International Journal of Minerals, Metallurgy and Materials

Volume 30, Number 3, March 2023, Page 570

https://doi.org/10.1007/s12613-022-2476-6

Ultralight pyrolytic carbon foam reinforced with amorphous carbon

nanotubes for broadband electromagnetic absorption

Luo Kong ✉, Sihan Luo, Shuyu Zhang, Guiqin Zhang, and Yi Liang
School of Materials Science and Engineering, Shaanxi Key Laboratory of Green Preparation and Functionalization for Inorganic Materials, Shaanxi University of
Science and Technology, Xi’an 710021, China
(Received: 17 January 2022; revised: 2 March 2022; accepted: 16 March 2022)

Abstract: For electromagnetic wave-absorbing materials, maximizing absorption at a specific frequency has been constantly achieved, but en-
hancing the absorption properties in the entire band remains a challenge. In this work, a 3D porous pyrolytic carbon (PyC) foam matrix was
synthesized by a template method. Amorphous carbon nanotubes (CNTs) were then in-situ grown on the matrix surface to obtain ultralight
CNTs/PyC foam. These in-situ grown amorphous CNTs were distributed uniformly and controlled by the catalytic growth time and can en-
hance the interface polarization and conduction loss of composites. When the electromagnetic wave enters the internal holes, the electromag-
netic energy can be completely attenuated under the combined action of polarization, conductivity loss, and multiple reflections. The ultralight
CNTs/PyC foam had a density of 22.0 mg·cm−3 and a reflection coefficient lower than −13.3 dB in the whole X-band (8.2–12.4 GHz), which is
better than the conventional standard of effective absorption bandwidth (≤−10 dB). The results provide ideas for researching ultralight and
strong electromagnetic wave absorbing materials in the X-band.
Keywords: ultralight; carbon foam; amorphous carbon nanotubes; broadband electromagnetic absorption

1. Introduction low density, strong conductivity loss, and stability. However,

Issues related to the high-frequency X-band electromag-
netic wave with the wavelength of 2.4 × 10−2–3.7 × 10−2 m
have become increasingly serious, such as severe pollution to
the surrounding environment and even threats to human
health and information security. Electromagnetic wave-ab-
sorbing (EA) materials could attenuate electromagnetic en-
ergy to reduce electromagnetic pollution [1–4]. An ideal EA
material should have the characteristics of thin thickness,
light density, strong absorption capacity, and wide absorp-
tion band; among them, ultralight and broadband EA materi-
al is the focus of current research [5]. Although EA materials
are continuously pursued to achieve maximum absorption at
a certain frequency, the challenge of reaching high absorp-
tion in the whole frequency band remains. In addition, EA
materials must be ultralight. A possible solution to this prob-
lem is suitable composition selection and structural design.
Although magnetic loss materials, such as CoNi [6], FeNi
[7], and Fe3O4 [8], have excellent EA performance, they have
a large density, and their application is limited by the Curie
temperature [9]. The characteristics of dielectric loss materi-
als depend on their microstructure, chemical, and phase com-
position [10–12]. Carbon materials, mainly including
graphene [13], carbon nanotubes (CNTs) [14], and carbon
fiber [15], have suitable compositions that meet the require-
ments of ultralight and broadband absorption because of their
the application of single-component carbon is hindered by its
too high or weak dielectric loss, which is mainly reflected in
the difficulty of regulating the dielectric constant to the op-
timal matching value. Therefore, single-component carbon
must be combined with other carbon materials to improve its
EA properties. In addition, the permittivity and dielectric loss
could be regulated by adjusting the structure.
How to synthesize an ultralight EA material that can
achieve high absorption in the whole frequency band is a ur-
gent problem. In our previous work, we obtained CNTs/re-
duced graphene oxide (RGO) hybrids by in-situ growing
amorphous CNTs on RGO sheets and then mixing them with
polydimethylsiloxane (PDMS). The generated composite
shows excellent absorption performance. When the content
of CNTs/RGO hybrids is 5wt%, the minimum reflection
coefficient (RC) reaches −55 dB, and the electromagnetic
wave-absorbing broadband (EAB) is 3.5 GHz [16].
However, CNTs/RGO hybrids cannot meet the requirements
of ultralow density because they are added into PDMS as ab-
sorbents to form a macro block EA material. On this basis,
we carried out further research on reducing the density. Ac-
cording to the Maxwell Garnett theory [17–19], a porous
structure can reduce the density, adjust the dielectric loss, and
improve impedance matching. Using the previously de-
scribed CNTs/RGO hybrids as the structural unit, we as-
sembled a self-supporting 3D CNTs/RGO foam with the

