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Electrical Characterization
of Non-Conducting
Materials Using Reflection
Based Microwave
Technique
B Y
PALL AVI M AL AM E ( TP2 F1 2130 01)
GU ID E
D R . R AJ IV GU PTA
Submitted in partial fulfilment of the
requirements
of the degree of
Master of Engineering
by
Pallavi R. Malame
TP2F1213001
Supervisor:
Dr. RAJIV K. GUPTA
27-02-2015 TERNA COLLEGE : ME THESIS 2
ACKNOWLEDGEMENT
Dr. R. K. Gupta, HOD , EXTC Department,
Dr. Deven Shah, Principal.
Mr. Rajesh Harsh (Scientist F), HOD, Technology Innovation
Dept.(TID), SAMEER
Mr. Anil Kulkarni (Scientist F) ,HOD, Industrial Meteorological and
System Dept. (IMSD), SAMEER
Mr. Tapas K. Bhuiya (Scientist D), IMSD , SAMEER
27-02-2015 TERNA COLLEGE : ME THESIS 3
Introduction
Microwave Reflectometry
Features of FDR
Motivation
Problem Statement
Objectives
27-02-2015 TERNA COLLEGE : ME THESIS 4
Motivation
Society for Applied Microwave Electronics
Engineering & Research
Department of Electronics and
Information Technology
Under the aegis
of
Core Project : Moisture
Measurement System
Brix Measurement for
Sugar Industry
}
My Role
Problem Statement
• Need for accurate, rapid measurement system
which can be used for in-situ, online
measurements
• a research study is needed in the field of dielectric
spectroscopy
• Exploration of Reflection based method
• Exploration of Transmission/Reflection based
method
• Analysis of permittivity of wide variety of materials
(liquid-semi solids-solids) using Microwaves
27-02-2015 TERNA COLLEGE : ME THESIS 5
Objectives
To electrically characterize variety of liquids like oils, sugar solution,
honey and milk using open ended coaxial cable technique (simulation as
well as experimentally) which is a reflection based microwave method.
To electrically characterize variety of solids like substrates and wood
using waveguide fixture method (simulation as well as experimentally)
which is based on Transmission/Reflection based method.
To explore other dielectric spectroscopy techniques
How did I achieve this
??
27-02-2015 TERNA COLLEGE : ME THESIS 6
Microwave Reflectometry
Time domain
reflectometry - TDR
Frequency domain
reflectometry - FDR
• Less expensive • More accurate
• Advantage of
Calibration
FDR Features:
• gives high accuracy
• for homogeneous materials
• fast replacing laborious and time-
consuming physical and chemical
laboratory analytical methods
• applicable to materials and products of
agricultural origin
• non-destructive and rapid
measurements
• applications using automation
• Ideal for in-situ/in vivo online
measurement systems
• influence of electrical conductivity is
negligible
• penetration depth is much greater
• continuous remote monitoring
• insensitive to environmental factors
• enabling detection of even small
amounts of water
• Do not pollute the tested material
27-02-2015 TERNA COLLEGE : ME THESIS 7
Electrical Characterization of Non-
Conducting Materials Using Reflection
Based Microwave
Technique
Electrical Characterization Non-Conducting Materials Reflection Based Microwave Technique
Figures Just for Illustration Purpose
Non Magnetic
materials Products
Measuring Electrical
Parameter only:
Dielectric
S11
Reflection
S21
Transmission
Er’
Dielectric
Constant
Er’’
Loss Factor
C Band ( 5.81 GHz)
Why 5.81??
27-02-2015 TERNA COLLEGE : ME THESIS 8
Literature survey
• Polar dielectrics and modelling studies date back more than 70 years reported by
Debye in 1929.
• In the last 10-15 years, the concept of permittivity measurement has been extended
and applied to various agricultural, food, and biological problems
• 1945 - carrots at frequencies in the range of 18 kHz to 5 MHz by Dunlap and Makower.
• 1949 - potato, carrot, apple, and peach tissue from 1 to 40 MHz by Shaw and Galvin
• 1984 - tabulated the dielectric properties of selected vegetables and fruits at a
frequency range 0.1 to 10 GHz by tran et al.
