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resistance in ohm/square was identical over the entire surface
indicating the uniform quality of the applied coating and its
electrical characteristics. In nearly all instances, the SRM
ohm/sq reading was less than 104 ohm/sq.
A four-point-probe test, using Keithley 4200 semi-
conductor characterization system via Keithley interactive test
environment software, was also used to determine the surface
resistivity of each sheet and CNT/composite. Each specimen
was placed in the four-point-probe test fixture that utilizes four
source measurements units (SMU) connected to four
autonomous gold probes extending through a Teflon base lying
parallel to the surface of the sample under test.
Simulating electron-charging phenomena in the space
environment, a preliminary assessment of CNT/(M55J/CE)
/CNT panel (Fig. 1) was also performed by conducting
electron-charging tests under vacuum conditions in the Plasma Fig. 1. Photograph of CNT/(M55J/CE) Panel in vacuum chamber for
Interaction Test facility. During the test, an electron flood beam electron charging tests.
was generated using a Kimball Physics 8104 Electron Gun
capable of operation up to 100 keV. Electron current densities
of ~1 nA/cm2 were utilized as per common design environ-
ments. Similarly, electron energy of 20 keV was used, along
with several lower energy levels of 2.5 keV, 5 keV, and 10
keV. In general, a test environment of 20 keV and 1 nA/cm2
represents most spacecraft design environments.
EMI shielding effectiveness (SE) dB tests were conducted
at the EMC test facility. Different CNT-based composite
panels, and composites with aluminum foil surface layer, were a) 20 to 200-MHz test set up b) 2 to 18-GHz test setup
tested over the frequency range from 20 MHz to 18 GHz Fig. 2. Electromagnetic shielding effectiveness testing of CNT composite
(Fig. 2). panels, Al foil composite panels, and Aluminum plates from 20 MHz to 18
GHz.
D. Mechanical Property Tests
Fig. 4a shows one of the CNT sheets (from NCTI) that
Using NCTI’s CNT sheet as an outer ply, eight CNT/
were examined at multiple locations on the sheet, and later on
(M55J/CE) tubular struts were fabricated, Compression testing
the as-processed CNT/composite laminates. Fig. 4b shows
was performed to determine the ultimate compressive strength
nearly uniform distribution of bundles of CNTs held together
primarily of M55J/CE composite. These tests also provided
by van-der-walls forces. In each case, the presence of residual
insight into the quality of adhesion of outer CNT ply to the
catalyst-type (e.g., iron, nickel or cobalt) impurity was quite
underlying laminates. Four M55J/CE composite sandwich
low. Fig. 4c shows two representative FIB images of the
panels (~50 cm x 50 cm x 1.3 cm) were also fabricated with
surface of the co-cured CNT sheet as an outer ply indicating
co-cured CNT prepreg ply on both of the outer surfaces.
dispersed CNT bundles within CE matrix. Microstructures
Flexure testing of the sandwich panel coupons was performed
indicate that during the SOA composite processing, the CE
to ascertain the quality of CNT/CE ply and underlying
wicks into the CNT sheet forming a very thin layer of resin on
M55J/CE substrate.
CNT bundles. Overall, each of the co-cured CNT sheets was
well adhered to the underlying M55J/CE substrate with no
III. RESULTS AND DISCUSSION significant resin-rich regions.
A. Microstructure
Using scanning electron microscopy, and focused ion beam
(FIB) imaging techniques, each nanocarbon-based sheet
material was examined. Fig. 3 shows the photomicrographs of
the representative regions. For example, MWNT showing
tangled distribution of MWNTs apparently held together by a) MWNT b) CNO c) Graphene Nanoplatelet
van-der-walls forces, CNO particles showing onion-skin like Fig. 3. Photomicrographs of MWNT, CNO, and Graphene Nanoplatelet in
structure, and GnPs well dispersed in the sheet along with the processed sheet materials.
MWNTs.
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thin, co-cured CNT sheet/M55J/CE. Each of the EMI shielding
effectiveness measurements over the 200 MHz to 18 GHz
indicated that the co-cured CNT M55J/CE panel exhibited
shielding effectiveness equivalent to the typical spacecraft
panel with aluminum foil-based M55J/CE composite or solid
aluminum plate. It must be recognized that each test was
performed in the identical test setup and conditions. Results of
a) NCTI’s CNT sheet b) CNT (as-received sheet) all these tests confirm that nanocarbon film-based composite
panels exhibit EMI shielding effectiveness in the acceptable
range for the spacecraft system requirements (including the
nickel nanostrand-based composite panel.
C. CNT Material Design Downselection
After successfully verifying that nearly all CNT-based
composites do satisfy the EMI and ESD requirements for the
spacecraft system, the challenge was to either prioritize or
down select the material and processes that would be
acceptable to spacecraft designers. Key elements of the down
selection criteria were as follows:
c) Co-cured CNT sheet layer i) Composite should be robust and reproducible to provide
acceptable EMI/ ESD performance.
Fig. 4. Photomicrographs of NCTI’s CNT sheet materials: a) as-received
sheet, b) FIB image of a representative region, c) FIB image of co-cured CNT ii) Provide ease of manufacturing (consistent with SOA
sheet revealing presence of CE resin wicked in to the distributed CNT processes), and provide cost savings.
bundles.
iii) Should preferably provide mass savings.
