Proceedings of the 41st European Microwave Conference

Dielectric Permittivity Measurements of Thin Films

at Microwave and Terahertz Frequencies
Liu Chao, Benjamin Yu, Anjali Sharma, Mohammed N. Afsar
High Frequency Material Measurement and InformationCenter,
Department of Electrical and Computer Engineering, Tufts University, Medford, MA02155-5528

Abstract The measurement of complex dielectric permittivity shift in addition to the amplitude loss. The dielectric properties
of thin films are very difficult at microwave, millimeter and THz of the sample shift and distort the interferogram signature.
frequencies because the phase shift is not large enough to Using a double-sided complex Fourier transform, the phase
evaluate the real part of dielectric permittivity. It is now and modulus spectra of the sample in question are produced.
necessary to determine the dielectric permittivity values of such This data, along with a comparison to the reference
films directly because of the growing use of thin films in interferogram can be used to derive the refractive index and
integrated circuitry. Two different types of instrumentation were the real part of complex dielectric permittivity of the sample
utilized and new techniques were developed so that the dielectric [5]. DFTS provides a broad-band measurement of the
permittivity values can be determined accurately at microwave
permittivity of a sample in frequencies much higher than those
as well as at millimeter wave and terahertz frequencies. The
Agilent 8510C vector network analyzer was employed together
measured in slotted-cavity methods. Thus, successfully
with a specially designed slotted cavity for the X-band microwave applying DFTS methods to low-loss thin film materials is
measurements of thin films. A step size of 500 nano meter for the expedient.
mirror movement was implemented for the dispersive Fourier
transform spectroscopy (DFTS) technique to provide higher
resolution phase reproduction leading to the determination of the
II. MEASUREMENT TECHNIQUE
real part of dielectric permittivity values for thin films as a A. Slotted cavity technique
continuous function of frequency from about 60 GHz to 1,000
GHz. Data for one mil (25 m) thin Teflon, Mylar and black
polyester are shown.
Index Terms slotted waveguide cavity technique, dispersive
Fourier transform spectroscopy(DFTS), nano step size, thin
films, complex permittivity

I. INTRODUCTION
Thin film materials are already used in a variety of
microwave and higher frequency applications such as radomes
and some integrated circuitry. The determination of the
dielectric properties of these films is thus of significant
importance. Although there are various well documented
methods for determining the dielectric properties of low-loss
ultra-thin films, such as using thin material slab technique,
closed and open cavity resonators[1-4], finding methods that
are applicable and sensitive enough for use on ultra-thin
materials is a challenge.
The newly developed slotted cavity technique described in this
paper can measure very thin materials around 1 mil (25.4 m)
thickness over a finite range of frequencies. A slotted cavity
measurement scheme is shown here which employs a
transverse slot in the narrow wall through which the sample
can be inserted and removed. This method is much simpler
and the sample occupies the entire cross section of the cavity.
The transverse slot is more sensitive than longitudinal slot
because the sample is parallel to the wavefront which can
provide a reduced transmission and higher reflection.
Fourier spectroscopy has proven to be a viable method for
broadband measurement of materials. In depressive Fourier
transform spectroscopy (DFTS), the interferogram of a sample
is measured and compared to a reference. It introduces a phase
Fig. 1 Setup for transverse slotted cavity measurement for the measurement at
X band. The cavity has a slot in transverse configuration.
The Agilent 8510C vector network analyser is used to make
the slotted cavity measurement. Fig. 1 shows the special
slotted cavity setup. The thin films can be placed inside the
waveguide. TRL calibration was used in order to minimize the
systematic errors in the measurement process. The advantage
of a transverse slotted cavity for X band connected at the other
port to measure the thin films was also utilized here. The
transverse slotted waveguide method is a novel technique and
a number of known samples such as Teflon, Mylar and black
polyesterare measured for validation of this new technique.
The resonance frequency of the TEM101 mode in the
sample-loaded cavity was measured using the Vector Network
Analyzer and this was used to calculate the real part of the
specimen permittivity using the following equation:

