Materials Research Express

PAPER

Microstructures and properties of glass fiber reinforced PTFE composite

substrates with laminated construction
To cite this article: Fangkai Huang et al 2019 Mater. Res. Express 6 075305

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 Mater. Res. Express 6 (2019) 075305 https://doi.org/10.1088/2053-1591/ab11f2

PAPER

Microstructures and properties of glass fiber reinforced PTFE

RECEIVED
15 November 2018
composite substrates with laminated construction
REVISED
5 March 2019
ACCEPTED FOR PUBLICATION
Fangkai Huang1,2, Ying Yuan1,2 , Zehua Jiang1,2, Bin Tang1,2 and Shuren Zhang1,2
21 March 2019 1
National Engineering Center of Electromagnetic Radiation Control Materials, University of Electronic Science and Technology of China,
PUBLISHED Jianshe Road, Chengdu 610054, People’s Republic of China
2
3 April 2019 State Key Laboratory of Electronic Thin Films and Integrated Devices, University of Electronic Science and Technology of China, Jianshe
Road, Chengdu 610054, People’s Republic of China
E-mail: yingyuan@uestc.edu.cn

Keywords: composites, polymers, PTFE, ceramics

Abstract
Three kinds of composite substrates have been fabricated by stacking layers of glass fiber cloth (GFC) or
glass fiber mat (GFM) impregnated with polytetrafluoroethylene (PTFE). The difference of the three
kinds of substrates is the layered structures, composed of simplex GFC or GFM, or GFC and GFM
alternately. The effects of glass fiber types and laminated constructions on the physical properties of
composite substrates, such as dielectric constant (εr), dielectric loss (tgδ), water absorption, coefficient of
thermal expansion (CTE) and microstructures were studied. The PTFE/GFM composites show similar
performances with PTFE/GFC composites. The results demonstrate that the dielectric constant (GFM
up to 2.23, GFC up to 2.24) and dielectric loss (GFM up to 0.0016, GFC up to 0.0018) are increased with
an increase of the number of layers, on the contrary, the temperature coefficient of dielectric constant (τε)
of composites has a decreasing tendency (GFM of −121 ppm °C, GFC of −114 ppm °C). At the same
time, the water absorption of composites is decreased with an increase of the number of layers, which is
almost twice that of other literatures (GFM of 0.019% and GFC of 0.005%). In consideration of low CTEx
and CTEy of PTFE/GFC composites and low CTEz of PTFE/GFM composites, composite substrates
with PTFE and alternate GFC and GFM were prepared, exhibiting relatively low CTE of 28.64, 30.52,
223.7 ppm C−1 at X, Y, Z directions, which is obviously superior to other substrates of the same type.

1. Introduction

Polytetrafluoroethylene (PTFE) polymer is widely used for microwave substrates, which are applied to radar system
and satellite communication, because of superior electrical properties at high frequencies, chemical inertness, ability
of withstanding high temperature and low water absorption [1–3]. However, the deficiencies of PTFE limit its
application to substrates, such as high linear coefficient of thermal expansion (CTE∼109 ppm C−1) and low surface
energy [4–6]. One of approaches to decrease the high CTE of PTFE polymer is adding ceramic powders or glass fiber
to PTFE matrix [7–10]. As well known, ceramic reinforced PTFE composites have relatively higher dielectric
constants compared with glass fiber reinforced PTFE composites, due to high dielectric constants and filling content
of ceramic in PTFE based composites [11]. As reported by Murali et al [9], fused amorphous SiO2 filled PTFE
composite has the lowest dielectric constant of approximate 2.9 among ceramic filled PTFE composites, resulting
from a low dielectric constant of amorphous SiO2 (εr =3.8). Generally, the velocity of signal propagation is
determined by laminate dimension and dielectric constant, which is faster as the dielectric constant of substrate is
lower. Laminate εr is determined by the respective εr of the materials used to manufacture laminates, including resin
and fillers, such as ceramic and glass fiber, as well as the amounts of components. Therefore, glass fiber reinforced
PTFE composite substrate is more appropriate for high speed electrical circuit. In this work, two kinds of glass fiber
were used as reinforcement materials for composite substrates: one is glass fiber mat (GFM), and the other is glass
fiber cloth (GFC). The differences between GFC and GFM are the preparation process and their corresponding
structures. Glass fibers are randomly distributed in GFM and connected by organic binder. The loose spongy

© 2019 IOP Publishing Ltd

Mater. Res. Express 6 (2019) 075305 F Huang et al

Table 1. Properties of glass fiber [12].

