem theoretically could
be solved by making the pigment surfaces more organ-
ophilic. one way of doing this is by treating the
pigments with silanes.
If a pigment is properly treated with a silane, its
surface will become extremely water repellent. Based
on the surface area of a pigment, enough silane is
used to provide a monomolecular layer. The silane
reacts chemically with the pigment, orienting itself
with the organic portion of it outward, presenting a
hydrophobic, organophilic surface.
The following procedure was used to treat all pigments:
1. The amount of silane necessary to treat each
pigment was calculated. Lampblack, for ex-
ample, with a surface area of 38 square meters
per gram would require 0.095 grams of Union
Carbide A-154 to provide a monomolecular layer
- 281 -
of silane. This figure was based on the silane
supplier's figure of 400 square meters per gram
of A-154 silane.
2. The moisture content of each pigment was adjusted
by adding water or ammonium hydroxide (as recom-
mended by the silane supplier). The water (or
ammonium hydroxide) was thoroughly distributed
throughout the pigment by placing the wetted pig-
ment in a can and tumbling for several hours on
pebble mill rollers.
3. The necessary amount of silane was then added
and the container was tumbled an additional 4
hours.
4. The pigment was removed from the can and air dried.
Pigment treated with A-154 was dried at 300OF for
1 hour to remove as much excess hydrochloric acid
as possible.
5. A small amount of the treated pigment was tested
for wettability by stirring in a beaker of water.
Only pigment not wetted by water was used.
Five silanes, Union Carbide's A-154 (methyltrichlorosilane).
A-162 (methyltriethoxysilane), Y-2525 (vinyltrimethoxysilane),
Y-2815 (amyltrimethoxysilane), and Dow Corning Sylkyd 50,
were evaluated. The A-154 silane reacted faster and more
efficiently than the other materials but the SCi liberated
reacted with some of the pigments and changed their color.
The other materials caused no undesirable changes in color
but reacted very slowly.
The treated pigments were used to prepare olive drab
topcoats. These materials were applied over primers and
evaluated for resistance to galvanic corrosion. All top-
coats prepared from silane-treated pigments failed the
bimetallic corrosion test within 150 hours.
-282 -
F. Flexibility Study of 301-284-D Topcoat
Samples of the better coatings developed during the
work on this contract were sent to the Coating and
Chemical Laboratory, Aberdeen Proving Grounds,
Maryland, for evaluation. A comment was made that
the 301-284-D olive drab topcoat was lacking in
flexibility.
Several things were tried in an attempt to improve
the flexibility of this coating. They included:
a. Increasing the amount of Multron R-16 used.
b. Varying the proportions of all ingredients.
c. Adding a plasticizer other than Multron R-16.
d. Altering the PVC of this coating.
e. Using isocyanates other than Mondur CB-75.
It was found that removing the Multron R-16 and part
of the Mondur CB-75 and catalyzing with Trancoa 560B
provided the best flexibility. A topcoat made from
this vehicle, 301-433-J, was almost perfect in galvanic
corrosion resistance. A coating very similar to
301-433-J can be made by catalyzing 301-284-D with
component C (see section B in the appendix) rather
than component B, the normal catalyst used with
301-284-D.
G. Olive Drab Topcoats Containing Miscellaneous Vehicles
Olive Drab Topcoats were prepared from a number of
miscellaneous vehicles. All were considered inferior
to the best topcoats in galvanic corrosion resistance
as can be seen from Table 77. No salt spray tests
were performed.
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- 2o5 -
Section XI
Miscellaneous Wiuite Topcoat Work
A. Effect of Various W'Uite Pigments on Corrosion Resistance
Since very few of the initial wnite topcoats showed good
corrosion resistance, it was decided to evaluate otier
wiiite pigments for improved corrosion resistance. The
pigments used were:
1. Antimony oxide
2. Zinc oxide
3. Zinc sulfide
4. Barium sulfate
5. CL.loride process titanium dioxide
These pigments are represented by ti.e symbols in Table '/.
