
|
|
|
Figure 1. Results of 200 h corrosion tests on: Left) Commercial chromate-free Boegel conversion coating, Right) Alodine chromate containing coating. |
|

|
|
|
Figure 2. OMs of scored portion of samples after 200 h corrosion test on: Left) Boegel conversion coating, Right) Alodine coating. |
|
|
|
Four of our chromate-free SQ coating systems outperformed the commercial chromate-free conversion coating, Figures 3 and 4. Optical micrographs (OMs) of scores are shown in Figure 4. |
|
|

|
|
|
Figure 3. Results of 200 h corrosion test on SQ coating systems: A) SQ1, B) SQ2, C) SQ3, D) SQ4 |
|
|

|
|
|
Figure 4. OMs of scores from 200 h corrosion test on SQ coating systems: A) SQ1, B) SQ2, C) SQ3, D) SQ4 |
|
|
|
Figures 5 and 6 show that two of our chromate-free SQ coating systems also had corrosion inhibiting properties similar to the chromated coating, Alodine. Micrographs of the region near a score of these coating systems are shown below in Figure 6. |
|
|

|
|
|
Figure 5. Results of 200 h corrosion test on SQ coating systems: Left) SQ5, Right) SQ6 |
|
|

|
|
|
Figure 6. OMs of 200 h corrosion test on SQ coating systems: Left) SQ5, Right) SQ6 |
|
|
These latter two systems offer properties superior to the other Mayaterials systems but it is possible to also add epoxy and amine functionality to the surfaces of these coatings making it potentially possible to produce a conversion and primer coating in one step. Patents are pending.
Hardness Pencil hardness tests are conducted according to ASTM D 3363 using an Elcometer 501 PHT. By optimizing the composition of these systems, we are able to achieve the highest measurable pencil hardness for all systems. The scale for measure pencil hardness is:
6H > 5H-H > F > HB > B-5B > 6B
Table 1. Pencil hardness for all SQ based conversion coatings
Coating |
Hardness |
SQ1 |
≥ 6H |
SQ2 |
≥ 6H |
SQ3 |
≥ 6H |
SQ4 |
≥ 6H |
SQ5 |
≥ 6H |
SQ6 |
≥ 6H | |
Adherence To ensure proper adherence of the coating to a substrate’s surface, one-point bend tests are run according to ASTM D 552 Method B. Figure 7 provides a typical test result after a 200 h salt corrosion test. The coating is free from adhesion and cohesion failure meaning there is no cracking, crazing, or buckling of the coating on the bent surface. |
|
 |
|
|
Figure 7. Typical passing result from one point bend test on typical SQ coating |
|
|
|
Epoxy Primer Coating Systems
Mayaterials’ silsesquioxanes offer considerable potential to develop highly adherent epoxy coatings with tailored properties. For example we can tailor CTEs, hardness and hydrophobicity. With our Janus cube systems we can also make multilayer materials. Their high thermal stability coupled with the ability to tailor properties at nanometer length scales makes them ideal for such applications including novel internal/external aircraft coatings, barrier coatings, no-flow flip-chip underfills, matrices for fiber reinforced composites, and many others.
Below are some of the epoxy systems we have developed. All current resin systems employ octaaminophenylsilsesquioxane (OAPS) as the curing agent. In the near future, we will greatly increase our catalog of coatings systems to include still lower viscosity epoxy systems, isocyanates and other related coating materials. |
|

|
|
|
Formulation Resins are formulated using OAPS (Ph-6), and OG (Q-4) and OC (Q-5) or one of the above epoxy compounds in a 1:1 epoxy to NH2 stoichiometry. Properties can be tailored by using one type of epoxy or mixtures of one or more, as suggested, but not limited to those shown below in Table 2. |
|
Table 2. Coating Name Abbreviation Definitions
Coating |
Constituents |
OAPS-DGEBA |
OAPS and DGEBA |
OAPS-OG |
OAPS and OG |
OAPS-DGEBA+ |
OAPS and ¾ DGEBA, ¼ OG |
OAPS-OG+ |
OAPS and ¼ DGEBA, ¾ OG |
OAPS-Z |
OAPS and ½ DGEBA, ½ OG |
OAPS-TGMX |
OAPS and TGMX |
OAPS-Os |
OAPS and ½ OG, ½ OC | | |
|
|
Coating Properties and Testing After the coatings are completely cured (2-7 d), we test them to both Boeing spec and Milspec for such properties as hardness, adhesion, and chemical and corrosion resistance. The results from some of these tests are shown below in Tables 3-5. |
|
Table 3. General Properties of OAPS Coatings
Property |
OAPS Coating Characteristic |
Color |
Transparent; slightly yellow |
Drying Time |
Tack free, 6 h at 19±2°C |
Curing Time |
90% hardness, 4 d at 19±2°C |
Viscosity |
16.5 s in Zahn #2 Cup | |
|
 |
Table 4. Pencil hardness, dry, wet, and bend adhesion for several OAPS coatings
|
Hardness |
Dry Adhesion |
Wet Adhesion |
Bend Adhesion |
|
ASTM |
Boeing |
ASTM |
Boeing |
|
Spec* |
1H-2H |
4B |
7 |
4B |
7 |
4 |
OAPS-DGEBA |
2-3H |
4B |
8 |
4B |
8 |
1 |
OAPS-OG |
F-1H |
4B |
8 |
2B |
4 |
4 |
OAPS-DGEBA+ |
3-4H |
5B |
10 |
3B-4B |
7 |
3 |
OAPS-OG+ |
3-4H |
4B |
8 |
3B-4B |
7 |
3 |
OAPS-Z |
3-4H |
5B |
10 |
4B-5B |
9 |
4 |
OAPS-TGMX |
6H |
5B |
10 |
5B |
10 |
4 |
OAPS-Os |
F |
5B |
10 |
5B |
10 |
4 | |
|