Properties GFM GFC

Diameter of glass fiber (μm) 9–12 4.5

Thickness (μm) 130 28
Grams per square meter (g m−2) 30 23
Dielectric constant 6.1 6.1
Dielectric loss 0.0006 0.0006
Coefficient of thermal expansion (ppm °C−1) 5.4 5.0

structure of GFM is in favor of PTFE resin adherence to glass fibers. GFC is weaved by weaving loom, therefore, it has
a denser structure and higher strength compared with GFM. Although the structure is different, both GFC and GFM
are made of the same E-glass fiber, which has extremely low alkali metal content (<0.8 wt%). The alkali metal ions in
the glass migrate under the action of an electric field, resulting in an increase in leakage current and dielectric loss.
Therefore, alkali-free E-glass fiber has high insulation resistance and low dielectric loss, which is a suitable
reinforcement material for microwave composite substrate.
The properties of composite substrate depend not only on components, but also on its thickness. The circuit
material companies afford series of composite substrates with different thickness. There are some dominant
factors controlling the thickness of composite substrate, such as PTFE content, thickness of prepreg and number
of prepreg layers. Our previous work demonstrated that the layered structure affected the properties of
substrates, such as dielectric constant and CTE. In previous literatures, effects of thickness on the properties of
layered structure composite substrate were seldom researched.
Glass fiber mat reinforced PTFE composite (PTFE/GFM) substrate provides outstanding properties, but
this kind of substrate has a relatively higher CTE at X (CTEx) and Y directions (CTEy). In-plane restraint from
GFC contributes to lower CTEx and CTEy for glass fiber cloth reinforced PTFE composite (PTFE/GFC).
However, high CTEz still exists for PTFE/GFC substrate that gets rise to unreliability of plated through hole
(PTH) [4]. The characteristic will probably result in less dimensional stability because of CTE distinction
between composite substrates and copper foil. To decrease the CTE of composite substrate, either low CTE
fillers or low CTE structure are necessary. Therefore, we have used a new sandwich structure that combines the
advantages of GFM and GFC to improve the thermal expansion of the substrate.
In this study, substrate composites with layered structure were prepared using PTFE, GFC and GFM as raw
materials. The type of glass fiber, including GFM and GFC, and the effects of laminated construction on the
properties, such as dielectric properties, coefficient of thermal expansion, water absorption, temperature
coefficient of dielectric constant and microstructure, were studied and discussed in detail.

2. Experiment

2.1. Material description

The GFM and GFC used in this work were provided by Shanxi Huate Fiberglass Corporation, China. The
properties of GFM and GFC are displayed in table 1. PTFE suspension (TE-3865C, DuPont, China) was used.
Perfluorooctyltriethoxysilane (F8261, C14H19F13O3Si, Guangzhou Jianyi chemical import and export co. Ltd,
China) was used for surface modification of glass fiber.

2.1.1. Modification of glass fiber

In this work, the coupling agent F8261 (1.2 wt%) was used for surface modification of GFM and GFC. Firstly, the
GFM and GFC were baked at 120 °C for 2 h. The coupling agent was hydrolyzed in alcohol and deionized water
at 55 °C for 1 h by water bath, in the meantime, the pH of mixture solution should be maintained between 4 and
6. The GFM and GFC were put in groove with hydrolyzed coupling agent at room temperature for 6 h. Finally,
the modified samples were sent into drying oven for 2 h for further dry.

2.1.2. Composites preparation

The modified GFM and GFC were impregnated with PTFE emulsion for 1 min, and then naturally dried.
After drying, the PTFE impregnated GFM and GFC were baked at 120 °C to remove residual water. The
impregnation, air-drying and baking procedures were repeated for three times. The next step is the calcining of
impregnated GFM and GFC at 200 °C for 4 h to remove the surfactant in PTFE. Then, the composites are
sintered at 370 °C for 4 h to eliminate the adhesive in GFM. Subsequently, the processed GFM (PTFE content:
91.2 wt%, GF content: 8.8 wt%) or GFC (PTFE content: 89.7 wt%, GF content: 10.3 wt%) were stacked in a
metallic mould and were heated in thermo compressor with a static pressure of 45 MPa. In consideration of

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Figure 1. The cross-sectional elevation view of PTFE/GFM/GFC composites.