Tae vehicles used in tiiese topcoats were:
1. Midland R-55
2. Dow Corning R-6-0031: Multron R-16: Mondur CB-75
3. Epon 1001: Dow Corning Z-6020
I;
- 286 -
Table 'b
Symbols Representing Pigments
A - Sulfate process titanium dioxide
B - Antimony oxide
C - Zinc sulfide
D - Barium sulfate
E - Chloride process titanium dioxide
F - Zinc oxide
- 287 -
The bimetallic corrosion results in Table 79 show the
following pigment systems to be better than the sulfate
process titanium dioxide pigmentation:
1. 657 sulfate type Ti02 : 35% zinc oxide
2. 50Z sulfate process Ti02 : 507 zinc sulfide
3. 100% chloride process Ti02.
B. White Topcoats Containing Same Vehicles as Best Olive
Drab Topcoats
Based on the results obtained when other white pigments
were used, some white topcoats were prepared using a
combination of chloride process titanium dioxide and
either zinc oxide, zinc sulfide, or barium sulfate.
Tne same vehicles used in the best olive drab topcoats
were used for this study. None of these materials was
any better in corrosion resistance than the same coatings
using the sulfate process titanium dioxide. Galvanic
corrosion and salt spray results can be found in
Tables 80 and 81.
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-297 -
C. Effect of Various Extender Pigments on Corrosion Resistance
All previous work on white topcoats had been done using
only talc as the extender pigment. In addition, the
pigment content had been kept constant at 53% by weight.
It was then decided to evaluate a number of inert pigments
at a wide range of pigment contents. The following
extender pigments were chosen for evaluation:
(1) calcium carbonate
(2) micronized talc
(3) Cab-O-Sil
(4) Santocel 54
(5) Syloid 162
Pigment content was varied from 20 to 70% by weight.
The bimetallic corrosion results in Table 82 indicate
the following combination of inert pigments and pigment
contents to be better than the initial combination:
(1) Talc at 70 or 53% pigment
(2) Santocel 54 or Syloid 162 at 20% pigment
Only a representative number of these coatings were
tested for salt spray resistance. The coatings were
all very similar in salt spray performance as can be
seen in Table 83.
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-303-
D. Addition of Chromate and Aluminum Pigments to White
Topcoats
Since the chromate pigments seemed to inhibit corrosion
when used in primers, it was decided to add small quanti-
ties of chromates to some of the white topcoats. A series
was also prepared with an addition of 17. aluminum pigment,
based on total pigment. In the case of the chromates,
3% of the chromate pigments were used. All of these
coatings were somewhat yellow in color.
The results of bimetallic corrosion testing contained in
Table 84 show none of these coatings to be substantially
better than the corresponding coatings without the
chromate or aluminum pigments.
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- 306
E. White Topcoats Containing Same PVC as Olive Drab
Topcoats
Since all the original white topcoats had pigment
volume concentrations considerably lower than the
olive drab topcoats, it was decided to prepare some
white topcoats which had PVC's equal to the olive
drab topcoats.
The olive drab coatings, as can be seen from Table 85
were better in galvanic corrosion resistance than the
corresponding white materials. The white topcoat made
from the R-6-0031: BRS-2600 was a dark buff in color
and developed cracks while drying.
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- 308 -
F. Previously Eliminated White Topcoats
Since the study of various white and extender pigments
indicated the initial pigmentation used in the white
topcoats might not be optimum, some of the white topcoats
'9 which originally were borderline in performance were
re-evaluated with the new pigmentation. The vehicles
in these topcoats were:
(1) Dow Corning R-6-0031: k" RS Nitrocellulose
(2) Dow Corning DC-805: k" Cellulose Acetate Butyrate
(3) General Electric SR-82: Formvar 7/70
While the galvanic corrosion resistance of some of
these white coatings was marginally better than that
of the original coatings, not enough improvement was
shown to warrant further testing. Galvanic corrosion
results can be found in Table 86.
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- 315 -
C. Silane Treatment of White Pigments
As in the case of the olive drab pigments, sulfate
process titanium dioxide was treated with silanes.
Once again topcoats made from the treated pigments
were inferior in galvanic corrosion resistance to
coatings made from untreated pigments. Coatings
containing pigments whicn had been treated by the
silane supplier were equally unsatisfactory.
