National Aeronautics and

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IS20

George C. Marshall Space Flight Center

Marshall Space Flight Center, Alabama

35812
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i

NASA/TM—2009–215901

NASA Materials Research for Extreme 

Conditions

R.J. Sharpe

The University of Alabama, Tuscaloosa, Alabama

M.D. Wright

Marshall Space Flight Center, Marshall Space Flight Center, Alabama

July 2009

National Aeronautics and

Space Administration

Marshall Space Flight Center • MSFC, Alabama 35812
ii

Available from:

NASA Center for AeroSpace Information

7115 Standard Drive

Hanover, MD 21076 –1320

443–757–5802

This report is also available in electronic form at

<https://www2.sti.nasa.gov>

Acknowledgments

Special thanks to Donald Frazier (ED10) for reviewing this Technical Memorandum for scientific accuracy.
iii

TABLE OF CONTENTS

1. INTRODUCTION ............................................................................................................. 1

2. MATERIALS RESEARCH IN THE 1960S ....................................................................... 2

2.1 Silazane Polymers ......................................................................................................... 2

3. MATERIALS RESEARCH DURING THE 1970S ........................................................... 4

3.1 Solvent-Resistant Elastomers for Extreme Environments ............................................. 4

3.2 Siloxane Derivatives ...................................................................................................... 5

4. MATERIALS RESEARCH IN THE 1980S ....................................................................... 7

4.1 Space Shuttle Thermal Protection System ..................................................................... 7

5. MATERIALS RESEARCH IN THE 1990S ....................................................................... 9

5.1 Phenolic-Impregnated Carbon Ablator ......................................................................... 9

6. MATERIALS RESEARCH IN THE PRESENT ............................................................... 12

6.1 Carbon Nanotubes ....................................................................................................... 12

7. CONCLUSION .................................................................................................................. 13

REFERENCES .................................................................................................................................... 15
iv
v

LIST OF FIGURES

1. Structures of the three forms of products of reaction between ethylene 

diamine and dichlorosilane: (a) Linear structure, (b) ladder structure, 

and (c) cyclic structure ................................................................................................. 3

2. Structures of (a) polyurethane and (b) polyisocyanurate ............................................. 4

3. Space Shuttle external tank .......................................................................................... 5

4. A general siloxane compound ...................................................................................... 6

5. Diagram of the HRSI Space Shuttle tile ...................................................................... 7

6. Diagram of the two reaction routes of the phenolic resin polycondensation 

reaction ........................................................................................................................ 10

7. Structures of (a) phenol and (b) formaldehyde ............................................................ 10

8. Structure of phenolic resin product ............................................................................. 11
vi
vii

LIST OF ACRONYMS, ABBREVIATIONS, AND SYMBOLS

ARC Ames Research Center

C2H4(NH2)2 ethylene diamine

CNT carbon nanotube

CVD chemical vapor deposition

HRSI high-temperature, reusable surface insulation

ISS International Space Station

LCA lightweight ceramic ablators

MeSiCl2 dichlorosilane

MSFC Marshall Space Flight Center

MWNT multiwalled nanotube

N-H amino functional group

PICA phenolic-impregnated carbon ablator

Pol polymer chain

R1 methyl radical

R2 phenyl radical

RCC reinforced carbon-carbon

Si silicon

SILC Shuttle ice liberation system

SWNT single-walled nanotube

TPS thermal protection system

X hydrogen, halogen, alkyl or aryl radical
viii
1

TECHNICAL MEMORANDUM

NASA MATERIALS RESEARCH FOR EXTREME CONDITIONS 

1. INTRODUCTION

Since its birth, NASA has faced the challenge of developing materials suitable for the harsh 

environment that space travel presents. These environments run the gamut from various atmospheric pressures to extremes of hot and cold to reentry into Earth’s atmosphere. With each mission NASA has undertaken (Mercury, Gemini, etc.), scientists have confronted new and unfamiliar 

materials development issues. However, out of these challenges have risen some of the most important innovations in science and technology of the modern age. 