Figure 2. The number of layers and thickness of different composites.

symmetry and thickness, the structure of PTFE/GFM/GFC laminate is designed in figure 1. The preparation
condition was similar to that of PTFE/GFM composites. Finally, PTFE/GFM, PTFE/GFC and PTFE/GFM/
GFC composites were obtained. The variation of composites’ thickness with an increase of layers were shown in
figure 2. Sample A to E are PTFE/GFM composites. Sample F to J are PTFE/GFC composites. As seen from
figure 2, the thickness of composites is increased with an increase of number of layers. The thickness of sample
D, sample J and sample K are almost the same.

2.2. Measurements
The dielectric constant (εr), dielectric loss (tgδ) and temperature coefficient of dielectric constant (τε) of the
composites were measured by Agilent E8363A microwave network analyzer with strip line resonator method
according to IPC-TM-650 2.5.5.5 specification. The range of testing frequency is from 1 GHz to 18 GHz. The
coefficients of thermal expansion (CTE) of the composites were measured by TMA 2940 referred to IPC-TM-
650 2.4.41. The water absorption of composites was measured as mentioned earlier by Murali et al according to
IPC-TM-650 2.6.2. The coefficients of thermal expansion were measured during −25 °C to 100 °C. The testing
specimens of dielectric constant, dielectric loss, temperature coefficient of dielectric constant and coefficients of
thermal expansion were 70 mm at length and 30 mm at width. The scanning electron microscopy (SEM) was
applied to obtain micro-morphology of the composites. The composites samples were cut by sharp knife and
then coated with a gold layer in vacuum.

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Figure 3. SEM images of two types glass fiber (a) GFM, (b) GFC.

Figure 4. (a)–(e) Surface SEM micrographs and h-j cross sectional micrographs of PTFE/GFM composites at different layers (a),
(f) 4 layers, (b), (g) 6 layers, (c), (h) 8 layers (d), (i) 10 layers and (e), (j) 12 layers.

3. Result and discussion

The properties of glass fiber reinforced polymer composites depend not only on the individual properties of fiber
and polymer, but also on other factors, such as the morphology, composition, distribution of filler and the
interfacial connection between fiber and matrix. Figure 3 shows morphologies of two types of glass fiber. It can be
observed in figure 3(a) that glass fibers connected by adhesive in GFM are randomly distributed. Figure 3(b) shows
that glass fibers in GFC are weaved without any adhesives. The structure of GFC is more compact compared with
GFM. According to table 1, diameter of glass fiber in mat and cloth are 9∼12 μm and 4.5 μm respectively.
SEM micrographs of the surface of composites are shown in figures 4(a)–(e), figures 5(a)–(e). As it can be seen,
there are many holes in surfaces but most of holes are closed on interior. Thus, these holes affect rarely water
absorption. The holes are resulted from the flow of fused PTFE and emission of impurities during sintering process.
The interstice is an important factor affecting moisture ingression and dielectric properties. Most interstices
occur at the interface between PTFE and glass fiber. Figures 4(f)–(j) shows cross section morphologies of PTFE/
GFM composites, which indicates that the glass fibers in PTFE/GFM composites are randomly distributed in x,
y and z direction. Moreover, it is obvious that the interstices are decreased with an increase of layers. As shown in
figures 4(f), (g), the interstices are obvious at the interface between PTFE and glass fiber when the number of
layers is less than 6. With an increase of layers, the interstices between PTFE and glass fiber are decreased
(figures 4(h), (i)) and disappear finally (figure 4(j)). In figure 4(j), the glass fiber and PTFE show a compact
interfacial microstructure without delamination.

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Figure 5. (a)–(e) Surface SEM micrographs and (f)–(j) cross sectional micrographs of PTFE/GFC composites at different layers (a),
(f) 3 layers, (b), (g) 6 layers, (c), (h) 9 layers (d), (i) 12 layers and (e), (j) 15 layers.

Figure 6. The variation of density and water absorption of (a) PTFE/GFM and (b) PTFE/GFC composites with number of layers.

Figures 5(f)–(j) shows cross section morphologies of PTFE/GFC composites. The glass fibers in cloth are
interwove and limited in two-dimensional plane, therefore, glass fibers in PTFE/GFC composites are mainly
distributed in x and y directions. It can be observed that the interface between PTFE and glass fiber is more
obvious than that of PTFE/GFM composites. With an increase of layers, the combination of PTFE and glass
fiber becomes more tightly and the interstices are decreased gradually. It was further proved that the changes of
composite microstructures have great influences on the properties of substrates, such as density, water
absorption, dielectric constant and dielectric loss, as shown in figures 6 and 7.

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Figure 7. The variation of dielectric constant and dielectric loss at about 10 GHz for (a) PTFE/GFM and (b) PTFE/GFC composites
with number of layers.