• 1980 - moisture content on the dielectric properties of granular solids at 9.4 GHz over
a wide range of temperature and moisture contents by M.A. Stuchly, and S.S. Stuchly
• Several techniques to measure the dielectric properties of agri-food materials are
described in 1) Handbook of Microwave Measurements by M. Sucher and J. Fox
2) Industrial Microwave Heating by A.C. Metaxas and R. Meredith
• 1980 -The dielectric properties of food materials in the microwave region can be
determined by several methods using different microwave measuring sensors [22-23]
Microwave aquametry by A.W. Kraszewski.
• 1989 - Nyfors and Vainikainen [24] has reported four groups of measurement
methods, namely, lumped circuit, resonator, transmission line, and free-space
methods.
27-02-2015 TERNA COLLEGE : ME THESIS 9
Open ended Coaxial Method
• 1980 - Open ended coaxial probe method has been reported by Stuchly and Stuchly
• 1989 - For liquid and semi-solid materials, including biological and food materials, open-
ended coaxial-line probes have been used for broadband permittivity measurements.
Grant et al and Blackham et al.
• For liquid and semi-solid materials, including biological and food materials, open-ended
coaxial-line probes have been used for broadband permittivity measurements [25-26].
• A similar technique is used for permittivity measurements on fresh fruits and vegetables
by Nelson.
Oils
• 2008 -Dielectric properties of vegetable oils and fatty acids in low frequencies (0.1-1
MHz) are studied by Lizhi et al.
• 2010 - On the basis of this research it is possible to detect whether olive oil has been
adulterated with cheaper vegetable oil [29].
• 2010 - Latest studies based on TDR have been reported by Piuzzi et al [30]
Milk
Use of open ended coaxial probe technique for dielectric property measurement of
milk is mentioned in Advanced Dairy Chemistry by McSweeney
27-02-2015 TERNA COLLEGE : ME THESIS 10
• 1974 - Mudgett et.al.[32] has observed dielectric properties of skim milk over the
temperature range 25-55oC.
• 2006 - Nunes et al. [33] has examined the complex dielectric permittivity of UHT milk in a
frequency range 1-20 GHz.
• 1992 & 2010 - Latest studies are reported by Kudra et al [34] and W Guo et al [35].
Honey
• 2010 - Study of honey using open ended coaxial cable has been reported by W Guo et al.
Dielectric spectroscopy is used for determining difference between different honey and
sucrose and water content of honey [36-37].
Waveguide Fixture
• Microwave measurement systems to determine the dielectric properties of grain, Early
efforts to characterize the dielectric properties of materials using transmission/reflection
based method which are open resonant structures are fabricated at the Massachusetts
Institute of Technology [11, 38].
• 1973,1983,1984 - Coaxial-line and rectangular wave-guide sample holders are used with
various mid, and fruit and vegetable tissue samples at frequencies from 1 to 22 GHz [8,39-
41].
• 1983 -The sample holders are also used to measure dielectric properties of pulverized coal
and mineral samples [40].
• 1970 - Dielectric properties of grain samples are measured using a precision bridge over
audio frequencies from 250 Hz to 20 kHz with sample holders confined in a coaxial sample
holder and reported in [42].
27-02-2015 TERNA COLLEGE : ME THESIS 11
Permittivity and Dielectric
Mechanism
"'
0
rrr
j


 
'
"
tan
r
r


  r
'
r
''
r
Complex
Relative
Permittivity
Dielectric
Constant
Loss
Factor
Loss
Tangent
Complex Permittivity: Permittivity describes
the interaction of a material with an electric
field.
Dielectric Constant :It is a measure of how
much energy from an external field is stored
in a material.
Loss Factor: It is a measure of how dissipative
or lossy a material is to an external field.
Loss Tangent: The loss tangent or tan δ is
defined as the ratio of the imaginary part of
the dielectric constant to the real part.
27-02-2015 TERNA COLLEGE : ME THESIS 12
Dielectric Theory
"'
rrr j "'
rrr j 
Electric Magnetic
Permittivity Permeability
FieldsFields
STORAGE
LOSS
MUT
STORAGE
LOSS
Non Magnetic Material!