✉ Corresponding author: Luo Kong E-mail: kongluo@sina.com

© University of Science and Technology Beijing 2023
L. Kong et al., Ultralight pyrolytic carbon foam reinforced with amorphous carbon nanotubes for broadband ...
density reduced to 33 mg·cm−3 by freeze-drying. However,
its aperture is too small, and the large volume fraction of the
absorbent leads to a large dielectric constant and conductiv-
ity. Therefore, the foam can only be used as an ultralight
electromagnetic interference shielding material. When the
thickness of the CNTs/RGO foam is 2 mm, its average elec-
tromagnetic shielding effectiveness in X-band reaches 36 dB
[20]. Therefore, reducing the volume fraction of absorbent
and the conductivity have become a new research goal. A
method of loading carbon material into nickel foam as a tem-
plate and then etching it to produce porous carbon foam has
been recently developed [21] and shows the advantage of ob-
taining porous carbon material with controllable microstruc-
ture and low density. Inspired by it, we used high-porosity
nickel foam as a template to prepare graphene (G) foam by
chemical vapor deposition (CVD) and grow amorphous
CNTs on the surface to obtain CNTs/G foam. The volume
fraction of the CNTs in the G foam was reduced, and the
density of CNTs/G foam was only 97.1 mg·cm−3. However,
the G foam matrix still cannot meet the requirements of wave
absorption due to its ultrahigh conductivity and continuous
3D network structure that may cause impedance mismatch-
ing [22]. On the basis of the above analysis, further reduction
in the conductivity of the matrix in composites is the key to
obtaining ultralight EA materials.
In this work, pyrolytic carbon (PyC) foam with low con-
ductivity was employed as the matrix and further modified
using low crystalline CNTs. PyC foam was prepared from Ni
foam as sacrificial templates. Polydopamine (PDA) was used
as the precursor of PyC and the carrier of catalyst to achieve
the controllable distribution of in-situ grown CNTs on the
matrix. The CNTs/PyC foam is a self-supporting 3D struc-
ture with submillimeter-sized holes that allow multiple re-
flections and repeated loss of incident electromagnetic wave
[23–28]. The in-situ grown CNTs can significantly enhance
the conductivity loss of the composite. A systematic study
was conducted on the influence of the morphology and com-
position of CNTs/PyC foam on the dielectric loss and EA
property. Finally, an ultralight material with strong electro-
magnetic absorption across the entire X-band was synthes-
ized using the design strategy of macro and micro structure.
2. Experimental
2.1. Fabrication of CNTs/PyC foam
The Ni foam template (Alantum Advanced Technology
Materials Shenyang, 1.6 mm thickness and 320 g·m−2 in area
density) was ultrasonically cleaned and then soaked in
dopamine (DA) suspension (dispersed in 30 mmol·L−1 Tris
buffer, 2 mg·mL−1, pH = 8.5) for four cycles. The reaction
condition was kept for 12 h under light exclusion. After soak-
ing, the PDA@Ni foam was heat-treated in a tube furnace
(GSL-1100, Hefei Kejing Materials Technology Co.) at
450°C in an inert atmosphere. The sample was then sub-
merged in 3 mol·L−1 HCl solution for 24 h at 80°C to com-
pletely dissolve the nickel and obtain a 3D free-standing PyC
foam. For the preparation of functionalized PyC, the sample
571
was again immersed in DA suspension for 1 h under the same
condition. The functionalized PyC foam was then immersed
in Co(CH3COO)2 solution (5 mg·mL−1) for 3 h, washed with
deionized water several times, and dried under 80°C. Cobalt
catalyst was then uniformly loaded onto the sample surface.
The as-prepared PyC foam was heated to 600°C and held for
5 min in a tube furnace under H2/Ar (20vol%, 200 mL·min−1)
to reduce the cobalt catalyst. CNTs were then in-situ grown
in the PyC foam under 600°C by flowing the liquid precurs-
or (acetone) and H2/Ar carrier gas mixture (20vol%, 200 mL·
min−1) into the furnace at ambient pressure. The reaction time
was 10, 20, 30, 40, and 50 min.
2.2. Characterization
The crystal structure of CNTs/PyC foam was identified by
an X-ray diffractometer (XRD, Rigaku D/Max-2400, Japan)
using Cu target Kα radiation (λ = 0.15406 nm) at a working
voltage of 40 kV, current of 100 mA, scanning step of 0.02°,
and scanning range of 5°–70°. Raman spectra were meas-
ured by a Renishaw Ramoscope (Confocal Raman Micro-
scope, inVia, Renishaw, He–Ne laser, λ = 514 nm). The mor-
phology of the CNTs/PyC foam was observed by a scanning
electron microscope (SEM, FEI, 5 kV) and a transmission
electron microscope (TEM, FEI-Tecnai, 200 kV). The
CNTs/PyC foam was ultrasonically dispersed in ethanol for
30 min and then dropped onto a TEM grid for TEM observa-
tions. The direct current (DC) conductivity of the CNTs/PyC
foam was calculated according to Ohm’s law using the two-
probe measurement. The sample was cut into a standard cube
with two ends completely connected to the copper wires us-
ing a brushing silver paste. Resistance was directly measured
by volatility, and the average value was obtained after mul-
tiple measurements using Keithley 6220 DC power supply.
Conductivity was calculated according to the following
equation of Ohm’s law:
l
σ= (1)
RS
where σ is the electrical conductivity of the material, l is the