B. EMI/ESD Charcateristics iv) Should offer ≥SOA composite properties.
Table III lists the measured surface resistivity and average v) Cost-effective availability of material form with adequate
bulk electrical resistivity values of the bare M55J/CE material safety data sheets for approval by Employee
composite panel, nanocarbon-based sheets/membranes, and the Safety and Health Organization.
co-cured sheets on the composite panels. In each case, the co-
cured nanocarbon-sheet-based panel, exhibiting surface
resistivity values of <100 ohm/sq, satisfies the ESD require- TABLE III. MEASURED SURFACE RESISTIVITY OF CNT BASED
COMPOSITES
ments for spacecraft exterior surfaces. For example, the CNF-
spray-coated composite panel exhibited surface resistivity of CNT-based
Surface
Electrical
103 to 104, satisfying the ESD requirements. However, the Resistivity
Composite Process Resistivity
4-Point Probe
electron-charging experiments need to be performed to ensure Specimen
Ohm/sq
(Ohm-cm)
there are no resin-rich regions that could lead to charge build As-Processed (no
up and, consequently, ESD damage. The electron charging M55J/CE 108-1011 x
CNT)
tests performed at 20 keV of co-cured, thin CNT sheet/ CNF/(M55J/CE) Spray Coated 3
10 –10 4
x
(M55J/CE) panels indicated no observed surface potential
100%MWNT
values of less than –25 V were measured throughout. A few Sheet
~63-gsm Sheet 1–3 0.02
such panels were examined, and it was found that given the due Co-cured
MWNT/
care in processing, the CNT/composite surfaces did not exhibit (M55J/CE)
CNO/MWNT 20–25 x
any charge build up. Based on the results of several test Sheet
specimens and panels, the presence of thin CNT layer provides 60%CNO/
Sheet 2.5 0.025
40%MWNT
adequate electron mobility, and charges are distributed evenly
Co-cured
around the surface. Of the several nanocarbon-based panels CNO/ M55J/CE
CNO/MWNT
40–80 x
evaluated in the project, the NCTI’s CNT-based panels
CNT (NCTI) Sheet 0.271 8 x 10-4
exhibited consistently low surface resistivity and ease of
handling and processing. Co-cured Dry
CNT/(M55J/CE) 1–7 x
CNT Sheet
Fig. 5a shows the shielding effectiveness (dB) versus CNT Prepreg/ Co-cured CNT
10–30 x
(M55J/CE) Prepreg Outerply
frequency plots of four types of panels: 1) SOA M55J/CE 80%GnP/20%
composite laminate with outer layer of thin aluminum foil, Sheet 1.5–2 0.02
MWNT
2) thin, co-cured CNT sheet/M55J/CE laminate, 3) CNT/ Co-cured GnP
GnP/(M55J/CE) 20–30 x
(M55J/CE) sandwich panel, and 4) panel with a co-cured Sheet
nickel nanostrand-based film (areal density 120 gsm, not
discussed in this paper) on M55J/CE substrate panel. Similarly,
Fig. 5b shows the SE effectiveness testing of a solid plate and a
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D. CNT-based Materials and Processes for Protoflight
Composite Components
Consistent with conventional composite manufacturing
processes, CNT sheet materials specifications and processing
guidelines were established to produce tubes, laminates, and
sandwich panels. For example, tubes were manufactured by
applying the CNT sheet wrapped as an outer ply on the
underlying composite lay-up, and manufactured by conven-
tional autoclave process, thus yielding a well-consolidated
CNT-based composite tube. However, to manufacture
composite sandwich panels, it was best to use CNT/CE prepreg
as the outer ply on both sides of the sandwich panel and to co-
cure the assembly in the oven.
Using these materials and processing guidelines, a few
CNT/ (M55J/CE) composite tubes and sandwich panels were
a) Four test panels: 1) Ni nanostrand/composite laminate, 2) CNT/composite fabricated. The ESD performance of each composite part was
honey comb panel, 3) Al foil/composite laminate, and 4) CNT/composite verified to be consistent with the spacecraft structures require-
laminate.
ments. For example, the surface resistivity values were
consistently ~1 to 10 ohm/sq. Compression testing of the
CNT/composite tubes (Fig. 6a) was conducted to ensure that
the average stiffness and strength values were equal to or better
than the baseline M55J/CE composite. The CNT/(M55J/CE)
sandwich panels were tested using the four-point bend/flexure
tests (Fig. 6b). Results of flexure tests indicated that the
average facing bending strength of CNT-based panels was
equivalent or better than M55J/CE panel without co-cured
CNT sheet.
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CNT REM
Strut
a) CNT Sheet outer ply on inner and outer surfaces of composite sandwich
Fig. 7. Layup of REM support strut with CNT outer layer on M55J/CE panel.
composite.
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was also procured, and CNT/(M55J/CE) composite panels
were fabricated. Each of these nanocarbon sheet material-based REFERENCES
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Ravine of Nanocomp Technology Inc. and Nanotechnology
Laboratory, respectively, for several technical discussions
regarding processing of thin sheets of CNTs, MWNT, CNO,
and GnPs.
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