978-2-87487-022-4 2011 EuMA 202 10 -13 October 2011, Manchester, UK

 d f0 f
= 1+
t f 0
where, d is the thickness of slotted waveguide, t is the
thickness of thin film sample, f0 is the resonant frequency
without sample, f if the resonant frequency when sample is
inserted.
B. Dispersive Fourier transform spectroscopy
In a dispersive Fourier transform Spectroscopy (DFTS), the
specimen rests in one the mirror arm of a two beam
interferometer to provide the phase information in addition to
the amplitude information. This leads to the determination of
both the real and imaginary parts of complex dielectric
permittivity as a continuous function of frequency. The
polarization configuration of the two beam Fourier transform
interferometer gives a pass band energy spectrum from 30
GHz to 6 THz thus enhancing lower frequency performance of
the interferometric system. It is necessary to employ an ultra
sensitive liquid helium cooled indium antimonide detector at
millimetre wave frequencies. The millimetre wave free carrier
absorption of the semiconductor material becomes an ultra
sensitive broadband detector from about 30 GHz to 1000 GHz.
A mercury lamp provides the signal radiation which is
directed within the interferometer by collimating
mirrors[6][7].
Fig. 2.Ray diagram of the dispersive Fourier transform interferometer. The
beam division is accomplished by using a pair of free standing wire grid
polarizers. One grid acts as a polarizer/analyzer and other grid as a beam
divider and beam recombiner. Note that the specimen rests in one of the
active mirror arm of the interferometer to provide the phase information in
addition to the amplitude information.
Figure 2 shows a line diagram of the dispersive Fourier
transform spectrometer. It consists of a water cooled quartz
encapsulated medium pressure 125 Watts mercury vapor lamp
that acts as the source of radiation. The mainframe of the setup
consists of two cubes, a focusing lens, beam splitters, a two
mirror modulator, stepping motor, phase modulator, a long
compensating arm with a moving mirror and micrometer setup,
and the sample holder. The radiation emitted from the source
and travelling through the arms of the interferometer can be
collimated by either a lens or an off-axis parabolic mirror.
Lens systems are not very practical in the submillimeter
region because problems arise from placing transparent lenses
close to an extremely hot source. Also, most materials used for
lenses have absorption bands. The two mirror collimator
203
consists of one concave and one plane mirror. The concave
mirror intercepts the beam from the source, collimates it, and
directs it towards the plane mirror which then directs the beam
towards the central cube. The mirrors can both be tilted from
outside the evacuated interferometer by using three screws in
order to align the mirrors optically. Different modulation
frequencies provide different signal to noise ratios. When
using different detectors, several modulation frequencies are
required in order to achieve the most favorable signal to noise
ratio. For the thin film measurement, a 500 nano-meter step
size of the scanning mirror movement is achieved for the first
time. It thus provided us with highly resolved phase
information. This high resolution phase information lead us to
determine the real part of complex dielectric permittivity of
one mil (25.4 m) thickness thin films very accurately from 60
GHz to 1000 GHz.
Once the two interference patterns, shift, and sample
thickness are known, multiple reflection signatures can be
edited out, and a double-sided Fourier transform of the
interferograms is performed to yield more stable phase
information in the frequency domain. One can then proceed to
calculate the five optical and dielectric parameters
investigated in this paper namely the absorption coefficient,
the refractive index, the real and imaginary part of complex
dielectric permittivity and the loss tangent. The refractive
index is found by
x ph{S T (v)} ph{S O (v)} ph{(Sl(v))2}
n(v) =1+ +
dS 4 vd
S
where x is the shift, d S is the sample thickness, v is the wave
number per cm, the wave number is related to frequency  via
c, the speed of light, and ph{} indicates the phase of the
 T (v ) and S O (v ) are the
contents within the parentheses. S
Fourier transforms of the edited sample and reference
interference pattern. S (v ) is derived from the ratio of
S T (v ) and S O (v ) . Similarly, the absorption coefficient can
be found by
1 S O (v )
(v ) = [ln + ln( Sl(v ))2 ]
dS S T (v )
From Maxwells Equation and dielectric definitions such as