H. White Topcoats Made from Miscellaneous Vehicles
A number of miscellaneous vehicles were used to
prepare white topcoats. None of these coatings
were considered satisfactory. Bimetallic corrosion
results may be found in Table 87.
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- 318 -
Section XII
Miscellaneous Testing
A. Optimum Thickness of Primer and Topcoat
As mentioned earlier, both primers and topcoats were
applied at thicknesses of 0.0015". It was decided to
try one system with thicknesses of 0.0005", 0.0010",
and 0.0015" for both primer and topcoat. The primer
chosen was the 301-103-A Midland R-55 system while
the topcoat was the olive diab coating made from
the same vehicle. It was determined that any thick-
ness of topcoat would be satisfactory if 0.0015" of
primer was used. In addition, if the heaviest thick-
ness of topcoat is used, 0.0010" of primer will produce
a satisfactory coating. While it is apparent that a
thickness less than 0.0015" for both primer and topcoat
may not be necessary for optimum protection, it is
believed desirable to use as heavy a coating as possible
for best results.
B. Exterior Exposure Panels
Some of the preferred olive drab systems were applied
to a variety of substrates and exposed at the following
test sites:
1. South Florida
2. South Florida Tidewater
3. Waukegan, Illinois
1 - 319-
The coating systems exposed were:
Primer Topcoat
1. 301-103-A 301-270-C
2. 301-103-A 301-284-D
3. 301-275-E 301-270-C
4. 301-275-E 301-284-D
5. 301-275-E 301-264-B
6. 407 wash primer 301-270-C
7. 407 wash primer 301-284-D
8. 407 wash primer 301-264-B
The following substrates were used for the testing:
1. Dow 17 treated HK-31 magnesium alloy.
2. 24ST aluminum alloy.
3. Cold rolled steel.
4. Bonderite 1000 treated cold rolled steel.
5. Dow 17 treated HK-31 magnesium alloy coupled
with 24ST aluminum alloy.
6. Dow 17 treated HK-31 magnesium alloy coupled
with cold rolled steel.
These panels are presently being tested. After 12 months
exposure, the following developments have occurred:
1. The 600 gloss on all panels has decreased from
around 25o to 00.
2. All panels have developed a heavy bronzing.
-320-
3. All coatings have shown medium to pronounced
fading.
4. Film integrity of all coatings is excellent.
C. Evaluation of Clear Coatings
Since a great deal of time is necessary to prepare
pigmented coatings, it was decided to check the possibility
of testing a promising vehicle as a clear over primers for
resistance to galvanic corrosion. Only those vehicles
which performed well in the clear would then be made into
pigmented coatings. This idea was tried and it was felt
that it would be satisfactory for any future galvanic
corrosion testing.
It was also decided to evaluate some of these clear
coatings over some of the better white topcoats. To
obtain the necessary low gloss, however, some Syloid 162
was used to flat these clears. The flatted clears were
susceptible to water penetration and consequent galvanic
corrosion failure.
D. Riveted Bimetallic Panels
Since all bimetallic corrosion testing had been done
using the galvanic "cells", it was believed desirable4
to prepare some coupled panels and test them for
resistance to 5. salt spray. Panels were prepared
coupling Dow 17 treated HK-31 magnesium panels with
either cold rolled steel or 24ST aluminum alloy panels.
• •, ~~j~-i....
SI- 321
The panels were fastened with 5056S aluminum alloy
rivets. It was impossible, when coupling the panels
in this manner, to completely eliminate the air space
between the panels where the two metals lapped. It was
also impossible to cover this space when applying the
primer and topcoat by spray.
Panels joined in this manner were sprayed with some of
the preferred coating systems and placed in a 5% salt
spray cabinet. All failed within 48 hours due to severe
corrosion of the magnesium. In each case the corrosion
occurred at the unprotected lapped portion of the panel.
Duplicate panels were prepared. This time, however, some
unreduced primer was placed in a syringe and applied to
the problem area. The panels were primed, topcoated, and
tested as before. There was a dramatic improvement in
results. (See figs. 11 and 12) Almost all systems
developed no more than a few small blisters within 500
hours. Most coupled panels on exterior exposure testing
were protected in this manner.