Chemistry and materials science have played a major role in these innovations. For example, 

experimentation in stable and efficient organic polymers yielded results in developing materials 

resistant to extreme temperatures and pressures. In addition, carbon fiber/phenolic composites, 

developed in the late 1990s, have proven useful in structural aspects of mission programs. Such vital 

research supports and ensures the continued success of the American Space Agency.

The NASA technical reports server provides an extensive archive of such advancements 

in materials development. This Technical Memorandum outlines a brief survey of significant 

materials developments over NASA’s history, explains the basic development of these materials, 

and discusses their use and importance.
2

2. MATERIALS RESEARCH IN THE 1960S

The Space Race pitted the USSR and the United States against each other in launch vehicle 

development. NASA scientists faced the problem of producing a vehicle powerful enough to leave 

Earth’s orbit (the Saturn V rocket) while also developing the Apollo capsule that would carry 

Americans to the Moon. The materials with which the launch vehicle and spacecraft would be built 

needed to meet specific qualifications of resistance to temperature, pressure, and durability. 

2.1 Silazane Polymers

During the mid-1960s, James Byrd and James Curry, materials scientists at Marshall Space 

Flight Center (MSFC), Huntsville, AL, proposed the use of silazane polymers in their research 

for the applications of heat-sensitive portions of spacecraft.1 Byrd pointed out in his paper “Studies in Silazane Chemistry” that silicones and their traditional compounds, while particularly useful 

at room temperature, broke down at temperatures in excess of 482 oF (250 oC). However, when 

silicone (Si) bonds with amino functional groups (N-H), the physical properties of these materials 

become much more durable. The product is known as a silazane, and when this material undergoes 

polymerization, its characteristics make it a viable candidate for materials needed for successful 

space flight. 

Byrd and Curry noted that in the chemical reaction between ethylene diamine 

(C2H4(NH2)2) and dichlorosilane (MeSiCl2), there were three possible polymeric structures—the 

linear form, the ladder form, and the five-membered, cyclic form. Their structures are given in 

figure 1.

Further research showed that this concept of forming polymers with the silicone-nitrogen 

(N) bond linkage would be useful in developing materials resistant to high temperatures. In addition, due to its high elasticity, silazane polymers were found to have applications as seals and 

gaskets under high temperature. Today, silazane polymers are used as a tool for patching reinforced 

carbon-carbon (RCC) surfaces on the Space Shuttle before returning to Earth.2 The polymer 

is mixed with a silicon carbide and various other metal carbides to form a paste that can resist 

temperatures up to 3,500 oF (1,927 oC).

This innovation, amongst others, illustrated the incorporation of research in organic chemistry into the Space Agency during the 1960s; Curry and Byrd’s work served as a springboard in the 

development of new, stronger materials for use in the Space program.
3

Pol

Pol

(a) Linear Structure (b) Ladder Structure (c) Cyclic Structure

Pol

Pol

Pol

Pol Pol Pol

Si

Si

Si

Si Si

N

N

N N

N

N

n n n

CH3

CH3

CH3

CH3

CH3

H3C

H3C

H3C

H

H

CH3

CH2

CH2

CH3

Figure 1. Structures of the three forms of products of reaction between ethylene 

diamine and dichlorosilane: (a) Linear structure, (b) ladder structure, 

and (c) cyclic structure.
4

3. MATERIALS RESEARCH DURING THE 1970S

The closing of the Apollo program brought about new challenges as NASA scientists 

sought to establish a temporary home in space (Skylab) as well as develop a reusable space transportation vehicle (Shuttle). These new challenges led to more innovation in the fields of engineering 

and chemistry. Two major scientific problems and their solutions are briefly outlined in sections 3.1 

and 3.2.

3.1 Solvent-Resistant Elastomers for Extreme Environments

A need for materials in fuel tank development encouraged research in elastomeric polymer 

chemistry in the early 1970s, and in particular, the chemistry of polyurethane and polyisocyanurate. 

Both of these compounds exhibited strong elasticity and showed a resistance to extreme temperatures.3 Their structures are provided in figure 2.