The density and moisture absorption of the composites are significant signals of porosity. Moreover, the
ideal composite substrate requires a low moisture absorption. The variations of density and water absorption
with number of layers for PTFE/GFM and PTFE/GFC composites are shown in figure 6. It can be found that the
density of laminate increases and the water absorption decreases with the increase of number of layers for PTFE/
GFM and PTFE/GFC composites. In figures 4(f)–(j) and figures 5(f)–(j), it is noted that glass fibers and PTFE are
more compact with the increase of layers.
The dielectric constant and dielectric loss are the most important properties for application of composite
substrates. The dielectric constant and dielectric loss of PTFE/GFM and PTFE/GFC composites at about
10 GHz are shown in figure 7. It is obvious that the dielectric constant and dielectric loss increase continuously
with an increase of number of layers. For two-component system composites, the theoretical dielectric constant
can be calculated according to Lichtenecker model (equation (1)). In equation (1), εr is the effective dielectric
constant of the composite and εr1 and εr2 are dielectric constant of PTFE and glass fiber. The V1 and V2 are
volume fraction of PTFE and glass fiber, respectively. The volume fraction can be calculated through
equation (2). The W1 is mass fraction of PTFE and W2 is mass fraction of glass fiber. Based on Lichtenecker
model, the dielectric constant of either PTFE/GFM or PTFE/GFC composite is invariable with different
number of layers because of the same content of PTFE and fiber in every composite substrate. However, the
interstices were decreased as increasing the thickness of substrate, proved by SEM observation, as shown in
figures 4(f)–(j), resulting in the increase of dielectric constant for PTFE/GFM composites. The increase in
dielectric constant is due to the tighter bonding of the glass fibers to the PTFE, resulting in a reduction in voids
within the composite. The dielectric constant of air is smaller than that of other components, so the dielectric
constant becomes large. The reduction of voids inside the composite reduces the dielectric loss of the composite,
but the test results show that the dielectric loss of the composite increases. This is because as the number of layers
increases, the interface of the composite material also increases, resulting in an increase in dielectric loss. The
effect of increased interface on dielectric loss is greater than the effect of void reduction on dielectric loss [13].

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Figure 8. The variation of τε and CTEx at temperature from −25 to 100 °C of (a) PTFE/GFM composites and (b) PTFE/GFC
composites with number of layers.

This is because larger interface volume can cause anharmonicity in the composite system which in turn increases
dielectric loss [14]. Therefore, as the number of superposed layers increases, the dielectric loss of the composite
material shows an increasing trend. PTFE/GFC composites show similar variation tendency of dielectric
properties with PTFE/GFM composites, as shown in figure 7(b).
log (er) = V1 log (er1) + V2 log (er2) (1)
W1 r1 W2 r 2
V1 = V2 = (2)
W1 r1 + W2 r 2 W1 r1 + W2 r 2

The temperature coefficient of dielectric constant (τε) of composites is a significant performance in

application. The important parameters which control the τε are the change in the polarizability of the material
with respect to its temperature and its linear coefficient of thermal expansion (CTE) (equation (3)) [15]. In this
equation, the first term represents the change in polarizability of the system, and the second term represents the
linear coefficient of thermal expansion. The dominant polarization for glass fiber is knew as ionic and electronic
polarizations which contribute to dielectric constant. On the other hand, electronic polarization is dominant
polarization in PTFE for the symmetrical structure. The internal particles have longer distance with composites’
expansion when temperature increases. Therefore, the increase of temperature strengthened ionic polarization
(this would lead to a positive τε). On the other hand, electronic polarization is attenuated when the composites
expand because the number of polarized particles in unit volume would decrease (this would result in a negative
τε), in the meantime the orientational polarization would be deceased (this would result in a negative τε). In
PTFE/glass fiber composites, the dominant polarization is electronic polarization, and therefore there are
negative τε for this PTFE/glass fiber composites. As seen from figure 8, the variation of τε and CTEx about two
types of composites are shown. The τε values have a tendency of decrease with increase of layers. In the
meantime, it is shown that two types of composite have a tendency of increase in CTEx. In equation (3),
influence of polarizability term is little compared with coefficient of thermal expansion term, furthermore,

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Mater. Res. Express 6 (2019) 075305 F Huang et al

Figure 9. (a) Surface SEM micrograph and (b)–(e) cross sectional micrographs of PTFE/GFC/GFM composite.

Table 2. The properties of PTFE/GFM/GFC composites.