length between the end faces of the silver paste coated on the
sample to be measured, S is the cross-sectional area of the
sample, and R is the measured resistance. The wave-guide
method was used to measure the dielectric properties of
CNTs/PyC foam by a VNA (Anritsu, MS4644A). The
sample was cut with a dimension of 22.86 mm × 10.16 mm.
RC was calculated from the complex permeability and per-
mittivity according to the following equations [29]:
Zin − 1
RC = 20lg (2)
Zin + 1
√
µr ( √ )
Zin = tanh j2π µr εr f d/c (3)
εr
where Zin is the normalized input impedance, εr is the relative
complex permittivity (εr = ε′ − jε″), µ r is the relative com-
plex permeability (µ r = µ' − jµ″), j is the imaginary part unit,
c is the velocity of light in the free space, f is the frequency,
and d is the sample thickness. Here, µ' was approximately
equal to 1, and µ″ was approximately equal to 0 because the
572
materials exhibited negligible magnetic properties. RC fre-
quency range smaller than −10 dB was defined as EAB.
3. Results and discussion
3.1. Structure design strategy
The design of material structure mainly consists of two as-
pects: microstructure and macroscopic configuration. In
terms of macroscopic configuration, we selected 3D porous
structure for the following advantages. First, this structure
can greatly reduce the density of the material. Second, the
porous structure is beneficial in adjusting the permittivity and
improving the impedance matching. According to the Max-
well Garnett theory, a change in pore volume correspond-
ingly alters effective permittivity. Therefore, the pores could
tune the permittivity and impedance matching. Finally, when
the aperture satisfies 2πh/λ ≈ 1 (where h is the cell size of ma-
terials and λ is the wavelength of the electromagnetic (EM)
wave), the porous structure facilitates the multiple reflections
of incident electromagnetic wave. The electromagnetic wave
energy is repeatedly attenuated to improve the absorption
properties. For their application in different wavebands, por-
ous materials must be prepared with tunable pore size. In-
spired by the adhesion of mussels, the DA monomer can con-
tinuously oxidize and self-polymerize on any substrate sur-
face to form a PDA film. The thickness can be adjusted ac-
cording to the reaction conditions. When the thickness con-
stitutes enough strength to support the 3D structure, the pre-
cursors of porous PyC foam can be quickly obtained by etch-
ing the templates. The aperture size is adjusted according to
the template structure.
However, the conductivity of PyC foam is extremely low
due to its low crystallization degree. Although it has suitable
impedance matching characteristics for incident electromag-
netic wave, its conductivity loss is weak and cannot meet the
requirements of EA. Materials with high absorbing capacity
need to have a low real part of the dielectric constant and an
appropriate conductivity (1 S·m−1). Therefore, introducing
strong dielectric loss materials to PyC foam is necessary to
improve its EA performance. Compared with crystalline
CNTs, amorphous CNTs have moderate conductivity and
better impedance matching characteristics and can be used as
an excellent electromagnetic absorbent with abundant struc-
tural defects and nanoscale interfaces. On the microscale, the
hierarchical structure nanocomposite obtained by combining
amorphous CNTs and PyC foam can form abundant nano
heterogeneous interfaces and conductive connections. In ad-
dition, the dielectric loss of CNTs/PyC foam is greatly im-
proved compared with that of PyC foam alone.
Nanomaterials are inevitably agglomerated, difficult to
disperse, and unevenly distributed. Controllable CNTs distri-
bution is an important technology that can be achieved
through in-situ catalytic growth. With this approach, each
CNT unit can play a full role and further improve the absorp-
tion efficiency. However, uniform CNTs distribution and im-
proved polarization loss are difficult to achieve using physic-
al mixing methods. Traditional catalyst preparation tech-
niques, including sputtering and coating, are unsuitable for
Int. J. Miner. Metall. Mater., Vol. 30 , No. 3 , Mar. 2023
porous substrates because of their complex pore wall struc-
ture. Thus, uniformly loading the catalyst particles in a por-
ous structure is difficult [30]. In this work, an active buffer
layer PDA containing a large number of catechol groups was
formed on the surface of the PyC foam. With Co(CH3COO)2
as a catalyst precursor, Co nanoparticles were uniformly
loaded onto the surface of the PyC foam through chelating so
that a uniform catalyst layer can be loaded onto the inner sur-
face of the 3D porous structure substrate [31]. Only this
method can produce uniformly and densely grown CNTs.
The length and content of CNTs can be adjusted by con-
trolling the reaction time to reach the most suitable conduct-
ivity and permittivity for the CNTs/PyC foam.
3.2. Morphology and crystalline phase
SEM images of the CNTs/PyC foam demonstrate the
growth and distribution of CNTs on the surface of the PyC
foam with increasing gas-phase reaction time, as shown in
Fig.1. Fig. 1(a) indicates that the PyC transformed by the
pyrolysis of the PDA coating layer can be self-supported into