E. Baked Coatings
While the provisions of this contract call for an air
dry coating, it was agreed that we should bake some of
the preferred systems to determine if baking would
improve their corrosion resistance. A cure of 15
minutes at 3500 F. was chosen. In all cases, only the
301-275-K primer was used.
- 322 -
The 301-284-D and 301-270-C systems were improved
only slightly by the bake. The 3 01- 2 64-A system
was unaffected after 500 hours in the galvanic
cell, however. The 3 01-284-D system also was
perfect when cured 30 minutes at 4000 F.
-323 -
FIG. 11
Fig. 11
5% SALT SPRAY RESULTS (ON MAGNESIUM-STEEL COUPLED PANELS)
OF OLIVE DRAB COATING SYSTEM WITHOUT AND WITH PROTECTION
OF LAPPED AREA
upA
r -324 -
Fig. 12
5% SALT SPRAY RESULTS (ON MAGNESIUM-STEEL COUPLED PANELS)
OF WHITE COATING SYSTEM WITHOUT AND WITH PROTECTION
OF LAPPED AREA.
- 325 -
F. Final Testing of Preferred Systems
All of the promising coating systems developed
were, of course, subjected to bimetallic and
salt spray corrosion testing. In addition, they
were tested for resistance to MIL-S-3136 fluid and
diester lubricant. The coatings were also tested for
heat stability. The results of these tests can be found
in Table 88.
All of these coating systems are regarded as having
satisfactory resistance to the test fluids.
Those coatings which soften in the fluids soften
only slightly and recover full hardness within 24
hours. The coatings which are indicated as being
satisfactory for heat resistance are so rated
because no flaking of the coating has occurred.
Most of them, however, do become quite inflexible
but are still not easily removed from the substrate.
The 301-360-F material became very dark brown in
color and the 301-368-F coating was only slightly
less dark. All of the olive drab coatings will
withstand 2 hour exposures to temperatures as
high as 6000 F. without flaking off the panel
although their film integrity is definitely
adversely affected by the increase in temperature.
-328-
Section XIII
Additional Resaearch
The preceding sections of the report cover the work
done during the contracted time. It was decided that
several promising areas required additional work and
the contract was extended for the necessary time.
A. Vinyl Coatings
Bakelite's XYHL, VAGH, and QYNV were screened in
clear coatings. The XYHL and VAGH were combined
with an isocyanate and/or tetrabutyl titanate.
The results of the screening may be found in
Table 89.
9. Epoxy Coatings
The complete range of epoxy resins was catalyzed
with varying amounts of an isocyanate. Screening
test results may be found in Table 90.
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334 -
C. Silicone-Polyester Coatings Catalyzed with
Isocyanates and Amines
Since we had earlier found a silicone-polyester
catalyzed with an isocyanate to produce a coating
with most of the properties needed, some additional
testing was done in this area. Two experimental
silicone-polyester copolymers were catalyzed with
Mondur CB-75 and screened in the usual manner. In
addition, Dow Corning Z-6020 aminosilane and
triethylamine (TEA) were also evaluated as catalysts.
The test results may be found in Table 91.
D. Miscellaneous Materials
A number of otner polymers were also screened. Some
of these were chosen because similar types of materials
had previously performed well. Others were included
because ta'eir chemical type had not been studied
before and their omission would prevent this contract
from being as complete as it could be.
' -I
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-338-
Included in the latter group are some materials not
normally associated with coatings. In many cases
it was necessary to use unusual solvents or to apply
the coatings from dispersion to obtain continuous
films. Some materials also required the use of heat
but for preliminary screening purposes were not
eliminated for this reason. Attempts were made to
obtain inorganic polymers but these materials were
unavailable. The screening results may be found in
Table 92.
E. Bimetallic Corrosion and Salt Spray Testing of Primers
and Clear Coatings
A number of the clear coatings in sections XIII A-D
(above) were believed worthy of additional testing.
These materials were evaluated in the normal manner
for resistance to galvanic corrosion. The clears
were tested over unprimed Dow 17 treated HK-31
magnesium alloy and/or over the same substrate
primed with 301-275-E calcium chromate primer. In
addition some of these resin systems were incorporated
into calcium chromate primers. Some isocyanate
S4 catalyzed silicone copolymers were also tested in the
galvanic cells. The silicone copolymers include
Midland X-4641, X-4646, X-4664, X-4649, X-4661,
X-4676, Dow Corning XR-6-0066, XR-6-0059, and
JM-6-0041. Galvanic corrosion test results may
be found In Table 93.