Pol

Pol

Pol Pol

Pol

N

N N

N

n

n n

n

H

N

H

R

R R

R

O O

O

(a) Polyurethane (b) Polyisocyanurate

'' ''

O

O

O

O

R

''

''

''

Figure 2. Structures of (a) polyurethane and (b) polyisocyanurate.

Research on these types of polymers was needed for development of a foam insulator 

for the proposed Space Shuttle external tank. MSFC materials scientist W.E. Hill discussed in his 

paper that polyurethane, having a density of 48.06 kg/m3 and being a material of choice in the 

coating of the Saturn rocket, was found to be too heavy a material to be acceptable as the insulating foam for the needs of the Shuttle program. Furthermore, he noted that three-dimensional 

foam polyurethane underwent a decomposition reaction at 302 oF (150 oC). This eliminated threedimensional foam from serious consideration in the discussion of what could be used to insulate 

the Shuttle fuel tank, as shown in figure 3.

Polyisocyanurate, however, showed much more promising qualities. Its density of 28.80 kg/

m3 (almost half of the three-dimensional foam) made it a significantly more efficient material for 

keeping within the weight limits of the external tank. Polyisocyanurate was also found to perform 

consistently over various temperature range tests. 
5

Figure 3. Space Shuttle external tank.

These properties, along with its elasticity, made polyisocyanurate an excellent candidate 

for sealant of fuel tanks. Today, this research bears significance in that polyisocyanurates have 

become the material of choice for the foam coating of the Space Shuttle’s external tank.4 The polyisocyanurate regulates the temperature of the propellants in the external tank, effectively clings to 

its surface, and minimizes ice formation.

The need for elastomeric materials for Space Shuttle applications became extremely important when the Challenger disaster took place in 1986. The tragedy, which was caused by the failure 

of an O-ring under unusually low temperature, called for even more innovation in elastomeric 

polymer chemistry.

3.2 Siloxane Derivatives

Another major problem that NASA scientists faced was the development of effective lubricant systems for spacecraft and launch vehicles. Several lubricants had been used, but none had yet 

proven to be properly resistant to extensive amounts of radiation from outerspace. MSFC materials scientist Norman Billow developed a organosilicon-based compound with a resistance to 

radiation.5 His discovery is outlined below.

Thiophenyl ether siloxanes exhibit several physical properties useful in applications of 

spacecraft lubricant. The structure of a general thiophenyl siloxane is given in figure 4.

The key feature in the synthesis of the disiloxane compound is a Grignard reaction between 

the Grignard reagent of a bromo-substituted phenylthiobenzene with a dichlorosilane and then 

hydrolysis with water. Synthesis of the trisiloxane takes place through a similar Grignard reaction.
6

R1 R2 X

n1

n2

n3

O

X

Si Si

S

S

CH3 CH3

Figure 4. A general siloxane compound (no specific regiochemistry is shown).

Once the compound was synthesized, Billow began to measure its properties; he then 

discovered that the siloxanes had very low pouring points (the lowest temperature at which 

a compound will pour or flow) and a strong lubricity. In addition, these siloxanes were resistant 

to extreme temperature as well as radiation. In practice today, siloxanes are used to prevent ice 

buildup on the U.S. Space Shuttle.6 The siloxanes are mixed with ethyl alcohol, ethyl sulfate, isopropanol, and polytetraflouroethylene to form a coating known as the Shuttle ice liberation 

system (SILC). 

This invention was a significant step in materials development in that the problem of radiation had been addressed in the area of lubrication development. Organic/polymer chemistry was at 

the core of a great deal of research that took place during the early decades of the Space Agency.
7

4. MATERIALS RESEARCH IN THE 1980S

The advent of a spacecraft that could go into space, return, and be used again brought 

about an enormous need for new technology in the Space Agency. New systems needed to be developed for launch and reentry, and a new system for propulsion had to be devised. The Shuttle age 

drew from the knowledge and strategies used in the Apollo program to shift into a higher standard 

of materials research. One focus of this research, the thermal protection system (TPS) developed 

by scientists Ian MacConochie, Ashby Lawson, and H. Neale Kelly, is outlined in section 4.1.