1
27-02-2015 TERNA COLLEGE : ME THESIS 13
Interaction of Medium with
EM Waves
27-02-2015 TERNA COLLEGE : ME THESIS 14
Dielectric Mechanism
Random Motion of
water molecules
Orientation in Electromagnetic Field
27-02-2015 TERNA COLLEGE : ME THESIS 15
Frequency response of
Dielectric Mechanisms
Microwave
frequency
region
} Microwave
frequency
Loses are
introduced at
low frequency
Parameters contributing to
permittivity
Conduction: ionic
Dipolar relaxation
Atomic polarization
Electronic polarization
27-02-2015 TERNA COLLEGE : ME THESIS 16
Return
Relaxation time
1
1
10
100
10 100
Water at 20o C
f,
GHz
most energy is lost at 1/t
'
r
"
r
Cole Cole Plot
27-02-2015 TERNA COLLEGE : ME THESIS 17
Measurement Techniques
Parallel Plate Low Frequency
Best for thin flat sheets
Coaxial Probe Broadband
Best for liquids, semi-solids
Transmission Line Broadband
Best for machine-able solids
Transmission Free
Space
Broadband, mm-wave
Non-contacting
Resonant Cavity Single frequency
High accuracy, Best for low
loss, or very thin samples
27-02-2015 TERNA COLLEGE : ME THESIS 18
Vector Network Analyzer
N5221A PNA.
27-02-2015 TERNA COLLEGE : ME THESIS 19
Image Courtesy : Agilent Technologies
Reflection based Electrical
Characterization of Non-
Conducting Materials.
Sensor Probe, waveguide, patch
antenna
Measured parameter S11 reflection coefficient
Features:
Best for lossy MUTs, liquids or semi-solids.
 Broadband.
 Convenient and non-destructive.
 Require no machining of the sample, easy sample
preparation, after
calibration, the dielectric properties of a large number of
samples can be
routinely measured in a short time.
 Measurement can be performed in a temperature controlled
environment.
27-02-2015 TERNA COLLEGE : ME THESIS 20
Transmission/Reflection based
Electrical Characterization of
Non-Conducting Materials.
Sensor waveguide
Measured parameter S11 and S21
Features:
• Accuracy
• Best for solid materials.
27-02-2015 TERNA COLLEGE : ME THESIS 21
Open Ended Coaxial
Probe Technique
Sample thickness
d
27-02-2015 TERNA COLLEGE : ME THESIS 22
27-02-2015 TERNA COLLEGE : ME THESIS 23
Practical View
Calibration and Measurement
Technique
• Agilent Technologies N5221A PNA network
analyser
• Agilent Technologies 85070E open ended coaxial-
line probe
• 85070E software
• reflection coefficient was measured
• PNA Port OSL calibration
• Probe Calibration open, short and deionised
water
• Temperature maintained at 250C
• Ecal Module
27-02-2015 TERNA COLLEGE : ME THESIS 24
Oils
Result And Discussion
Sample oils:
50 ml coconut oil
50ml groundnut oil
50ml sunflower
27-02-2015 TERNA COLLEGE : ME THESIS 25
ε’
Low Frequency
ε"
27-02-2015 TERNA COLLEGE : ME THESIS 26
Brix
Result And Discussion
Sample: 100g Water and
Sugar Solution
27-02-2015 TERNA COLLEGE : ME THESIS 27
Sugar content ε’ ε"σ : conductivity
27-02-2015 TERNA COLLEGE : ME THESIS 28
Milk
Result And Discussion
27-02-2015 TERNA COLLEGE : ME THESIS 29
Milk Adulteration Detection
Sample: Fresh untreated cow’s milk
temperature is maintained at 250C
adulterants used are:
water at room temperature, sugar, wheat flour
as starch and sodium bi carbonate
27-02-2015 TERNA COLLEGE : ME THESIS 30
Image Courtesy: Times of India (6/3/14)
ε’’
ε’
Water
Water
ε’’
Water
27-02-2015 TERNA COLLEGE : ME THESIS 31
Dielectric Response
Sugar
ε’
27-02-2015 TERNA COLLEGE : ME THESIS 32
ε’
ε’’
27-02-2015 TERNA COLLEGE : ME THESIS 33
Honey
Result And Discussion
A sample of honey from
an apiary belonging to
apis indica species of
honeybee
Adulterants:
distilled water and
corn syrup.
