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Dielectric Permittivity Measurements of Thin Films at Microwave and Terahertz Frequencies

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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:

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

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

203

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

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

-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

2.6 [1] Baker-Jarvis, J.; Geyer, R.G.; Grosvenor, J.H., Jr.; Janezic,

2.4

M.D.; Jones, C.A.; Riddle, B.; Weil, C.M.; Krupka, J.; ,

"Dielectric characterization of low-loss materials a comparison

2.2

of techniques," Dielectrics and Electrical Insulation, IEEE

2 Transactions on , vol.5, no.4, pp.571-577, Aug 1998

300 350 400 450 500 550 600 650 700 750 800

Frequency (GHz)

[2] B. K. Chung, A convenient method for complex permittivity

measurement of thin materials at microwave frequencies, J.

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.

[3] Jin, H.; Dong, S.R.; Wang, D.M., "Measurement of Dielectric

Constant of Thin Film Materials at Microwave Frequencies,"

Figure 3 shows phase modulated interferogram signatures for Journal of Electromagnetic Waves and Applications, Volume

an empty reference run and with a single layer of Mylar thin 23, Numbers 5-6, 2009 , pp. 809-817(9).

film sample run. The average shift in path difference unit is [4] V.A. Vyas, D.H. Gadani, A.N. Prajapati, "Cavity perturbation

about 40 micrometers technique for complex permittivity measurement of dielectric

Figure 4 above shows a comparison of real part of dielectric materials at X-band microwave frequency," Conference on

permittivity spectra for Teflon, Mylar and Black Polyester thin Recent Advances in Microwave Theory and Applications, pp.

film samples from about 300 GHz to 800 GHz. For 836-838 Nov 2008.

[5] M. N. Afsar, "Dielectric Measurements of Millimeter-Wave

DFTS,small errors can lead to a large error in calculation of Materials", IEEE Transactions on Microwave Theory and

permittivity. The measurement of thickness should be Techniques, Vol.MTT-32, No.12, December,1984

accurate, the film should be smooth without folds. It is not that [6] M. N. Afsar, "Precision Millimeter Wave Dielectrics

easy to measure the thickness of the thin film accurately. Measurements of Birefringent Crystalline Sapphire and Ceramic

However the average value of the real part of dielectric Alumina", IEEE Transactions on Instrumentation and

permittivity spectrapresented in Fig.4 agree very well with Measurements, Vol.Im-36, No.2, June 1987

previouslymeasuredpermittivity values of bulk materials.A [7] M. N. Afsar, "Precision Millimeter Wave Measurements of

better idea of the thickness measurement is to measure the Complex Refractive Index, Complex Dielectric Permittivity and

total thickness of many layers divided by the total number of Loss tangent of Common Polymers", IEEE Transactions on

Instrumentation & Measurements, Vol.IM-36, No.2, June 1987

205

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