TECHNOLOGIES>FASTENERS

Epoxies and adhesives fit for

space
Key points: Space is a harsh environment for all materials, including adhesives and
epoxies. Adhesives and epoxies used for space applications should have low-
outgassing levels. ASTM E595 is the standard test for determining outgassing levels.

Robert Michaels, Vice President, Technical Sales, Master Bond Inc. | Jul 09, 2013

Satellites and spacecraft must survive and operate in an environment entirely different
from that on Earth. There is no atmosphere to protect them from radiation or provide a
blanket of warmth. Instead, they must put up with extreme hot and cold temperatures,
exotic forms of some common materials and elements, and high vacuum conditions. For
some space-bound components, such as propulsion subsystems and certain
experimental devices on the International Space Station, they must withstand exposure
to cryogenic temperatures as low as 4°K. These factors impose a strict set of constraints
on spacecraft equipment and materials.

Adhesives and epoxies used for space-borne equipment must withstand the
temperature extremes and vacuum of outer space while maintaining their performance
qualities. They must also not outgas too much as the volatile by-products can degrade
nearby optics and circuitry.

Depending on where a spacecraft is headed, additional environmental factors may affect

its design. In low-Earth orbits, where space stations and most artificial satellites are
deployed, there is highly reactive atomic oxygen (AO). Higher up, in geostationary orbits
where communications and weather satellites operate, particulate radiation (protons,
electrons, and heavy ions) can cause problems. And in interplanetary regions and deep
space where space probes travel, high temperatures and intense radiation are of
particular concern.
Problems with adhesives in space

Adhesives and other polymers are used extensively in all types of spacecraft for
structural, mechanical, and electronics purposes — including bonding, potting,
encapsulating, coating, sealing, and staking. Most adhesives used on spacecraft are not
exposed to atomic oxygen or ionizing radiation because they are inside or sandwiched
and protected between parts they are holding together. But whether directly exposed to
space or not, most adhesives employed in space applications are subject to high vacuum
and extreme cold. They must function properly despite the surrounding conditions
without degrading other spacecraft components.

Optics for space applications can be protected by using low-outgassing adhesives.

Otherwise, contaminants put off by the adhesive can fog and degrade the lenses.
Adhesives on spacecraft are often near electronic or optical devices, where
contamination can lead to serious problems. For example, many adhesives outgas,
potentially releasing volatile products which condense and contaminate electronic,
optical, and other precision instruments. Outgassed compounds can cloud or fog optical
and electro-optical components and interfere with circuit continuity. Even tiny amounts
of condensed organic material can alter the reflectivity or absorbency of optical
components. Precise control over outgassing levels is critical in preventing contaminant
deposits and the resulting loss of performance to mission-critical subsystems.

Requirements for adhesives

Adhesives for space applications must function in high vacuums, extremely low
temperatures, and withstand temperature fluctuations. Their bonds should also last the
length of the mission. Adhesives directly exposed to space for long periods of time
should also strongly resist radiation and microcracking and, if in a low-Earth orbit, also
resist atomic oxygen. That’s because radiation can make some adhesives brittle,
ultimately resulting in cracks. And lengthy exposure to AO can erode adhesives.
Low-outgassing epoxies are used for structural, mechanical, electronic, and adhesive
applications on spacecraft and satellites.

Other application-specific requirements include electrical conductivity, optical clarity,

thermal conductivity or insulation, low ionic content, and cryogenic serviceability.

But all adhesives designated for space applications must meet the outgassing acceptance
criteria defined in NASA specification SP-R-0022A, Vacuum Stability Requirements of
Polymeric Material for Spacecraft Application. This specification stipulates that the total
mass lost from a polymer-based adhesive specimen in a vacuum shall not exceed 1% of
its original mass and that collected volatile condensable materials shall not exceed
0.10% of the original specimen mass. An addendum states that the total mass lost may
exceed 1.0% if it can be shown that mass lost in excess of 1.0% was made up of water
vapor.
Measuring outgassing

Researchers at NASA developed a standard test procedure, ASTM E595: A standard

test method for total mass lost and collected volatile condensable materials from
outgassing in a vacuum environment, to determine the mass lost in a vacuum and
collect the outgassed products. This procedure also measures the volatile content of
adhesives in a heated vacuum chamber.

Specimens are kept at 25°C, 50% humidity, and standard atmospheric pressure for
24 hr prior to the test to ensure all specimens are prepared the same. Samples are
then weighed and placed in individual compartments within a solid copper heater
bar, with separate covers for each compartment. An exit port in each cover provides
the only means for volatile gases to escape, and a collector plate is placed 0.5 in.
from each port. Barriers separate neighboring plates.