27-02-2015 TERNA COLLEGE : ME THESIS 34
ε’
Water
ε’’
Water
27-02-2015 TERNA COLLEGE : ME THESIS 35
ε’
cornsyrup
ε’’
cornsyrup
27-02-2015 TERNA COLLEGE : ME THESIS 36
Rectangular Waveguide as
Fixture: Simulation in HFSS
27-02-2015 TERNA COLLEGE : ME THESIS 37
27-02-2015 TERNA COLLEGE : ME THESIS 38
S11 vs Frequency
S11= -19.927 at 5.81GHz
Permittivity 1
27-02-2015 TERNA COLLEGE : ME THESIS 39Video
Permittivity 10
27-02-2015 TERNA COLLEGE : ME THESIS 40Video
SIMULATION RESULTS
27-02-2015 TERNA COLLEGE : ME THESIS 41
Experimental Setup
27-02-2015 TERNA COLLEGE : ME THESIS 42
Coax to Waveguide
Adaptor
27-02-2015 TERNA COLLEGE : ME THESIS 43
SAMPLE HOLDER AND
SAMPLE
27-02-2015 TERNA COLLEGE : ME THESIS 44
85071E Software
27-02-2015 TERNA COLLEGE : ME THESIS 45
Waveguide Fixture S11 S21
Coax to waveguide adapter 1 -21.79dB -
Coax to waveguide adapter 2 -25.85dB -
Combined waveguide -24.85dB -0.94dB
Material
Teflon 2.1 2.53
UHM 2.4 2.66
Wood 1.2-5 5.43
Wet-Wood - 12.58
27-02-2015 TERNA COLLEGE : ME THESIS 46
Frequency 5.71GHz
0.2
0.1
27-02-2015 TERNA COLLEGE : ME THESIS 47
Conclusion
The experimental results on oil and brix content are close to the values
specified in Literature and Theory
Open ended coaxial technique can be utilised for oil adulteration
detection-More experimentation with TDR required
The Technique can satisfactorily used in Sugar Industries for measurement
of brix due to wide variation in S11 data
Milk and Honey adulteration detection methods are proved reliable and
accurate
Transmission/Reflection based method using software 85071E gives a very
accurate
Result compared to reflection based method. The fabricated waveguide
design proves very useful in wood, paper and pulp industries for wood
moisture measurement for instant results
27-02-2015 TERNA COLLEGE : ME THESIS 48
Scope for Future Work
Dielectric spectroscopy of oil
Investigations for fat content measurement
Cheese Industry
Instead of Rectangular waveguide a circular waveguide can be used.
More materials like metamaterials can be studied for their dielectric
and magnetic property
Different sensors including Patch antennas ,horn antennas etc. can be
explored.
27-02-2015 TERNA COLLEGE : ME THESIS 49
27-02-2015 TERNA COLLEGE : ME THESIS 50
References
[1] W. Skierucha; A. Wilczek, and A. Szyplowska, “Dielectric spectroscopy in agro
physics”, Int. Agrophys., pp. 187-197, 2012.
[2] T.W. Athey, M.A. Stuchly and S.S. Stuchly, “Measurement of radio-frequency
permittivity of biological tissues with an open-ended coaxial line - Part I”, IEEE
Transactions on Microwave Theory and Techniques, vol. 30 ,no.1, pp.82-86. 1982.
[3] D. Bérubé, F.M. Ghannouchi, and P. Savard, “A comparative study of four open-ended
coaxial probe models for permittivity measurements of lossy dielectric biological
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Techniques, vol. 44, no.10, pp. 1928-1934, 1996.
[4] M.M. Brady, S.A. Symons, and S.S. Stuchly, “Dielectric behaviour of selected animal
tissues in vitro at frequencies from 2 to 4 GHz”, IEEE Transactions on Biomedical
Engineering, vol. 28, no.3, pp.305-307, 1981.
[5] R. ZAJÍČEK, L. OPPL, J. VRBA, “Broadband Measurement of Complex Permittivity
Using Reflection Method and Coaxial Probes”,Technická 2, Prague.
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Vincent P. and Nowack, Robert L., “Improvements of Soil Dielectric Mixing Model for
Inversion Analysis of Time Domain Reflectometry Measurements", Proc. TDR 2006,
Purdue University, West Lafayette, USA, vol 4, pp.19 , Sept. 2006.
. New York, NY: The Chemical Catalog Company. 1929.