(v) , one can
 (v ) = {n (v )}2 = (v ) i (v ) and tan =
(v )
calculate the complex permittivity and loss tangent.
III. RESULTS AND DISCUSSION
Teflon, Mylar Polyester and Black Polyester thin films were
chosen to investigate the validity of these newly developed
techniques at the beginning. The thickness of each samples are
approximately about1 mil (25.4 m)and 0.5 mil(12.7
m)respectively. The experiment was conducted with a single
layer of the thin film as well as with multiple layers of the
same sheet of thin film to observe the variation of the real part Number of Resonant Permittivity
of permittivity value with increasing total thickness of the Layers Frequency (GHz)
stacked material. One can place three layers maximum at a 1 8.7988 1.817624
time to even up to ten layers depending upon the base 2 8.7899 1.914149
thickness of the film. The measurement was then extended for 3 8.7814 1.931183
several other thin film materials. Tables below show the 4 8.7736 1.919827
resonant frequency and the real part of permittivity values for 5 8.7659 1.910743
different layer of thin films for Teflon, Black Polyester with Measured resonant frequency without sample= 8.806 GHz.
different film thicknesses, Mylar, Polyphenylene Sulfide, 6. Polyethylene Film (0.003 inch)
Fluoropolymer, Polyethylene with film thicknesses and Acetal Number of Resonant Permittivity
Polyoxymethylene. The resonant frequency decreases with Layers Frequency (GHz)
increasing layers of thin films stacked inside the slotted cavity. 1 8.7751 2.169657
The real part of permittivity value seem to be consistent and 2 8.7429 2.194261
the variation does fall within the random error limit.Data for a 3 8.7106 2.203725
total of eleven different thin film samples measured with the Measured resonant frequency without sample= 8.806 GHz.
new slotted cavity are presented. 7. Polyethylene Film (0.005 inch)
A. Slotted cavity measurement Number of Resonant Permittivity
Layers Frequency (GHz)
1. Teflon (thickness=0.001 inch) 1 8.7521 2.224165
Number of Resonant Permittivity 2 8.6981 2.225301
Layers Frequency (GHz) Measured resonant frequency without sample= 8.806 GHz .
1 8.7965 2.0788 Known permittivity value = 2.26.
2 8.7865 2.1072 8. Acetal Polyoxymethylene Film (0.003 inch)
3 8.7767 2.1091 Number of Resonant Permittivity
4 8.7677 2.087 Layers Frequency (GHz)
5 8.7577 2.097 1 8.7575 2.835869
Measured resonant frequency without sample= 8.806 GHz. 2 8.7019 2.970248
The permittivity of Teflon is known to be close to 2.1. The value obtained 3 8.6585 2.861105
from the measurements is close to 2.1. Measured resonant frequency without sample= 8.806 GHz.
2. Black Polyester (thickness=0.001 inch) 9. Black Polyester (thickness=0.001 inch)
Number of Resonant Permittivity Number of Resonant Permittivity
Layers Frequency (GHz) Layers Frequency (GHz)
1 8.7885 2.9873 1 8.79156 3.028508
2 8.7708 2.9986 Measured resonant frequency without sample= 8.80943GHz.
3 8.753 3.0062 10. Black Polyester (thickness=0.00075 inch)
4 8.735 3.0157 Number of Resonant Permittivity
5 8.7117 3.1417 Layers Frequency (GHz)
Measured resonant frequency without sample= 8.806 GHz. 1 8.7930 3.486729
3. Mylar Polyester Film (thickness=0.001 inch) 2 8.77648 3.49354
Number of Resonant Permittivity 3 8.7600 3.493792
Layers Frequency (GHz) 4 8.7437 3.487108
1 8.7888 2.953214 Measured resonant frequency without sample= 8.80943GHz.
2 8.7721 2.924824 11. Black Polyester (thickness=0.0005 inch)
3 8.7554 2.915361 Number of Resonant Permittivity
4 8.7379 2.933341 Layers Frequency (GHz)
5 8.7212 2.92596 1 8.7976 3.748786
Measured resonant frequency without sample= 8.806 GHz . 2 8.7856 3.736527
Dielectric constant of mylar has been published to be 3.2. 3 8.7737 3.724873
4. Polyphenylene Sulfide (0.003 inch) 4 8.7615 3.736073
Number of Resonant Permittivity 5 8.7498 3.72009
Layers Frequency (GHz) 6 8.7386 3.690517
1 8.7554 2.915361
7 8.7280 3.649934
2 8.7029 2.951321
8 8.7150 3.687603
3 8.6512 2.953214
9 8.7024 3.706812
Measured resonant frequency without sample= 8.806 GHz.
Reference from industrial data sheet: Dielectric constant at 1 GHz is 3.3. 10 8.69129 3.688352
5. Fluoropolymer Film (0.001 inch) Measured resonant frequency without sample= 8.809708 GHz.