a 3D foam structure after the Ni foam etching. Fig. 1(b) re-
veals that the surface of PyC is not smooth but has dense con-
vex particles. DA hydrochloride is a monomer molecule in-
volved in polymerization that first oxidizes to form dispersed
PDA aggregate particles and then further adheres to the sur-
face of the substrate.
According to the CNTs growth mechanism, CNTs uni-
formity can be determined by the dispersion of catalytic met-
al nanoparticles to a large extent. In the gas-phase reaction,
too high catalyst concentration will lead to catalyst agglom-
eration, and a large carbon source flow will speed up the de-
position rate of PyC and result in catalyst deactivation. After
the appropriate catalyst concentration and acetone flow rate
were selected, the microstructure of the composites was ad-
justed by changing the catalytic reaction time. Fig. 1(c–h)
shows that the composites maintained a 3D porous network
structure with an aperture of about 200–300 µm after the
catalytic growth of CNTs. For the 10 min reaction time, most
of the growing CNTs were still in the initial stage, and only
some long CNTs scattered on the PyC foam surface. The
content of CNTs was only 16.7wt%. The length and distribu-
tion of CNTs significantly changed with the gradual prolong-
ation of reaction time. When the time was extended to
50 min, villous CNTs with a length of more than 10 µm grew
uniformly on the pore walls of the PyC foam and the content
increased to 43.2wt%. The pores in the PyC foam provided
enough space for CNTs growth and a broad path for the pen-
etration of the gaseous carbon source.
Fig. 2(a) shows the densely and uniformly grown CNTs
with a diameter of about 25 nm on the PyC substrate. The
high magnification shows the in-situ grown CNTs have an
amorphous microstructure because of the low reaction tem-
perature (Fig. 2(b)). Co catalysts can be found on top of the
CNTs, which is consistent with the top growth mechanism.
Raman spectroscopy is helpful in characterizing the de-
fect and structure of carbon materials. Fig. 2(c) exhibits two
prominent Raman peaks at ~1300 and ~1580 cm−1 corres-
ponding to the D and G bands of carbon, respectively. By
L. Kong et al., Ultralight pyrolytic carbon foam reinforced with amorphous carbon nanotubes for broadband ...
(a) CNTs: 0wt%
200 μm
(c) CNTs: 16.1wt%
200 μm
(e) CNTs: 25.6wt%
200 μm
(g) CNTs: 43.2wt%
200 μm
Fig. 1. SEM images of PyC foam and CNTs/PyC foam at different reaction times: (a–b) 0 min; (c–d) 10 min; (e–f) 30 min; (g–h) 50 min.
contrast, after the growth of CNTs in PyC foam, the intensity
of the D band gradually exceeded that of the G band, indicat-
ing that the in-situ grown CNTs have many defects and a low
crystallization degree. The crystal structure of CNTs/PyC
foam was analyzed by XRD, as shown in Fig. 2(d). The typ-
ical peaks of both samples were observed at 9.5°, corres-
ponding to the matrix component of PyC with a low graphit-
ization degree. After the catalytic growth of CNTs, a broad
peak appeared at 26.3°, corresponding to the (002) crystal
planes of graphite structure, thus confirming the low graphit-
ization degree. In addition, two diffraction peaks appeared at
41.2° and 51.5°, corresponding to the (111) and (200) crystal
planes of Co, respectively [32].
3.3. Dielectric properties
The dielectric constant of the samples was measured in X-
band (8.2–12.4 GHz) by the wave-guide method, as shown in
Fig. 3(a–b). The real part of the permittivity (ε′) corresponds
to the storage capacity of electromagnetic wave energy, and
the imaginary part of the permittivity (ε″) corresponds to the
dissipation capacity of electromagnetic wave energy [33].
The ε′ and ε″ of pure PyC foam were ~1.26 and ~0.03, re-
spectively. The extremely low permittivity indicates the low
573
(b)
5 μm
(d)
5 μm
(f)
5 μm
(h)
5 μm
dielectric loss, resulting in the high transmission of incident
electromagnetic waves. After the in-situ growth of CNTs on
PyC foam for 10, 30, 40, and 50 min, the value range of ε′
was 1.23–1.44, 1.43–1.6, 1.43–1.63, and 1.65–1.78, respect-
ively, and that of ε″ ranged 0.05–0.22, 0.39–0.58, 0.58–0.84,
and 0.9–1.3, respectively. As shown in the curves of the real
and imaginary parts of permittivity with each sample in the
figure, on the whole, ε′ began to show a decreasing trend
with increasing frequency. This finding may be attributed to
the electrons in CNTs that are responsible for polarization at
low frequency. ε″ also showed a decreasing trend in the fre-
quency range 8.2–12.4 GHz. According to similar reports on
carbon materials, a relaxation peak in ε″ occurs below
8.2 GHz [34]. Among the different samples, ε′ and ε″
showed an overall gradual upward trend with increasing re-
action time. The dielectric loss in X-band was further ana-
lyzed by using the loss tangent (tan δ = ε″/ε′) of PyC foam
(black line) and CNTs/PyC foam, as shown in Fig. 3(c).
When the permittivity meets the impedance matching re-
quirements, a high dielectric loss means a high EA capacity.
The results showed that the dielectric loss increased with the
growth time of CNTs from the initial loss tangent value of
0.01–0.02 to the maximum value of 0.53–0.74 at different re-
574 Int. J. Miner. Metall. Mater., Vol. 30 , No. 3 , Mar. 2023