27-02-2015 TERNA COLLEGE : ME THESIS 51
[7] Scott B. Jones, Jon M. Wraith and Dani or, “Time domain reflectometry measurement
principles and applications” Hydrol. Process., Vol 16, pp.141–153, 2002.
[8] S.O. Nelson, “Dielectric properties of agricultural products - Measurements and
applications”, IEEE Transactions of Electrical Insulation, vol. 26, no.5, pp.845-869.
1991.
[9] J. W. Choi, J. Cho, Y. Lee, J. Yim, B. Kang, K. Oh, et al., “Microwave detection of
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[10] P. Debye, Polar Molecules. New York, NY: The Chemical Catalog Company. 1929.
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[12] S.O. Nelson, “Dielectric properties measuring techniques and applications”, ASAE
,No. 983067. St. Joseph, MI: ASAE. 1998.
[13] W.C. Dunlap,and B. Makower, “Radio frequency dielectric properties of dehydrated
carrots”, Journal of Physical Chemistry , vol. 49: pp. 601-622, 1945.
[14] T.M. Shaw, and J. A. Galvin, “High frequency heating characteristics of vegetable
tissues determining from electrical conductivity measurements”, In Proceedings
Institution of Radio Engineering, Institute of Radio Engineering and Electronics
Publication, Chaberska, Prague: IREE, vol. 37, pp. 83-86. 1949.
[15] W.E. Pace, W.B. Westphal and S.A. Goldblith. “Dielectric properties of commercial
cooking oils”, Journal of Food Science, vol. 33, pp. 30-36, 1968.
[16] V.N. Tran, S.S. Stuchly and A.W., “Kraszewski. Dielectric properties of selected
vegetables and fruits at 0.1 - 10 GHz”, Journal of Microwave Power, vol. 19, no.4, pp.
27-02-2015 TERNA COLLEGE : ME THESIS 52
[17] M.A. Stuchly, and S.S. Stuchly, “Dielectric properties of biological substances –
Tabulated”, Journal of Microwave Power, vol. 15, pp.19-26,1980.
[18] M. Sucher and J. Fox, Handbook of Microwave Measurements. New York, NY:
Polytechnic Press Institute. 1963.
[19] G.P. de Loor, and F.W. Meijboom, “The dielectric constant of foods and other
materials with high water contents at microwave frequencies”, Journal of Food
Technology, vol. 1, pp.313-322, 1966.
[20] N.E. Bengtsson, and P.O. Risman, “Dielectric properties of food at 3 GHz as
determined by a cavity perturbation technique. II. Measurements on food materials”,
Journal of Microwave Power, vol. 6 , no.2, pp. 107-123, 1971.
[21] A.C. Metaxas and R. Meredith. Industrial Microwave Heating (IEEE Power
Engineering Series). Piscataway, NJ:Peter Peregrinus. 1983.
[22] A.W. Kraszewski, “Microwave aquametry - A review”, Journal of Microwave Power,
vol. 15, no.4, pp. 209-220, 1980.
[23] A. Kraszewski, Microwave Aquametry – Electromagnetic Interaction with Water
Containing Materials, Piscataway, NJ: IEEE Press. 1996.
[24] E. Nyfors, and P. Vainikainen, Industrial Microwave Sensors, chapter 2. Boston, MA:
Artech House, Norwood. 1989.
[25] J.P. Grant, , R.N. Clarke, G.T. Symm and N.M. Spyrou, “A critical study of the openended
coaxial line sensor technique for RF and microwave complex permittivity measurements”,
Journal of Physics: Electronics and Scientific Instrument, vol. 22, pp.
757-770, 1989.
27-02-2015 TERNA COLLEGE : ME THESIS 53
[26] D.V. Blackham, and R.D. Pollard, “An improved technique for permittivity
measurements using a coaxial probe”, IEEE Transactions of Instrumentation and
Measurement , vol. 46 , no. 5, pp.1093-1099. 1997.
[27] S.O. Nelson, “Measurement of microwave dielectric properties of particulate
materials”, Journal of Food, 1994.
[28] H. Lizhi, K. Toyoda, and I. Ihara, “Dielectric properties of edible oils and fatty acids
as a function of frequency, temperature, moisture and composition,” J. Food Eng., vol.
88, pp. 151–158, 2008.