204
B. Dispersive Fourier transform spectroscopy layers. A thorough error analysis will be presented at the
conference.
Reference Shifted

5.00E-01

4.00E-01
IV. CONCLUSION
3.00E-01

The direct measurement of complex dielectric permittivity

2.00E-01
of materials is really important because various dielectric
1.00E-01
materials are now in routine use in integrated circuitry. The
Detector Signal

0.00E+00 accurate determination of dielectric permittivity at microwave

-1.00E-01
and at millimeter wave is necessary as feeding parameters in
the design of such circuits. Two new techniques described
-2.00E-01
here allowed us to measure the real part of complex dielectric
-3.00E-01
permittivity of low absorbing thin films for the first time. The
-4.00E-01 transverse slotted cavity technique seems to be extremely
-5.00E-01
sensitive for the frequency (phase) shift for a low absorbing
8 8.5 9 9.5 10
Microns
10.5 11 11.5 12
thin films. With the improved 500 nano-meter stepscanning
Fig. 3. The recorded interferogram for a reference and a Mylar specimen. The
mirror movement in a dispersive Fourier transform
shift which is about 40 micrometers in path difference unit represents the spectrometer, the phase shift is highly resolved. The
phase shift due to the dispersion in the Mylar sample. determination of the real part of complex dielectric
permittivity of low absorbing thin film material is really a
Teflon Mylar Black Polyester

4
straight forward matter. The transverse slotted cavity
technique is a novel technique to measure permittivity of thin
3.8
film samples. Improvements will be made for the data
3.6
evaluation so that the reliable value of spectra for the
3.4 imaginary parts of the permittivity can be presented.
3.2
Real Permittivity

2.8
2.6
2.4
2.2
2 Transactions on , vol.5, no.4, pp.571-577, Aug 1998
300 350 400 450 500
Frequency (GHz)
Fig. 4. The real permittivity spectra of 1 mil thick single layer of Teflon,
Mylar, and Black Polyester thin film specimens.
Figure 3 shows phase modulated interferogram signatures for
an empty reference run and with a single layer of Mylar thin
film sample run. The average shift in path difference unit is
about 40 micrometers
Figure 4 above shows a comparison of real part of dielectric
permittivity spectra for Teflon, Mylar and Black Polyester thin
film samples from about 300 GHz to 800 GHz. For
DFTS,small errors can lead to a large error in calculation of
permittivity. The measurement of thickness should be
accurate, the film should be smooth without folds. It is not that
easy to measure the thickness of the thin film accurately.
However the average value of the real part of dielectric
permittivity spectrapresented in Fig.4 agree very well with
previouslymeasuredpermittivity values of bulk materials.A
better idea of the thickness measurement is to measure the
total thickness of many layers divided by the total number of
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