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F-348Some of these coatings were also applied to Dow 17
treated HKC-31 magnesium alloy and tested for
resistance to 5% salt spray. Salt spray exposure
results may be found in Table 94.
A number of other primer type coatings were evaluated.
These included the following:
1. International Rustproof Irco LOAX. 1011 and
Irco 9301. These materials were used as additives
in the silicone-epoxy: polyamide primer.
2. Hercules Powder Co. Rosin Amine D. This
material was added to the same primer.
3. Amercoat Corporation Dimetcote #4 zinc silicate
coating.
4. Napko Corporation Zacrote #1360 zinc silicate
coating.
5. Union Carbide Ucar R-101 and R-104 silicone metal
treatments. These materials were used as an under-
coat for the silicone-epoxy: polyamide primer.
The Dow Corning R-6-0031: Mondur CB-75 white
topcoat was used.
Bimetallic corrosion testing results may be found in
Table 95.
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-352-
F. Bimetallic Corrosion Testing of Olive Drab and
White Topcoats
Several of tite vehicles mentioned in the preceding
sections were incorporated into olive drab and white
Stopcoats and evaluated for resistance to galvanic
corrosion. In each case, the 301-275-E silicone-
epoxy calcium cnromate primer was used. Some of
the coatings tested were the preferred materials
developed earlier in the contract. Many of these
coatings were baked to determine their optimum
corrosion resistance. Bimetallic corrosion testing
results may be found in Tables 96 and 97.
G. Bimetallic Salt Spray Testing of White Coating Systems
Since the Union Carbide UCAR R-10 and R-104 metal
treatments seemed to inhibit galvanic corrosion, some
riveted panels were prepared for salt spray testing.
Each coating system consisted of either UCAR R-101
or R-104, followed by 301-275-E silicone-epoxy:
polyamide primer, and topcoated with 301-368-F
silicone-polyester: polyurethane white topcoat.
Magnesium panels were coupled with steel or aluminum
panels. Two panels of each variation were prepared,
I one being coated in the normal manner and the other
having the lapped area protected with a layer of
unreduced primer. The bimetallic salt spray corrosion
results may be found in Table 98.
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358 -
Section MIV
A. Summary
The following is a summary of results of work done on
this contract:
1. 301-275-E silicone-epoxy copolymer primer is the
preferred primer. 301-103-A silicone-epoxy ester
primer is not as highly recommended because of
three problems:
a. Adnesion of topcoats to this primer is far inferior
to the adhesion of topcoats to the 301-275-E primer.
b. This primer is far more sensitive to lifting which
may be caused by any strong solvents present in
the topcoats.
c. The cure of this primer is quite variable which
causes inconsistencies in recoatability, performance,
etc.
2. The following olive drab topcoats, listed in order of
preference, are the best that were developed:
a. 301-2t4-D silicone polyurethane
b. 301-270-C epoxy ester
c. 301-264-B silicone phenolic
d. 301-278-C silicone-epoxy copolymer
e. 301-278-E silicone-epoxy copolymer
, I
V"-359 -
3. Although no completely satisfactory white topcoat
has been developed, the following are superior to
"others tested:
a. 301-360-F epoxy ester
4( b. 301-368-F silicone polyurethane
Formulas for all coatings are listed in the appendix.
4. It is believed that galvanic corrosion resistance is
directly related to panel preparation. If coupled
panels are properly protected around the lapped areas
by the unthinned coating of primer, all the coating
systems are satisfactory. If, however, no special
precautions are taken, no coating will protect the
magnesium from early failure.
B. Acknowledgement
The authors wish to acknowledge the invaluable suggestions and
advice given to them throughout the contract by Dr. William D.
Coder, Research Supervisor. They also wish to thank Mr.
George K. Hughes, Section Head, Resin Research Laboratory,
for the preparation of the experimental polymers used in this
program.