Number of PTFE content GF content Thickness Dielectric Dielectric loss Water absorption
Sample layers wt% wt% (mm) constant (10−3) (%)

K 11 90.6 9.4 1.34 2.24 1.2 0.02

increase of CTEx can result in the decrease of second term. The variation of τε for PTFE/GFM composites and
PTFE/GFC composites are resembled. But the variation of τε of PTFE/GFC composites is smaller than PTFE/
GFM composites because glass fiber in cloth is interwove and there are tractions between glass fiber and glass
fiber to resist the expansion when temperature is increased.
Dk ⎛ 1 ¶a ⎞
te = ⎜ ´ - 3aL⎟ (3)
3 ⎝a ¶T ⎠

In consideration of dielectric properties and respective advantage of GFM and GFC, the complex structure,
alternate GFC and GFM impregnated with PTFE laminated composites, was prepared. The properties of PTFE/
GFM/GFC composite (Sample K) are provided in table 2. The thickness of complex PTFE/GFM/GFC
composite is close to that of PTFE/GFM (Sample D) and PTFE/GFC (Sample J). The results demonstrate that
GFC is thin and it can be applied to adjust CTEz of laminate. The surface micrograph and cross section
micrograph of PTFE/GFM/GFC composite are shown in figures 9(a)–(e). There are many holes in surface of
composite. As seen from figures 9(b)–(e), PTFE/GFM layer was sandwiched between PTFE/GFC layers. The
connections between PTFE/GFC layer and PTFE/GFM layer are compact.
Microwave substrates which are multi-layered and phase sensitive are required dimensional stability in
application. The CTE is a property which can’t be neglected. The CTE of PTFE/GFM composites, GFC
composites and PTFE/GFM/GFC composites are shown in figure 10. In figure 10, the CTE of composites
prepared by GFM in x direction and y direction are bigger than PTFE/GFC composites’, because glass fibers and
PTFE in GFC have traction in plane and glass fibers in GFM connected by adhesive with less traction. However,
the CTEz of PTFE/GFC composites are bigger than composites made by GFM. As well known, the PTFE has a
high linear coefficient of thermal expansion (CTE ∼109 ppm C−1) and dispersion of z direction glass fibers in
GFM contribute to the lower CTEz. According to the advantages of GFC and GFM, GFC and GFM are combined

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Mater. Res. Express 6 (2019) 075305 F Huang et al

Figure 10. The CTE of PTFE/GFM composites (Sample D), PTFE/GFC composites (Sample J) and PTFE/GFM/GFC composites
(Sample K).

to the layered structure composites. It can be seen in figure 10 that the CTEy of complex PTFE/GFM/GFC
composites decrease compared with composites made by GFM and the CTEz decrease compared with
composite made by GFC. The CTEx of GFM-GFC layers structure composite is smaller than PTFE/GFM
composites but it is bigger than PTFE/GFC composites. In summary, the GFM-GFC layers structure can
decrease the CTEz effectively while it changed CTEx and CTEy slightly.

4. Conclusion

The properties of glass fiber reinforced PTFE composite substrates with different number of layers have been
studied. The glass fiber reinforced PTFE composite substrates have many advantages such as low dielectric
constant, dielectric loss and water absorption. The properties of composite substrates can be influenced by
composition and layered structure. The dielectric constant (up to 2.23) and dielectric loss (up to 0.0016) of
PTFE/GFM composites increase with the increase of layers. The composites are more compact and the water
absorption is reduced to 0.019% when the layers increase. The variations of dielectric constant (up to 2.24),
dielectric loss (up to 0.0018), density and water absorption (as low as 0.005%) with number of layers for PTFE/
GFC composites are similar to those for PTFE/GFM composites. The τε of PTFE/GFC composites is smaller
than PTFE/GFM composites because plane stability of PTFE/GFC composites. Furthermore, the CTE of the
substrate composed of GFC impregnated with PTFE is 27.04, 31.46, 302.4 ppm °C at X, Y, Z directions,
respectively. By the way, CTE of PTFE/GFM is 38.81, 47.14, 217.8 ppm °C at X, Y, Z directions, respectively. In
consideration of low CTEx and CTEy of PTFE/GFC composites and low CTEz of PTFE/GFM composites,
composite substrates including PTFE and alternate GFC and GFM were prepared, exhibiting relatively low CTE
of 28.64, 30.52, 223.7 ppm °C at X, Y, Z directions, respectively.

Acknowledgments

This work has been supported by the Science and Technology Planning Project of Guangdong Province of China
(No. 2017A010103001).

ORCID iDs

Ying Yuan https://orcid.org/0000-0002-0237-6867

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