Water Spot Analysis – RhinoHide®

Separator

C. La, and R.W. Pekala

ENTEK International LLC

January 9, 2012
 Background
 “Water spots” found on ENTEK GE separators
◼ Dark spots present on every lane across the web
 The spots are present on separators manufactured on all production lines through
out the entire run time.
 Washing separator samples that have water spots in boiling water or in solvent
followed by drying doesn’t eliminate them.

Water spots

Figure 1: Example of “water spots” on RhinoHide® separator

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 Background (cont.)

 These water spots develop in the drying step during the

production:
◼ Steam is sprayed on the separator web which is soaked with solvent in
the dryer.
◼ Small droplets of condensate are collected on the web and are carried
to the oven.
◼ Evaporation of the water droplets leaves behind darker spots at these
sites. These are so called “water spots.”
 Analysis tools:
◼ Scanning Electron Microscopy (SEM)
◼ Energy Dispersive X-ray spectroscopy (EDX)
◼ Thermo Gravimetric Analysis (TGA)

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 SEM Analysis - Surface

 The surface of the water spots were examined using SEM:

◼ The microscopic structure of the separator at the surface of the spots
appears normal.

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 SEM Analysis - Fractured

 The water spots were fractured along the MD, and the bulk
structure was examined with SEM:
◼ The microscopic structure of the separator at the water spots doesn’t
deviate from observations on normal area.

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 EDX Analysis
Element Atomic Weight% Weight% Sigma Element Atomic% Weight% Weight% Sigma
C % 38.2 26.62 0.35 C 47.32 35.3 0.25
O 38.83 36.04 0.24 O 40.73 40.47 0.22
Na 0.28 0.37 0.03 Na 0.21 0.3 0.03
Si 22.68 36.96 0.2 Al 0.05 0.08 0.02
Totals 100
Si 11.35 19.79 0.1
Table 1: Elements detected at the surface of a water spot
Sn 0.01 0.08 0.03
Yb 0 -0.01 0.04
Au 0.33 3.99 0.09
Totals 100
Table 2: Elements detected at the fracture of a water spot

 EDX was performed on the surface and fracture at the water spots:
◼ Samples were coated with gold prior to analysis, resulting in high Au
concentration.
◼ Some Na is present at the water spots, but at a very small concentration.

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 TGA – Water Spots vs. Normal Area

Moisture (%) Residual Oil (%) PE (%) SiO2 (%) SiO2/PE (%)
Water Spot 2.9 16.7 23.1 55.8 2.41
Normal Area 2.6 16.6 23.2 56.0 2.41

 TGA was performed on water spots and normal area next to

the water spots:
◼ Both regions show similar composition.

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 Inducing Water Spots in the Lab

 Oil filled ENTEK GE separator samples were extracted in

solvent to approximately 15% residual oil.
 After removal from the solvent, droplets of DI water at room
temperature was dropped onto the surface of the extracted
samples which were still wet with solvent.
 After drying in a convective oven at 90°C, there were dark
spots at the sites where the droplets were occupied.
 These water spots were not eliminated after washing in
boiling water or in solvent.

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 Inducing Water Spots in the Lab (cont.)

solvent wet sample Drying sample with

solvent wet water droplets
with water
sample
droplets

Water spots on
back side Water spots

Water penetrated through the sample,

resulting in water spots on the back side

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Summary

 Water spots found on ENTEK GE separators emerge from the

drying step during the separator production:
◼ Evaporation of minute droplets of water leaves behind darker spots.

 There is NO obvious structural or compositional change at the

water spots when compared to the normal area.

 The cause for differences in the optical characteristics (i.e.,

coloration) of water spots is still under investigation.

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