4.1 Space Shuttle Thermal Protection System

A reusable launch vehicle called for moving beyond the heat ablation system employed by 

the Mercury, Gemini, and Apollo programs—designed only to reenter the atmosphere once. Any 

new material used for regulating temperatures during reentry would have to be lightweight and 

sturdy while also providing the shielding necessary for the protection of the metal Space Shuttle. 

Most important was its need to be reusable.

NASA scientists worked to develop a new type of heat-shielding material based on a tile 

structure rather than the ablation covering that former missions used.7 The tile would be primarily 

composed of a layered design with an outer coating that adheres to the surface of the Space Shuttle. A diagram of the tile is provided in figure 5.

Coated Tile

Step

Uncoated

Filler Bar

Coating

Terminator

Sip

Adhesive

Gap Variable

Figure 5. Diagram of the HRSI Space Shuttle tile.8
8

The main interior of the tile is a pure silica that is fired at 2,300 oF (1,260 oC), and is covered in a borosilicate compound for purposes of waterproofing. The sip layer as well as the filler is 

comprised of a heat-resistant felt while the adhesive is made from silicone. This high-temperature, 

reusable surface insulation (HRSI) tile served as the primary material for the underbelly of the 

Space Shuttle. 

However, the nosecone and wing edges of the Space Shuttle called for stronger materials 

that would need to resist even higher temperatures as they would experience the most heat during 

reentry. NASA then introduced the RCC. RCC is made in a process that requires laying out the 

starting material (a carbon fiber) and then infusing it with carbon-forming gas such as acetylene. 

In today’s applications, similar materials are also used in the manufacturing of automotive brake 

systems. 

The TPS for the Space Shuttle brought about a revolutionary concept of reusable materials development that shifted the way NASA viewed the problem of outerspace temperatures. This 

innovation, along with many others in the age, made the case for the Shuttle as one of the most 

advanced machines ever built.
9

5. MATERIALS RESEARCH IN THE 1990S

The 1990s continued the return to flight after the Challenger incident and set in motion the 

transition of developing a home in space. NASA scientists began to work with other space agencies in order to plan and execute the building of the International Space Station (ISS). Materials 

innovation became increasingly vital as numerous agencies from across the globe began to assemble 

separate sections of a space station that would not be assembled until they met in Earth orbit.

5.1 Phenolic-Impregnated Carbon Ablator

Returning to the concept of ablative materials from the Apollo program for heat shielding, 

scientists at NASA Ames Research Center (ARC) began to develop a family of materials known as 

lightweight ceramic ablators (LCAs).9 These materials, known for their durability and low density, 

served as a springboard into research for future planetary missions.

LCAs consist of a low-density fiber infused with an organic resin. Specifically, phenolicimpregnated carbon ablators (PICAs) use FiberForm as the fiber substrate, a material developed 

by Fibermaterials Inc., that consists of a rigid, lightweight carbon fiber designed to be resistant 

to high temperatures in vacuum. The FiberForm is then infused with a phenolic resin. The resin 

is a product of a polycondensation reaction between phenol and formaldehyde in the presence 

of a catalyst. The reaction can occur via two routes, which are diagrammed in figure 6. Phenol 

and formaldahyde structures are given in figure 7.

The route by which the resin is made depends on the ratio of formaldehyde to phenol used in 

the reaction. If the formaldeyde/phenol ratio is >1, then the process would go through route A, in which 

the two compounds are mixed, heated, and begin to crosslink with each other in the presence of a base 

catalyst. If the opposite is true, then the reaction would go through route B, in which an acid catalyzes 

the reaction, and then a crosslinking agent must be introduced. The final structure of the cured resin 

is shown in figure 8.