[29] H. Lizhi, K. Toyoda, and I. Ihara, “Discrimination of olive oil adulterated with
vegetable oils using dielectric spectroscopy,” Journal of Food Engineering, vol. 96, pp.
167-171, 2010.
[30] A. Cataldo, E. Piuzzi, G. Cannazza, E. De Benedetto, and L. Tarricone, “Quality and
anti-adulteration control of vegetable oils through microwave dielectric spectroscopy,”
Measurement, vol. 43, no. 8, pp. 1031-1039, 2010.
[31] Paul L. H. McSweeney, Patrick F. Fox ,Advanced Dairy Chemistry: Volume 3:
Lactose, Water, Salts and Minor Constituents
[32] R.E. Mudgett , S.A. Goldblith, D.I.C. Wang and W.B. Westphal, “Dielectric
behaviour of semi-solid food at low, intermediate and high moisture contents”, Journal
of Microwave Power, vol .15, no.1, pp. 27-36. 1980.
[33] A C Nunes, X Bohigas, J Tejada, “Dielectric study of milk for frequencies between 1
and 20 GHz”, Journal of Food Engineering ,vol.76, no. 2, pp. 250–255, 2006.
[34] T Kudra, G S V Raghavan, C Akyel, R Bosisio, F R Voort, “Electromagnetic
properties of milk and its constituents at 2.45 MHz”, Journal of Microwave Power and
Electromagnetic Energy, vol. 27 , no.4 , pp. 199–204,1992.
27-02-2015 TERNA COLLEGE : ME THESIS 54
[35] W Guo, X Zhu, H Liu, R Yue, S Wang, “Effects of milk concentration and freshness on
microwave dielectric properties”, Journal of Food Engineering, vol. 99, pp. 344-350,
2010.
[36] W Guo, X Zhu, Y Liu, H Zhuang ,Sugar and water contents of honey with dielectric property
sensing, Elsevier: Journal of Food Engineering, vol. 97, no. 2, pp. 275–281 , March 2010.
[37] W Guo, Y Liu, X Zhu, S Wang, “Dielectric properties of honey adulterated with
sucrose syrup”, Elsevier: Journal of Food Engineering, Vol. 107, no.1, pp. 1-7, 2011.
[38] S. Roberts, and A. von Hippel, “A new method for measuring dielectric constant and
loss in the range of centimetre waves”, Journal of Applied Physics, vol. 17, pp.610-616,
1946.
[39] S.O. Nelson, “Electrical properties of agricultural products - A critical review”,
Transactions of the ASAE , vol.16, no. 2, pp. 384- 400, 1973.
[40] S.O. Nelson, “Density dependence of the dielectric properties of particulate materials
pulverized coal, flour, wheat samples”, Transactions of the ASAE , vol.26, no.6 ,
pp.1823-1825, 1983.
[41] S.O. Nelson, “Moisture, frequency, and density dependence of the dielectric constant
of shelled, yellow-dent field corn”, Transactions of the ASAE , vol. 30, no. 5, pp. 1573-
1578, 1984.
[42] P.T. Corcoran, S.O. Nelson, L.E. Stetson and C.W. Schlaphoff, “Determining
dielectric properties of grain and seed in the audio frequency range”, Transactions of the
ASAE , vol.13, no.3 , pp.348-351, 1970.
[43] Agilent, 2006. Basics of measuring the dielectric properties of materials. Application
Note:32, USA.
27-02-2015 TERNA COLLEGE : ME THESIS 55
[44] D.M. Slaten,; B.N. Scott,; Gordon, B. Lloyd, “ Techniques and applications of
permittivity measurements”, Electrical Insulation and Dielectric Phenomena, IEEE
1996 Annual Report of the Conference, Vol. 1 , pp. 94 – 97, 1996.
[45] L.F. Chen, C.K. Ong, C.P. Neo, V.V. Varadan, and V.K. Varadan, “Microwave
Electronics Measurement and Materials Characterization”, John Wiley & Sons Ltd,
England, pp. 119-123, 2004.
[46] L. OPPL, Measurement of Dielectric Properties. Dissertation Thesis, CTU in Prague,
Dept. of EM field, 2001. (in Czech)
[47] F. Harding, (Ed.) (1995), Chapter 5: Adulteration of milk. Chapter 6: Compositional
quality. In: Milk Quality. Blackie Academic & Professional, London.