(a) (b)

PyC Co

CNTs

CNTs

500 nm 50 nm

(c) (d)
D
G C
PyC
Relative intensity / a.u.

Relative intensity / a.u.

(002)
Co
2D D+G (111) Co
(200)

CNTs/PyC foam CNTs/PyC foam

PyC foam
PyC foam

1000 2000 3000 4000 10 20 30 40 50 60 70

Raman shift / cm−1
Fig. 2. (a–b) TEM and HRTEM images of CNTs/PyC foam, (c) Raman spectra of PyC foam and CNTs/PyC foam, and (d) XRD
spectra of PyC foam and CNTs/PyC foam.
action time. For further exploration of the dielectric loss
mechanism, resistance and conductivity were measured ac-
cording to Ohm’s law, as shown in Fig. 3(d). When the CNTs
reached a certain amount, the conductivity exceeded the
threshold and increased rapidly from 2.21 × 10−7 to 0.32
S·m−1, an increase of nearly 1.5 × 106 times. According to the
Debye theory [35−36], ε″ can be calculated by Eq. (4) as fol-
lows:
σ σ
ε′′ = = (4)
ωε0 2π f ε0
where ε0 is the free space dielectric constant (8.854 × 10−12
F·m−1), and ω is the angular frequency. Fig. 3(d) shows the
relationship between the conductivity of the material and the
average value of ε″. According to this figure, the increase in
the two factors corresponded to each other, that is, the dielec-
tric loss of materials depends on their conductivity. The in-
crease in ε″ was ascribed to the continuous growth of CNTs,
which correspondingly increases the conductivity of the
composite.
In general, the dielectric loss of carbon materials mainly
includes conductivity loss ε″c and polarization loss εp″ (dipole
polarization and interface polarization) [37]. The contribu-
tion of these two loss mechanisms can be calculated as fol-
lows:
(εs − ε∞ ) ωτ σ
ε′′ = ε′′p + ε′′c = + (5)
1 + (ωτ)2 ωε0
2θ / (°)
(εs − ε∞ ) ωτ
ε′′p = (6)
1 + (ωτ)2
σ
ε′′c = (7)
ωε0
where εs is the static permittivity (ω→0, ε = εs), ε∞ is the op-
tical frequency permittivity (ω→∞, ε = ε∞), and τ is the re-
( )
dA εB +dB εA
laxation time . The polarization loss calcu-
dA σB + dB σA
lated by Eq. (6) is shown in Fig. 3(e). The polarization loss of
the composite increased with prolonged reaction time. The
enhanced interface polarization loss can be attributed to the
large number of heterogeneous interfaces and nanoscale mi-
cro capacitors formed by the CNTs grown on the PyC foam
surface. Interface polarization at macroscopic heterogeneous
interfaces mainly responds in the MHz band because it takes
too long to respond in the GHz band. However, the presence
of a large number of nano-level heterogeneous interfaces and
the nano-effect affects the response band of interface polariz-
ation. The corresponding band of the polarization effect of
the nanoscale heterogeneous interface can move from MHz
to high frequency GHz [14]. Conductivity loss was calcu-
lated using Eq. (7), as shown in Fig. 3(f). The results showed
that the conductivity loss increases significantly with the in-
creasing of reaction time, which corresponds to the increase
of the conductivity. The effect of free electrons on ε″ is great-
er than that of polarization loss. Under the influence of an ex-
L. Kong et al., Ultralight pyrolytic carbon foam reinforced with amorphous carbon nanotubes for broadband ... 575

1.9 1.6 1.0

Imaginary part of permittivity

0 min 30 min 0 min 30 min
(a)
1.4
(b) 1.9 (c) 0 min 30 min
Real part of permittivity

1.8 10 min 40 min 10 min 40 min 10 min 40 min

0.8
50 min 1.2 50 min 50 min
1.7 0.7
1.0 0.6
1.6 0.8 0.5

tan δ
1.5 0.6 0.4
1.4 0.3
1.4
0.2
1.3 0.2 0.1
0 0
1.2
8 9 10 11 12 13 8 9 10 11 12 13 8 9 10 11 12 13
Frequency / GHz Frequency / GHz Frequency / GHz

0.35 1.2 0.9

0.7 (e) 0 min 30 min
0.30
(d)
10 min 40 min 0.8 (f) 0 min 30 min
1.0
Conductivity / (S·m−1)