By the end of this research, the result was an extremely durable material that could withstand 

both extreme temperature and a vacuum environment. In practice, PICA was used as the primary heat 

shield material for the Stardust spacecraft, whose mission was to collect samples from Comet Wild 2 

in February 1999. Due to the fact that Stardust reentered the atmosphere even faster than the Apollo 

capsule, PICA was a key factor in the mission’s success. In addition, NASA scientists are currently 

experimenting with PICA in their development of the Orion capsule’s heat shield for the Constellation 

program.

It is worth noting, however, that the supply of a key material used to make these composites, 

rayon, has come under jeopardy due to the prohibition of the method used to make it. This was done due 

to the harsh byproducts that are released in rayon’s synthesis. As a result, research is currently underway 

to develop an alternative material to replace the rayon cloth.
10

Phenol and Formaldehyde

Ratio P/F <1 Ratio P/F >1

A-Stage Resin

and

B-Stage Resin

B-Stage Resin

(Novolac)

(a) (b)

Ground and Mixed With

Various Filters and Pigments.

Hexamethylenetetramine

(CH2)

6N4 is added.

Molding Powder

Cured Resin (C Stage)

Oil-soluble

Liquid Resins

for Coatings

Liquid Resins

for Lamination

and Bonding

Casting

Curing Curing Curing Curing

Alkaline Catalyst Acid Catalyst

Figure 6. Diagram of the two reaction routes of the phenolic resin polycondensation reaction.

O

OH

H H

(a) Phenol (b) Formaldehyde

Figure 7. Structures of (a) phenol and (b) formaldehyde.
11

OH

OH OH

OH

H2

C

H2

C

H2

CH2 CH2

CH3 CH3

Pol O C O Pol

H2

C

H2

C

H2

Pol O C O Pol

n

Figure 8. Structure of phenolic resin product.
12

6. MATERIALS RESEARCH IN THE PRESENT

The 21st century has brought about even more challenges for the Space Agency as production on the ISS continued and as NASA began to answer then President George W. Bush’s challenge to return humans to the Moon and Mars. A human mission to Mars requires technology 

more advanced than has ever been developed before in the history of the Space Agency.

6.1 Carbon Nanotubes

Discovered in 1991 by Japanese scientist Sumio Iijima, carbon nanotubes (CNTs) have been 

a topic of great interest due to their remarkable strength and durability.10 CNTs are another configuration 

of carbon molecules in which a cylindrical shape is formed. CNTs have since been discovered to exist 

in the two following types: (1) The single-walled nanotube (SWNT), in which only one layer of atoms 

is rolled together and (2) the multiwalled nanotube (MWNT), in which multiple layers of atoms are 

rolled together with a constant spacing of 3.4 Å. CNTs have also been found to have practical applications both in the electrical/circuitry fields as semiconductors and in the structural fields for armor and 

spacesuits.

Regarding their formation, CNTs can be synthesized via several different means, one of which 

involves bombardment with an argon laser in the presence of a transition metal catalyst. Another method 

that has drawn recent interest is the process of chemical vapor deposition (CVD) of nanotubes. In a 

process similar to the argon laser method, a growth apparatus featuring a quartz tube with a transition 

metal catalyst is placed inside a furnace. The furnace is heated to temperatures of about 1,292–1,652 oF 

(700–900 oC) at atmospheric pressure while hydrocarbons are fed into the tube (usually ethylene 

for MWNTs and methane for SWNTs). This process produces in good yield, and scientists at ARC have 

speculated the possibility of using this method to synthesize CNTs much more selectively.

CNTs have been used by the Space Agency in the application of chemical sensors. Research is 

currently underway in the structural application of nanotubes with the potential of developing a composite with applications in a large range of structural materials. Their remarkable strength-to-weight 

ratio (several hundred times that of steel) make them attractive in numerous areas of materials science 

research.
13

7. CONCLUSION

These materials developments, amongst many others, have worked to effectively shape both 

the present and future of American space exploration efforts. Each advancement cited has served 

in some way to motivate the next, and to this day, NASA continues to rely on its past research 

in order to ensure its bright future. As the Agency brings the Shuttle program to a close and the 

Constellation program into focus, more advancements will be required. But with a history in which 

the successes far outnumber the failures, the Agency continues to move forward in its conquest of 

outerspace.
14
15

REFERENCES

 1. Byrd, J.D.; and Curry, J.E.: “Studies in Silazane Chemistry,” NASA-TM-X-53197, Marshall 

Space Flight Center, AL, February 1965.