L&
- 361 -
A. Bibliography
1. Fitzgibbon, C.R., Miller, E.H., and Glaser,
M.A., High Temperature Protective Coatings
for Magnesium, Wright Air Development Center
(1957).
!111
1 -362-
B. Formulations of Preferred Coatings
All compositions are by weight and represent 100
gallons.
Primers
4301-103-A Zinc Chromate Primer
Midland R-55 @507% NVM 450
Plaskon ST-847 @507% NVM 150
Imperial X-883 Zinc Chromate 163
Xylene 140
6% Cobalt Naphthenate 0.9
57. Calcium Naphthenate 1.5
47. Rare Eartn Naphthenate 0.9
Exkin #1 (Nuodex) 1.3
Nilskin (Naftone) 1.3
908.9
Weight per gallon - 9.09 pounds
Recommended thinners - Aromatic hydrocarbons
LiA
I 363
331-2Y5-E Calcium Chromate Primer
Component A
Dow Corning XR-6-0000 @bO NVM 734
Mineral Pigments #1376 Calcium Chromate 314
National Lead Bentone 27 5
, To luene 12.5
Cellosolve 15
Methyl Isobutyl Ketone 12.5
1093.0
Weignt per gallon - 10.93 pounds
Component B
General Mills Versamid 115 @100% NVM 157
General Electric SR-82 @60% NVM 23
Toluene 177
Cellosolve 213
Methyl Isobutyl Ketone 171
747
Weight per gallon - 7.47 pounds
Mix one volume component A with one volume component B
just prior to application.
Recommended thinner - Toluene 125 parts by weight
Cellosolve 150 parts by weight
Methyl isobutyl ketone 125 parts by weight
LA
1 -364-
Topcoats
301-264-D Silicone Polyuretnane Olive Drab Topcoat
Component A
Imperial X-1810 C.P. Chrome Yellow Medium 226
N.J. Zinc XX-50 Zinc Oxide 63
Mapico #516 Dark Red Iron Oxide 149
C.K. Williams Superjet Lampblack 53
#282 Clay 73
Johns Manville Celite #289 19
Davison Chemical Syloid 162 21
National Lead Bentone 27 5
Dow Corning R-6-0031 @507. NVM 487
Mobay Multron R-16 @100% NVM 56
Methyl Isobutyl Ketone 130
Dow Corning Paint Additive #1 1.5
1283.5
Weightr per gallon - 12.84 pounds
Component B
Mobay Mondur CB-75 @75% NVM 243
Methyl Isobutyl Ketone 275
Cellosolve Acetate (Polyurethane Grade) 275
793
Weight per gallon - 7.93 pounds
Equal volumes of Components A and B should be mixed Just
before using.
Recommended thinners - Methyl isobutyl ketone or a mixture
of methyl isobutyl ketone and aromatic hydrocarbons.
LA
V -365 -
If more flexibility is desired, the following catalyst
system might be used:
Component C
Trancoa Chemical Tranco 560B 060% NVM 440
Mobay Mondur CB-75 075% NVM 56
Methyl Isobutyl Ketone 176
Cellosolve Acetate (Polyurethane Grade) 176
848
Weight per gallon - 8.48 pounds
Equal volumes of Components A and C should be mixed just
prior to application.
Recommended thinners - Methyl isobutyl ketone or a blend
of methyl isobutyl ketone and aromatic hydrocarbons.
Catalyzing component A with component C (rather than
the usual catalyst, component B) will result in a more
flexible coating, similar to 301-433-J (see section X.F.
page 282)
lA
- 366 -
301-270-C Epoxy Ester Olive Drab Topcoat
Imperial X-l810 C.P. Chrome Yellow Medium 120
N.J. Zinc XX-50 Zinc Oxide 35
Mapico #516 Dark Red Iron Oxide 62
C.K. Williams Superjet Lampblack 26
#282 Clay 39
Jonns Manville Celite #269 11
National Lead Bentone 27 3
Midland R-55 @507. NVM 548
Xylene 158
67. Cobalt NapLithenate 0.7
57% Calcium Napntnenate 1.3
47. Rare Eartr, Naphtuienate 0.7
Exkin #1 (Nuodex) 1.1
Nilskin (Naftone) 1.1
Dow Corning Paint Additive #1 1.0
1007.9
Weight per gallon - 10.08 pounds
Recommended thinners - Aromatic hydrocarbons
4
! 4.