0.6 0.7 10 min 40 min

50 min

Conductivity loss
0.25
Polarization loss
0.8 0.5 0.6 50 min
Average ε″

0.20 0.4 0.5

0.6
0.15 0.3 0.4
0.4 0.3
0.10 0.2
0.2 0.2
0.05 0.1 0.1
0 0 0 0
0 10 20 30 40 50 8 9 10 11 12 13 8 9 10 11 12 13
Reaction time / min Frequency / GHz Frequency / GHz
Fig. 3. Relationship between dielectric constant and frequency of CNTs/PyC foam at different CNTs growth times: (a) real part
permittivity; (b) imaginary part permittivity; (c) loss tangent; (d) average ε″ and conductivity; (e) polarization loss; (f) conductivity loss.

ternal electromagnetic field, CNTs can form conductive cur- reaction time was due to the shortened relaxation time of
rents within the material, thus causing the loss of electromag- electron polarization. The imaginary part of the dielectric
netic energy in the form of heat energy. A comparison of constant also increased due to the increase in conductivity.
contributions revealed that polarization loss played a more However, the growth rate of ε″ was higher than that of ε′ by
dominant role than conductivity loss when the CNTs began nearly 100 times, indicating the fast increase in the conduct-
to grow on the PyC foam. When the CNTs had grown for 30
ivity loss of CNTs/PyC foam. At first, the PyC foam had ex-
min or longer, although the conductivity loss and interfacial
tremely low conductivity and barely exhibited conductivity
polarization loss of the composite showed an increasing
loss. Owing to the strong conductivity generated by the net-
trend, the contribution of the former increased significantly
and gradually exceeded that of the latter. This finding was at- work structure of densely distributed CNTs, the conductivity
tributed to the conductive network formed by the CNTs with loss of the composite was greatly improved.
high enough contents. Characteristic impedance (Z) is an important indicator to
Fig. 4(a) shows the comparison of change in the dielectric evaluate the electromagnetic absorption properties and the in-
√
constant of CNTs/PyC foams. The average dielectric con- µ
cidence of electromagnetic wave in materials. Z = =
stant of CNTs/PyC foam grown for 50 min increased by 36% ε
√ √ √
and 3872% in the real and imaginary part, respectively. The µ0 µr µr
increase in the real part of the dielectric constant with a long · = Z0 · , where Z0 is the intrinsic imped-
ε0 εr εr
360
1.8 (a) ε′ (b) 0 min 40 min
ε″ 10 min 50 min
1.6
340 30 min
36%
1.4 18% 22%
5%
Average permittivity

1.2 3872% 320

1.0
Z/Ω

0.8 300
2275%

0.6 1571%
280
0.4

0.2 307%
260
0
0 10 30 40 50 8 9 10 11 12 13
Reaction time / min Frequency / GHz
Fig. 4. Comparison of the (a) dielectric constant and (b) characteristic impedance of CNTs/PyC foams at different growth time.
576 Int. J. Miner. Metall. Mater., Vol. 30 , No. 3 , Mar. 2023

ance of free space (Z0 = 377 Ω), µ 0 is the permeability of va-
cuum (1.26 × 10−6 H·m−1), and ε0 is the permittivity of vacu-
um (8.85 × 10−12 F·m−1). When Z approaches the free space,
the electromagnetic wave energy can enter the absorber with
less surface reflection. Fig. 4(b) shows the Z of CNTs/PyC
foam with different growth time. The largest characteristic
impedance was observed for PyC foam. The Z of CNTs/PyC
foam decreased with prolonged growth, indicating that the
impedance matching gradually deteriorated. The lowest Z of
254–276 Ω was found for the CNTs/PyC foam with 50 min
growth.
3.4. EM absorption properties
On the basis of the metal backplane model, the RC of the
samples was determined from the complex permeability and
permittivity using Eq. (2) [29]. In general, RC and EAB
should be considered comprehensively in evaluating the per-
formance of EA materials.
Fig. 5 is the 3D representation of RC for CNTs/PyC foam
in X-band with different thicknesses and catalytic growth
time. Fig. 5(a) shows that the RC of the PyC foam was the
smallest at only −0.6 dB when the thickness and frequency
were 8.18 mm and 12.4 GHz, respectively. The RC of the
PyC foam cannot reach −10 dB in any frequency and thick-
ness, indicating its poor EA property. When CNTs were
grown on the PyC foam, the EA capacity of the latter was
strengthened, and the frequency corresponding to RCmin shif-
ted to a low level. With the growth time of 50 min, the EA
property of CNTs/PyC foam was significantly enhanced, as
illustrated in Fig. 5(d), with the RC reaching the minimum
value of −29.6 dB at 8.2 GHz and 7.94 mm. The above res-
ults revealed that the EA properties of CNTs/PyC foam are
regulated by its microstructural changes, and excellent EA
properties are achieved when the growth time reaches 50 min.
Fig. 6(a) shows the RC curves of CNTs/PyC foam with
different catalytic growth time in the X-band. No EAB was
obtained for the samples with a growth time of less than 50
min. When the catalytic growth time was 50 min, the EAB
was always wide enough to cover the whole X-band. In addi-
tion, the RC values in the whole X-band were all less than
−13.3 dB. The thickness of the sample has a significant ef-
fect on the EA properties, resulting in significant change in

