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

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


d f0 f consists of one concave and one plane mirror. The concave
= 1+
t f 0 mirror intercepts the beam from the source, collimates it, and
where, d is the thickness of slotted waveguide, t is the directs it towards the plane mirror which then directs the beam
thickness of thin film sample, f0 is the resonant frequency towards the central cube. The mirrors can both be tilted from
without sample, f if the resonant frequency when sample is outside the evacuated interferometer by using three screws in
inserted. order to align the mirrors optically. Different modulation
frequencies provide different signal to noise ratios. When
B. Dispersive Fourier transform spectroscopy using different detectors, several modulation frequencies are
required in order to achieve the most favorable signal to noise
In a dispersive Fourier transform Spectroscopy (DFTS), the
ratio. For the thin film measurement, a 500 nano-meter step
specimen rests in one the mirror arm of a two beam
size of the scanning mirror movement is achieved for the first
interferometer to provide the phase information in addition to time. It thus provided us with highly resolved phase
the amplitude information. This leads to the determination of information. This high resolution phase information lead us to
both the real and imaginary parts of complex dielectric determine the real part of complex dielectric permittivity of
permittivity as a continuous function of frequency. The one mil (25.4 m) thickness thin films very accurately from 60
polarization configuration of the two beam Fourier transform GHz to 1000 GHz.
interferometer gives a pass band energy spectrum from 30 Once the two interference patterns, shift, and sample
GHz to 6 THz thus enhancing lower frequency performance of thickness are known, multiple reflection signatures can be
the interferometric system. It is necessary to employ an ultra edited out, and a double-sided Fourier transform of the
sensitive liquid helium cooled indium antimonide detector at interferograms is performed to yield more stable phase
millimetre wave frequencies. The millimetre wave free carrier information in the frequency domain. One can then proceed to
absorption of the semiconductor material becomes an ultra calculate the five optical and dielectric parameters
sensitive broadband detector from about 30 GHz to 1000 GHz. investigated in this paper namely the absorption coefficient,
A mercury lamp provides the signal radiation which is the refractive index, the real and imaginary part of complex
directed within the interferometer by collimating dielectric permittivity and the loss tangent. The refractive
mirrors[6][7]. 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
Fig. 2.Ray diagram of the dispersive Fourier transform interferometer. The be found by
beam division is accomplished by using a pair of free standing wire grid
1 S O (v )
polarizers. One grid acts as a polarizer/analyzer and other grid as a beam
(v ) = [ln + ln( Sl(v ))2 ]
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
dS S T (v )
addition to the amplitude information. From Maxwells Equation and dielectric definitions such as
Figure 2 shows a line diagram of the dispersive Fourier 
(v) , one can
transform spectrometer. It consists of a water cooled quartz  (v ) = {n (v )}2 = (v ) i (v ) and tan =
encapsulated medium pressure 125 Watts mercury vapor lamp (v )
that acts as the source of radiation. The mainframe of the setup calculate the complex permittivity and loss tangent.
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, III. RESULTS AND DISCUSSION
and the sample holder. The radiation emitted from the source Teflon, Mylar Polyester and Black Polyester thin films were
and travelling through the arms of the interferometer can be chosen to investigate the validity of these newly developed
collimated by either a lens or an off-axis parabolic mirror. techniques at the beginning. The thickness of each samples are
Lens systems are not very practical in the submillimeter approximately about1 mil (25.4 m)and 0.5 mil(12.7
region because problems arise from placing transparent lenses m)respectively. The experiment was conducted with a single
close to an extremely hot source. Also, most materials used for layer of the thin film as well as with multiple layers of the
lenses have absorption bands. The two mirror collimator

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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.

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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 REFERENCES
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Frequency (GHz)
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Fig. 4. The real permittivity spectra of 1 mil thick single layer of Teflon,
Phys. D: Appl. Phys., vol. 39, pp. 19261931, 2006.
Mylar, and Black Polyester thin film specimens.
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