1. Baochau N. Nguyen, Haiquan N. Guo, and Linda S. McCorkle
Ohio Aerospace Institute, Brook Park, Ohio
Synthesis, Processing, and Characterization
of Inorganic-Organic Hybrid Cross-Linked
Silica, Organic Polyimide, and Inorganic
Aluminosilicate Aerogels
NASA/CR—2014-218328
July 2014
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3. Baochau N. Nguyen, Haiquan N. Guo, and Linda S. McCorkle
Ohio Aerospace Institute, Brook Park, Ohio
Synthesis, Processing, and Characterization
of Inorganic-Organic Hybrid Cross-Linked
Silica, Organic Polyimide, and Inorganic
Aluminosilicate Aerogels
NASA/CR—2014-218328
July 2014
National Aeronautics and
Space Administration
Glenn Research Center
Cleveland, Ohio 44135
Prepared under Contract NNC07BA13B, Task order NNC07TA79T
4. Acknowledgments
The researchers would like to acknowledge the following people who contributed their efforts and help in the completion and
success of the projects: Dr. Mary Ann B. Meador and Dr. Fran Hurwitz (NASA Glenn) for their leads in the projects, Dr. Felix A.
Miranda (NASAGlenn) for his lead in the Low DielectricAerogel and Patch Light WeightAntenna projects; Dr. Fred W. Vankuels
(Vantage Partners) and Dr. Carl H. Mueller (Qinetiq North America) for their contribution and support in the Low Dielectric
Aerogel and Patch Light Weight Antenna projects. Dan A. Scheiman (OAI) for performing all the Fourier Transform Infrared
Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), Thermal GravimetricAnalysis (TGA), TGA-FTIR, Pycnometry,
and Gel Permeation Chromatography (GPC). Dan Haas (NASA Glenn) for operating the supercritical fluid extraction, Dr. Bart
Hamilton, Dr. Jiao Guo, and Saurabh Batra from Professor Mukerrem Cakmak’s research group at the University of Akron for
the use of the film casting machine and help with the production of polyimide aerogel films. Derek Quade (NASA Glenn), Dr.
Bart Hamilton, and Dr. Jiao Guo (University of Akron) for performing the compression and tensile tests on aerogel films. Anna
Palczer (deceased) for running the BET surface area of aerogels and her training of the BET instrument. All interns from the
LERCIP, MUST, INSPIRE, and USRP programs for their help in the projects. They are Marissa E. Tousley, Jenna Proudfoot,
Alexandra Medoro, Victoria Arendt, Marcus Rhohovie, Sara Ercegovic, Anna Sandberg, Guilherme (William) Sprowl, Sheeba
Bali, and Brittany Wilkewitz.
Available from
NASA Center for Aerospace Information
7115 Standard Drive
Hanover, MD 21076–1320
National Technical Information Service
5301 Shawnee Road
Alexandria, VA 22312
Available electronically at http://www.sti.nasa.gov
Trade names and trademarks are used in this report for identification
only. Their usage does not constitute an official endorsement,
either expressed or implied, by the National Aeronautics and
Space Administration.
Level of Review: This material has been technically reviewed by NASA technical management OR expert reviewer(s).
5. NASA/CR—2014-218328 1
Synthesis, Processing, and Characterization of Inorganic-Organic
Hybrid Cross-Linked Silica, Organic Polyimide, and Inorganic
Aluminosilicate Aerogels
Baochau N. Nguyen, Haiquan N. Guo, and Linda S. McCorkle
Ohio Aerospace Institute
Brook Park, Ohio 44142
10. BAPP BTDA
APTES
TMOS
APTES end capped polyamic acid
Polyamic acid cross-linked silica gel
Polyimide cross-linked silica gel
NH3
.H2
O in NMP
Pyridine and Acetic
anhydride
NASA/CR—2014-218328 6
17. Si
OCH3
OCH3
Si
NH
CH3O
CH3O
OCH3
OCH3
Si
CH3O
CH3O
OCH3
+
N
N
N
O
O
O
HN
O
HN
O
O
HN
NN
N
O
O
O
HN
O
HN
O
HN
O
N
N
N
O O
O
HN
O
NH
O
NH
O
NH
O N
N
N
O
O
O
NH
O
NH
OSi
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
Si
Si
N
O
O
Si
O
O
N
N
N
N
NH
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
O
N
N
N
N
HN
N
NN
HN
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
Si
Si
NH
O
O
Si
O
O
NH
HN
NH
NH
NH
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
Si
O
O
Si
O
OSi
O
O
SiO
Si
O
OSi
O
Si O
SiO
Si
O
O
Si
O
O
Si O
O
Si
O
O
O
O
O
O
O
O
NH
NH
NH
NH
HN
NH
NHNH
HN
N
C
O
N
C
O
NN
N
O
O O
N
C
O
MTMS
BTMSPA
Desmodur N3300
Native aerogel
Reinforced aerogel
NASA/CR—2014-218328 13
18. Si NH + O C N R
N C O
N C O Si N C
O
NH R
N
N
C
C
O
O
Absorbed H2O
Si N C
O
NH R
NH2
NH2
+ 2 CO2
Chain
extension
Si N C
O
NH R NH C
O
NH
R N C O
n
Cross-linking
Si N C
O
NH R NH C
O
NH
R NH C
N
O
Si
n
O C N R
N C O
N C O
NASA/CR—2014-218328 14