The heater bar is placed in a test chamber where the pressure is 5 × 10-5 torr or less.
Both the samples and copper bar are heated to 125°C for 24 hr, driving off volatile
gases through the exit port. With the temperature of the collector plate set to 25°C, a
significant portion of the volatile material condenses on the plate. The total mass
lost (TML) for each specimen is calculated as a percentage by comparing the weight
of the specimen before and after the test. The collected volatile condensable material
(CVCM) for each specimen is calculated as a percentage by comparing the weight of
the clean collector plate to that of the collector plate after the test.
This flowchart shows the test procedures used to classify a material’s
propensity for outgassing.

If CVCM does not exceed 0.10% and TML does not exceed 1.0%, the material passes
the test. If CVCM exceeds 0.10% — regardless of TML — the material fails. However,
if CVCM is less than 0.10%, but TML exceeds 1.0%, a further measurement is made
to see how much water vapor the specimen can reabsorb after reconditioning
exposure, which takes place in a chamber with 50% relative humidity at 25°C for an
additional 24 hr. The water vapor regained (WVR), expressed as a percentage,
represents the mass of water vapor recovered compared to the mass of the original
specimen. If the difference between the TML and WVR does not exceed 1.0% (and
CVCM does not exceed 0.10%), the material passes the test.

To summarize the results of ASTM E595:

 If CVCM ≤ 0.10% and TML ≤ 1.0%, the material passes.
 If CVCM ≤ 0.10% and TML > 1.0%, the material can pass if TML – WVR ≤ 1.0%.
 If CVCM > 0.10%, the material fails.
 If TML – WVR > 1.0%, the material fails.

It’s important to note that test results are only applicable to adhesives with the same
chemistry that have undergone the same curing schedule.

There are other tests for outgassing, many of them proprietary, but they are not
considered credible. ASTM E595 is the only widely accepted industry standard for
quantifying outgassing in epoxies and other adhesives. The 24-hr test does have
limitations. For example, it doesn’t predict long-term outgassing performance or
reveal what will be outgassed under operating conditions. The test does, however,
give engineers a way to evaluate adhesives on the basis of outgassing.

Low-outgassing adhesives and polymers are screened for use in space through a
standard test known as ASTM E595 (see sidebar). Passing this outgassing test is a
necessary — but not always sufficient — criterion for adhesives on spacecraft or
equipment destined for use in space. For example, an adhesive that meets NASA’s
outgassing criteria may not always be appropriate for use near devices operating in
cryogenic temperatures.
Some adhesives, such as two-part epoxies, can be specially formulated to outgas at levels
well below the ASTM E595 standard. There are also some adhesives that were once
unable to pass that test, such as UV-curable adhesives. Recently, however, chemists
have cracked the code of UV curables and concocted several that meet the test.

Adhesives that outgas most severely cure using solvents or moisture. These include
several pressure-sensitive and contact adhesives as well as cyanoacrylates.

It’s worth noting that even within a given family of adhesives, outgassing can vary
substantially. For example, the more-flexible epoxies are more prone to outgassing due
to their lower cross-link density than their more-rigid counterparts. So adhesives should
be evaluated for outgassing individually rather than as families. And the only way to
know for certain whether a specific adhesive meets the low outgassing criteria spelled
out in ASTM E595 is to test it.

Epoxies for space

The dual challenge of achieving sufficiently low-outgassing levels while offering physical
properties that suit a variety of applications can be easily overcome by selecting certain
epoxies. Epoxies are versatile polymer compounds that offer excellent cohesion, resist
chemicals, adhere well to a variety of materials, and operate over temperatures ranging
from cryogenic (4°K) to 550°F. As mentioned earlier, outgassing varies tremendously
across epoxies. Numerous grades of one and two-part epoxies have been specially
formulated to meet or exceed NASA’s outgassing specification. Epoxies that have passed
ASTM E595 can provide a combination of electrical conductivity, cryogenic
serviceability, optical clarity, thermal conductivity or insulation, and resistance to
vibrations, thermal shocks, or impacts.

Epoxies can be engineered to have a variety of mechanical, thermal, optical, electrical,

and physical properties to match an application’s requirements. Adding inorganic fillers,
for example, can alter an epoxy’s strength, viscosity, thermal expansion, heat and
chemical resistance, electrical and thermal conductivity, and shrinkage.

One-part epoxies require no mixing but usually need heat to cure or improve their
performance. Most two-part epoxies cure at ambient temperatures once mixed. Heat
increases a polymer’s cross-link density which, in turn, limits outgassing, so adding a
heat cycle after applying an adhesive can prevent future problems. For instance, after
curing a two-part adhesive at room temperature overnight, an additional three to five
hours or more at 60 to 80°C completes the cure and improves its outgassing properties.

Edited by Stephen J. Mraz, stephen.mraz@penton.com