[48] Laleh Mehryar, Mohsen Esmaiili, Honey & Honey Adulteration Detection: A Review,
In proceeding of: 11th International Congress on Engineering and Food (iCEF11)
,Athens, Greece, Vol. 3, 2011
[49] G.F. Miner, Lines and Electromagnetic Fields for Engineers, Oxford University Press,
pp.741, 1996.
61
[50] Agilent 85071E, Materials Measurement Software : Technical Overview Published in
USA, June 14, 2012
Thank You
27-02-2015 TERNA COLLEGE : ME THESIS 56

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Electrical characterization of non conducting materials using reflection based

  • 1. Electrical Characterization of Non-Conducting Materials Using Reflection Based Microwave Technique B Y PALL AVI M AL AM E ( TP2 F1 2130 01) GU ID E D R . R AJ IV GU PTA
  • 2. Submitted in partial fulfilment of the requirements of the degree of Master of Engineering by Pallavi R. Malame TP2F1213001 Supervisor: Dr. RAJIV K. GUPTA 27-02-2015 TERNA COLLEGE : ME THESIS 2
  • 3. ACKNOWLEDGEMENT Dr. R. K. Gupta, HOD , EXTC Department, Dr. Deven Shah, Principal. Mr. Rajesh Harsh (Scientist F), HOD, Technology Innovation Dept.(TID), SAMEER Mr. Anil Kulkarni (Scientist F) ,HOD, Industrial Meteorological and System Dept. (IMSD), SAMEER Mr. Tapas K. Bhuiya (Scientist D), IMSD , SAMEER 27-02-2015 TERNA COLLEGE : ME THESIS 3
  • 4. Introduction Microwave Reflectometry Features of FDR Motivation Problem Statement Objectives 27-02-2015 TERNA COLLEGE : ME THESIS 4
  • 5. Motivation Society for Applied Microwave Electronics Engineering & Research Department of Electronics and Information Technology Under the aegis of Core Project : Moisture Measurement System Brix Measurement for Sugar Industry } My Role Problem Statement • Need for accurate, rapid measurement system which can be used for in-situ, online measurements • a research study is needed in the field of dielectric spectroscopy • Exploration of Reflection based method • Exploration of Transmission/Reflection based method • Analysis of permittivity of wide variety of materials (liquid-semi solids-solids) using Microwaves 27-02-2015 TERNA COLLEGE : ME THESIS 5
  • 6. Objectives To electrically characterize variety of liquids like oils, sugar solution, honey and milk using open ended coaxial cable technique (simulation as well as experimentally) which is a reflection based microwave method. To electrically characterize variety of solids like substrates and wood using waveguide fixture method (simulation as well as experimentally) which is based on Transmission/Reflection based method. To explore other dielectric spectroscopy techniques How did I achieve this ?? 27-02-2015 TERNA COLLEGE : ME THESIS 6
  • 7. Microwave Reflectometry Time domain reflectometry - TDR Frequency domain reflectometry - FDR • Less expensive • More accurate • Advantage of Calibration FDR Features: • gives high accuracy • for homogeneous materials • fast replacing laborious and time- consuming physical and chemical laboratory analytical methods • applicable to materials and products of agricultural origin • non-destructive and rapid measurements • applications using automation • Ideal for in-situ/in vivo online measurement systems • influence of electrical conductivity is negligible • penetration depth is much greater • continuous remote monitoring • insensitive to environmental factors • enabling detection of even small amounts of water • Do not pollute the tested material 27-02-2015 TERNA COLLEGE : ME THESIS 7
  • 8. Electrical Characterization of Non- Conducting Materials Using Reflection Based Microwave Technique Electrical Characterization Non-Conducting Materials Reflection Based Microwave Technique Figures Just for Illustration Purpose Non Magnetic materials Products Measuring Electrical Parameter only: Dielectric S11 Reflection S21 Transmission Er’ Dielectric Constant Er’’ Loss Factor C Band ( 5.81 GHz) Why 5.81?? 27-02-2015 TERNA COLLEGE : ME THESIS 8