t-I
- 367 -
301-264-B Silicone Phenolic Olive Drab Topcoat
Imperial X-1810 C.P. Chrome Yellow Medium 172
N.J. Zinc XX-50 Zinc Oxide 41
Mapico #516 Dark Red Iron Oxide 85
C.K. Williams Superjet Lampblack 33
#282 Clay 47
Johns Manville Celite #289 12
National Lead Bentone 27 5
Dow Corning R-6-0031 @507. NVM 318
Bakelite BRS-2600 @557. NVM 289
Dow Corning Paint Additive #1 1
Methyl Isobutyl Ketone 126
1129
Weignt per gallon - 11.29 pounds
Recommended thinner - methyl isobutyl ketone.
I•
- 368 -
301-276-C Silicone Epoxy Olive Drab Topcoat
Component A
Imperial X-1810 C.P. Chrome Yellow Medium 224
Red Lead 119
N.J. Zinc XX-50 Zinc Oxide 64
Mapico #516 Dark Red Iron Oxide 88
C.K. Williams Superjet Lampblack 43
#282 Clay 74
Jo•ins Manville Celite #289 19.5
National Lead Bentone 27 3.5
Dow Corning XR-6-0000 @60% NVM 416
Toluene 81
Cellosolve 97
Methyl Isouutyl Ketone 81
1310.0
Weignt per gallon - 13.10 pounds
Component B
General Mills Versamid 115 @100% NVM 83
Toluene 204
Cellosolve 245
Methyl Isobutyl Ketone 204
736
Weignt per gallon - 7.36 pounds
Mix equal volumes of components A and B just prior to
application.
Recommended thinner -
Toluene 125 parts by weight
Cellosolve 150 parts by weight
Methyl isobutyl ketone 125 parts by weight
- 369-
301-278-E Silicone Epoxy Olive Drab Topcoat
Component A
Imperial X-1810 C.P. Chrome Yellow Medium 222
Red Lead 118
N.J. Zinc XX-50 Zinc Oxide 64
Mapico #516 Dark Red Iron Oxide 87
C.K. Williams Superjet Lampblack 43
#282 Clay 73
Johns Manville Celite #289 19.5
National Lead Bentone 27 3.5
Midland X-4209 @62.5% NVM 412
Toluene 60
Cellosolve 96
Methyl Isobutyl Ketone 80
1298.0
Weight per gallon - 12.98 pounds
Component B
General Mills Ver3amid 115 @1007 NVM 86
To luene 204
Cellosolve 245
Methyl Isobutyl Ketone 204
739
Weight per gallon - 7.39 pounds
Mix equal volumes of components A and B just before
application.
Recommended thinner -
Toluene 125 parts by weight
Cellosolve 150 parts by weight
Methyl isobutyl ketone 125 parts by weight
- 370-
301-360-F Epoxy Ester White Topcoat
DuPont Ti-Pure R-610 264
Davison Chemical Syloid 162 27
Midland R-55 @50%. NVM 506
Methyl Isobutyl Ketone 206
67. Cobalt Naphthenate 0.3
5% Calcium Naphthenate 0.5
47 Rare Earth Naphthenate 0.3
Exkin #1 (Nuodex) 0.4
Nilskin (Naftone) 0.4
1004.9
Weight per gallon - 10.05 pounds
Recommended tninners - Aromatic hydrocarbons
h,,
- 371 -
301-368-F Silicone Polyurethane White Topcoat
Component A
DuPont Ti-Pure R-610 261
Micronized Talc 142
Dow Corning R-6-0031 @507. NVM 725
Mobay Multron R-16 @100% NVM 35
1163
Weight Per Gallon - 11, 63 pounds
Component B
Mobay Mondur CB-75 @757. NVM 99
Methyl Isobutyl Ketone 334
Cellosolve Acetate (Polyurethane Grade) 334
767
Weight per gallon - 7.67 pounds
Mix equal volumes of components A and B just prior to
application.
Recommended thinners - Methyl isobutyl ketone or a
mixture of methyl isobutyl ketone and aromatic
hydrocarbons.