 2. “Ceramic Paste for Patching High-Temperature Insulation,” NASA Tech Brief, Johnson Space 

Center, Houston, TX, February 1, 2007.

 3. “Materials for Foam Type Insulation,” Cryog. Res. at MSFC: Res. Achievements Rev., Vol. 4, 

No. 2, pp. 179–184, November 1, 1971.

 4. “Development of Polyisocyanurate Pour Foam Formulation for Space Shuttle External Tank 

Thermal Protection System,” Final Technical Report From University of Dayton Research 

Institute, Dayton, OH. Prepared by J.A. Harvey, Ph.D.; J.M. Butler, Ph.D.; and R.P. Chartoff, 

Ph.D., August 1988.

 5. “Thiophenyl Ether Disiloxanes and Trisiloxanes Useful as Lubricant Fluids,” U.S. Patent 

No. 3801617, Patented April 2, 1974.

 6. “Coating Reduces Ice Adhesion,” NASA Tech Brief, Kennedy Space Center, Orlando, FL, 

October 1, 2008.

 7. “Shell Tile Thermal Protection,” U.S. Patent 4456208, Patented June 26, 1984.

 8. Curry, D.M.: “Space Shuttle Orbiter Thermal Protection System Design and Flight Experience,” Structures and Mechanics Division, Johnson Space Center, Houston, TX, February 

1993.

 9. Tran, H.K.; Johnson, C.E.; Rasky, D.J.; et al.: “Phenolic Impregnated Carbon Ablators as 

Thermal Protection Systems for Discovery Missions,” NASA-TM-110440, Ames Research 

Center, Moffett Field, CA, April 1997.

10. Cassell, A.; Delzit, L.; Nguyen, C.; et al.: “Carbon Nanotubes by CVD and Applications,” 

Thirteenth European Conference on Chemical Vapor Deposition, J. Phys. IV, Vol. 11, 

pp. Pr3-401–Pr3-409, DOI: 10.1051/jp4:2001351, France, 2001.
16

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NASA Materials Research for Extreme Conditions

R.J. Sharpe* and M.D. Wright

George C. Marshall Space Flight Center

Marshall Space Flight Center, AL 35812

National Aeronautics and Space Administration

Washington, DC 20546–0001

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SEC 51

Technical Memorandum

NASA/TM—2009–215901

materials, silazane, polyurethane, polyisocyanurate, siloxane, thermal protection system, phenolicimpregnated carbon ablator, carbon nanotube

01–07–2009

UU 24

NASA

U U U

This Technical Memorandum briefly covers various innovations in materials science and development throughout the course of the American Space program. It details each innovation’s discovery and development, explains 

its significance, and describes the applications of this material either in the time period discovered or today. 

Topics of research include silazane polymers, solvent-resistant elastomeric polymers (polyurethanes and polyisocyanurates), siloxanes, the Space Shuttle thermal protection system, phenolic-impregnated carbon ablator, 

and carbon nanotubes. Significance of these developments includes the Space Shuttle, Apollo programs, and 

the Constellation program.

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custom thesauri, building customized databases, 

and organizing and publishing research results.

For more information about the NASA STI 

program, see the following:

• Access the NASA STI program home page at 

<http://www.sti.nasa.gov>

• E-mail your question via the Internet to 

<help@sti.nasa.gov>

• Fax your question to the NASA STI Help Desk 

at 443 –757–5803

• Phone the NASA STI Help Desk at 

443–757–5802

• Write to:

NASA STI Help Desk

NASA Center for AeroSpace Information

7115 Standard Drive

Hanover, MD 21076–1320
National Aeronautics and

Space Administration

IS20

George C. Marshall Space Flight Center

Marshall Space Flight Center, Alabama

35812