UNCLASSIFIED 2 62 93 - dtic.mil · 22. Epoxy-Polyamide (General Hills Genamid 310) Resina System~s....

UNCLASSIFIED

AD4 2 62 93

DEFENSE DOCUMENTATION CENTERFOR

SCIENTIFIC AND TECHNICAL INFORMATION

CAMERON STATION, ALEXANDRIA, VIRGINIA

UNCLASSIFIED

NOTICE: When government or other drawings, speci-fications or other data are used for any purposeother than in connection with a definitely relatedgovernment procurement operation, the U. S.Government thereby incurs no responsibility, nor anyobligation whatsoever; and the fact that the Govern-ment may have forxm2lated, furnished, or in any waysupplied the said drawings, specifications, or otherdata is not to be regarded by implication or other-wise as in any manner licensing the holder or anyother person or corporation, or conveying any rightsor permission to manufacture, use or sell anypatented invention that may in any way be relatedthereto.

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.

Butadiene Acrylonitrile (Naugatuck Paracril CV) 70-72


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.

Triazine Formaldehyde (Rohn and Haas Uformite M-311) 122

Modification d Fluorinated Hydrocarbon Resins.

34. Polyvinyl Formal (Shawinigan Foravar 7/70) Modification 124


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.

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

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


F. Triazine Formaldehyde (Robin and Haas Uformite M-311) 37


G. Polyvinyl Formal (Shawinigan Formvar 7/70) 37


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


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


S. Polyvinyl Butyral (Bakelite XYHL) Modification of 111


T. Acrylic (Rohm and Bass Acryloid A-101) Modification 116


U. Styrene Butadiene (Goodyear Pliolite S-5) Modification 116


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


B. Pigmentation 155

C. Preparation of Panels. 156

D. Bimetallic Corrosion and Salt Spray Testing. 156

Section VI Development of White Topcoat


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




5. General Electric SR-98 (now CR-116)




9. Dow Corning DC-802



12. Dow Corning DC-806A


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



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


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


II,

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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


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


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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


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


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- 56 -

J. Oxidizing Alkyd (Midland R-9) Modification of Silicone Resins


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.


5. For details of Midland R-9 modifications of silicone


K. Oxidizing Alkyd (Midland R-50) Modification of Silicone Resins


was limited.

2. Resistance to the test fluids was slightly better than

coatings containing Midland R-9, but was still

unsatisfactory.


4. For details of Midland R-50 modification of silicone


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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.


3. Some of the coatings containing 75. Paracril CV

decomposed at 5000 F.

4. For details of Paracril CV modifications of silicone


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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


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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.



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.


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.


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.



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.



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.

-'-4

Fig. I

MOUNTING OF BIMETALLIC CORROSION TEST PANELS

- 136-

FIG. 2

t I

Fig. 2

BIMETALLIC CORROSION TEST CELL

- 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


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.

II

1-4

Fig. 7

EXAMPLES OF GOOD AND POOR ADHESION

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- 167 -

Section VI

Development of White Topcoat


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-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-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

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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


24. 75. Jones-Dabney Epitex 148625% 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




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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FIG. 9

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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.

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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.



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:

- 274 -

I

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.

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-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.

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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


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


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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&

- 360-

Section XV

Appendix

- 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


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


Dow Corning R-6-0031 @507. NVM 487

Mobay Multron R-16 @100% NVM 56


Dow Corning Paint Additive #1 1.5

1283.5

Weightr per gallon - 12.84 pounds

Component B

Mobay Mondur CB-75 @75% NVM 243


Cellosolve Acetate (Polyurethane Grade) 275

793


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



848


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




#282 Clay 39

Jonns Manville Celite #269 11


Midland R-55 @507. NVM 548

Xylene 158

67. Cobalt NapLithenate 0.7

57% Calcium Napntnenate 1.3

47. Rare Eartr, Naphtuienate 0.7



Dow Corning Paint Additive #1 1.0

1007.9


Recommended thinners - Aromatic hydrocarbons

4

! 4.

t-I

- 367 -

301-264-B Silicone Phenolic Olive Drab Topcoat





#282 Clay 47

Johns Manville Celite #289 12



Bakelite BRS-2600 @557. NVM 289

Dow Corning Paint Additive #1 1


1129


Recommended thinner - methyl isobutyl ketone.

I•

- 368 -

301-276-C Silicone Epoxy Olive Drab Topcoat

Component A


Red Lead 119




#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


Component B

General Mills Versamid 115 @100% NVM 83

Toluene 204

Cellosolve 245


736


Mix equal volumes of components A and B just prior to

application.

Recommended thinner -

Toluene 125 parts by weight



- 369-

301-278-E Silicone Epoxy Olive Drab Topcoat

Component A


Red Lead 118




#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


1298.0


Component B

General Mills Ver3amid 115 @1007 NVM 86

To luene 204

Cellosolve 245


739


Mix equal volumes of components A and B just before

application.

Recommended thinner -

Toluene 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


67. Cobalt Naphthenate 0.3

5% Calcium Naphthenate 0.5

47 Rare Earth Naphthenate 0.3



1004.9


Recommended tninners - Aromatic hydrocarbons

h,,

- 371 -

301-368-F Silicone Polyurethane White Topcoat

Component A

DuPont Ti-Pure R-610 261

Micronized Talc 142


Mobay Multron R-16 @100% NVM 35

1163

Weight Per Gallon - 11, 63 pounds

Component B

Mobay Mondur CB-75 @757. NVM 99



767


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.

UNCLASSIFIED 2 62 93 - dtic.mil · 22. Epoxy-Polyamide (General Hills Genamid 310) Resina System~s....

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Transcript of UNCLASSIFIED 2 62 93 - dtic.mil · 22. Epoxy-Polyamide (General Hills Genamid 310) Resina System~s....