RC / dB RC / dB
0 (a) −0.1
(b) −4
−0.2 −5
RC / dB

−0.5 −6
RC / dB

12.4 GHz −0.3

−10 8.2 GHz
8.18 mm −8
−0.4 10 mm
−1.0 −0.6 dB −15 −11.4 dB
10
12 −0.5 10 9 −10
8 11 8 11 12
d/m 6 10 −0.6 d/m 7 6 10
m 9 / GHz m 5 8 9 G H z
c y cy /
Frequen Frequen

RC / dB RC / dB
−4
(c) (d) −10
−5 −6 −10
−15
RC / dB
RC / dB

−8 −15
−10 −20
8.2 GHz −10 −25 8.2 GHz −20
−15 9.04 mm −30 7.94 mm
10 9 −14.5 dB −12 10 9 −29.6 dB −25
8 11 12 8 11 12
d/m 7 6 9 10 −14 d/m 7 6 9 10
m 5 8 cy / G H z m 5 8 cy / G H z
Frequen Frequen
Fig. 5. 3D reflection coefficient of (a) pure PyC foam, (b) 30 min CNTs/PyC foam, (b) 40 min CNTs/PyC foam, and (d) 50 min
CNTs/PyC foam.

0 (a) −5
(b)

−5 −10

−10 −15
RC / dB

RC / dB

−13.3 dB

−15 −20

5.0 mm 5.5 mm
−25
−20 6.0 mm 6.5 mm
10 min 30 min 7.0 mm 7.5 mm
−30 8.0 mm
−25 40 min 50 min
8 9 10 11 12 13 8 9 10 11 12 13
Frequency / GHz Frequency / GHz

Fig. 6. Reflectance coefficient of CNTs/PyC foam: (a) different growth time with 6.6 mm; (b) different thickness at 50 min.
L. Kong et al., Ultralight pyrolytic carbon foam reinforced with amorphous carbon nanotubes for broadband ... 577

RCmin and EAB [38]. The RC values of CNTs/PyC foam with
50 min growth time and different thicknesses (5–8 mm) are
shown in Fig. 6(b). With the increasing matching thickness,
the RCmin transferred to a low frequency and the EAB gradu-
ally expanded. These phenomena can be explained by the law
of quarter-wavelength attenuation.
For the excellent EA performance of CNTs/PyC foam, a
potential absorption mechanism was proposed as shown in
Fig. 7. First, the 3D network and submillimeter porous struc-
ture allow the electromagnetic wave to enter the material and
form multiple reflections, thus increasing the propagation
distance of electromagnetic wave and resulting in the mul-
tiple dissipations of electromagnetic wave under alternating
electromagnetic fields [39]. Second, the in-situ grown CNTs
on the PyC foam presents a uniform distribution. The moder-
ate conductivity of CNTs improves the problem of insuffi-
cient conductivity of PyC foam without causing impedance
mismatch. In addition, under the action of alternating electro-
magnetic fields, electric charges accumulate on the in-situ
grown CNTs surface and the heterogeneous interface formed
by the CNTs and PyC foam, leading to polarization loss
[40–41]. Meanwhile, migration conductance within CNTs
and hopping conductance between each CNT might have oc-
curred [42]. The electron conduction and transition in the
CNTs transform the electromagnetic wave energy into heat
energy, which constitutes conductivity loss [43]. In sum-
mary, the in-situ grown CNTs enrich the loss mechanism of
PyC foam and enhance its electromagnetic absorption per-
formance.
Fig. 8(a) exhibits the histogram of serial samples with op-
timal thickness, bandwidth, density, and RCmin in the present
work, and Fig. 8(b) and Table 1 summarize the EA proper-

Incident waves
Ni foam PyC foam CNTs/PyC foam

PDA
Catalytic
coating
growth
Ni
etching
CNTs

Transmitted
waves
ehup E

Electron
transition Heterointerface Capacitor
22 mg·cm−3

Fig. 7. Schematic of EM absorption enhancement mechanisms in CNTs/PyC foam.

(a) −29.6 dB (b) MAMs X-band (EAB≤−13 dB) Bandwidth / GHz

This work 4.2
CNTs/PyC foam Carbon honeycomb [52] 2.3
Porous carbon [57]
Carbon 1.6
22.0 mg·cm−3 3D carbon foams [39]
3.2
materials C foam [58]
GF [27] 1.0
3.6
HCNFs-coated CFs [44] 3.9
TRGN [45] 3.4
7.9 mm Carbon
CNTCF [59]
PCHMs [28]
1.2
2.2
4.0 GHz CNT/RGO foam [16]
composite 3.0
PANI /Fe3O4/MWCNT [47]
materials 3.0
SiC/PyC-coated CF [53]
Co/N-doped CNTs/CS [48] 2.3
50 RGO/NBR [51] 2.6
2.5
in

40 2.6
/m

CF@G@PPy [49]
SiCnw/GA [46] 3.3
30
me

RGO/ZnOnws foam [24] 3.2

Composite C/SiCnws foam [56] 1.8
n ti
B

10 Ti3C2Tx/SiCnws foams [60] 3.5

|/d

materials
)

ctio
3
·cm −

RGO/SiCnws foam [50] 2.6

|RC

0 RGO/PPy/Fe3O4 acrogel [54] 2.2

Rea
/m

CF/MXene [55] 2.2

(mg

Hz
ess

/G

8 9 10 11 12
ty /

ckn

idth

Frequency / GHz
nsi

Thi

dw
De

Ban

Fig. 8. (a) Histogram of serial samples with optimal thickness, bandwidth, density, and minimum RC and (b) comparison of
CNTs/PyC foam with representative EA materials (marked 8.2–12.4 GHz).
578 Int. J. Miner. Metall. Mater., Vol. 30 , No. 3 , Mar. 2023

Table 1. EM absorption performance of CNTs/PyC foam and some representative EA materials in the X-band
Density / Thickness / RCmin / Frequency range (≤−13 dB) / Bandwidth (≤−13 dB) /
Materials Ref.
(mg·cm−3) mm dB GHz GHz
This
CNTs/PyC foam 22.0 6.6 −29.6 8.2–12.4 4.2 work
HCNFs-coated CFs — 2.5 −32 8.5–12.4 3.9 [44]
GF 14 10 −29 8.8–12.4 3.6 [27]
TRGN 12.4 3.5 −43.6 9–12.4 3.4 [45]
SiCnw/GA 41.3 3 −24.9 8.5–11.8 3.3 [46]
3D carbon foams 25 3 −24 8.8–12 3.2 [39]
RGO/ZnOnws foam — 4.8 −27.8 8.2–11.4 3.2 [24]
PANI/Fe3O4/MWCNT — 4 −16.5 8.8–11.8 3.0 [47]
Co/N-doped CNTs/Carbon 8 2.5 −47.8 9.8–12.4 2.6 [48]
Sponge
CF@G@PPy 8.8 2.5 −24.5 9.2–11.8 2.6 [49]
RGO/SiCnws foam 97 3 −19.6 8.7–11.3 2.6 [50]
RGO/NBR — 3 −57 8.5–11 2.5 [51]
Carbon honeycomb 67.9 30 −25 8.5–10.8 2.3 [52]
SiC/PyC-coated CF — 3.5 −22.5 9.2–11.5 2.3 [53]
PCHMs — 3.3 −32 9–11.2 2.2 [28]
RGO/PPy/Fe3O4 aerogel 38.3 3 −49.2 10.2–12.4 2.2 [54]
CF/MXene 6 4.5 −45 8.2–10.4 2.2 [55]
CNT/RGO foam 97 2.75 −55 9–11 2.0 [16]
C/SiCnws foam 9.2 2.85 −49.1 10.6–12.4 1.8 [56]
Porous carbon 90 1.5 −19.4 10.8–12.4 1.6 [57]

ties in the X-band of representative EA materials in literature. Acknowledgements

Density and EAB are the two key factors of EA materials.
The density of 3D porous CNTs/PyC foam is only 22.0
mg·cm−3, which is better than most other light EA materials,
such as carbon foam [58], CNTCF [59] and Ti3C2Tx/SiCnws
foam [60]. In particular, it exhibits a broadband electromag-
netic wave absorption lower than −13.3 dB in the whole X-
band compared with other typical EA materials. Therefore,
CNTs/PyC foam has a broad range of practical applications
as an EA material with ultralight and broadband charac-
teristic.
This work was financially supported by the National Nat-
ural Science Foundation of China (No. 51702197), the Creat-
ive Research Foundation of the Science and Technology on
Thermostructural Composite Materials Laboratory, the Nat-
ural Science Foundation of Shaanxi Province (No. 2022JM-
248), and the Doctoral Scientific Research Foundation of
Shaanxi University of Science & Technology (No. BJ16-06).
Conflict of Interest

4. Conclusions The authors declare no known competing financial in-

We prepared a PyC foam matrix by a template method and
obtained CNTs/PyC foam by the in-situ growth of amorph-
ous CNTs. Controlling the catalytic growth time of CNTs can
change the microstructure of the CNTs/PyC foam. EA prop-
erties are closely related to the growth and distribution of
CNTs on the PyC substrate surface. When CNTs with high
dielectric loss are in-situ grown on the PyC foam with low
dielectric loss, rich heterogeneous interfaces and moderate
conductivity meeting the impedance matching requirements
are achieved. Under alternating electromagnetic fields, the
micro-current formed by CNTs and the interface polarization
play an important role in EA. With its ultralow density of
22.0 mg·cm−3, CNTs/PyC foam has RCmin of −29.6 dB. In
particular, CNTs/PyC foam can achieve strong absorption of
less than −13.3 dB in the whole X-band. This work provides
an idea for manufacturing an excellent broadband EA materi-
al with light weight and strong absorption capacity.
terests or personal relationships that could influence the work
reported in this manuscript.
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