  • 9. Literature survey • Polar dielectrics and modelling studies date back more than 70 years reported by Debye in 1929. • In the last 10-15 years, the concept of permittivity measurement has been extended and applied to various agricultural, food, and biological problems • 1945 - carrots at frequencies in the range of 18 kHz to 5 MHz by Dunlap and Makower. • 1949 - potato, carrot, apple, and peach tissue from 1 to 40 MHz by Shaw and Galvin • 1984 - tabulated the dielectric properties of selected vegetables and fruits at a frequency range 0.1 to 10 GHz by tran et al. • 1980 - moisture content on the dielectric properties of granular solids at 9.4 GHz over a wide range of temperature and moisture contents by M.A. Stuchly, and S.S. Stuchly • Several techniques to measure the dielectric properties of agri-food materials are described in 1) Handbook of Microwave Measurements by M. Sucher and J. Fox 2) Industrial Microwave Heating by A.C. Metaxas and R. Meredith • 1980 -The dielectric properties of food materials in the microwave region can be determined by several methods using different microwave measuring sensors [22-23] Microwave aquametry by A.W. Kraszewski. • 1989 - Nyfors and Vainikainen [24] has reported four groups of measurement methods, namely, lumped circuit, resonator, transmission line, and free-space methods. 27-02-2015 TERNA COLLEGE : ME THESIS 9
  • 10. Open ended Coaxial Method • 1980 - Open ended coaxial probe method has been reported by Stuchly and Stuchly • 1989 - For liquid and semi-solid materials, including biological and food materials, open- ended coaxial-line probes have been used for broadband permittivity measurements. Grant et al and Blackham et al. • For liquid and semi-solid materials, including biological and food materials, open-ended coaxial-line probes have been used for broadband permittivity measurements [25-26]. • A similar technique is used for permittivity measurements on fresh fruits and vegetables by Nelson. Oils • 2008 -Dielectric properties of vegetable oils and fatty acids in low frequencies (0.1-1 MHz) are studied by Lizhi et al. • 2010 - On the basis of this research it is possible to detect whether olive oil has been adulterated with cheaper vegetable oil [29]. • 2010 - Latest studies based on TDR have been reported by Piuzzi et al [30] Milk Use of open ended coaxial probe technique for dielectric property measurement of milk is mentioned in Advanced Dairy Chemistry by McSweeney 27-02-2015 TERNA COLLEGE : ME THESIS 10
  • 11. • 1974 - Mudgett et.al.[32] has observed dielectric properties of skim milk over the temperature range 25-55oC. • 2006 - Nunes et al. [33] has examined the complex dielectric permittivity of UHT milk in a frequency range 1-20 GHz. • 1992 & 2010 - Latest studies are reported by Kudra et al [34] and W Guo et al [35]. Honey • 2010 - Study of honey using open ended coaxial cable has been reported by W Guo et al. Dielectric spectroscopy is used for determining difference between different honey and sucrose and water content of honey [36-37]. Waveguide Fixture • Microwave measurement systems to determine the dielectric properties of grain, Early efforts to characterize the dielectric properties of materials using transmission/reflection based method which are open resonant structures are fabricated at the Massachusetts Institute of Technology [11, 38]. • 1973,1983,1984 - Coaxial-line and rectangular wave-guide sample holders are used with various mid, and fruit and vegetable tissue samples at frequencies from 1 to 22 GHz [8,39- 41]. • 1983 -The sample holders are also used to measure dielectric properties of pulverized coal and mineral samples [40]. • 1970 - Dielectric properties of grain samples are measured using a precision bridge over audio frequencies from 250 Hz to 20 kHz with sample holders confined in a coaxial sample holder and reported in [42]. 27-02-2015 TERNA COLLEGE : ME THESIS 11
  • 12. Permittivity and Dielectric Mechanism "' 0 rrr j     ' " tan r r     r ' r '' r Complex Relative Permittivity Dielectric Constant Loss Factor Loss Tangent Complex Permittivity: Permittivity describes the interaction of a material with an electric field. Dielectric Constant :It is a measure of how much energy from an external field is stored in a material. Loss Factor: It is a measure of how dissipative or lossy a material is to an external field. Loss Tangent: The loss tangent or tan δ is defined as the ratio of the imaginary part of the dielectric constant to the real part. 27-02-2015 TERNA COLLEGE : ME THESIS 12
  • 13. Dielectric Theory "' rrr j "' rrr j  Electric Magnetic Permittivity Permeability FieldsFields STORAGE LOSS MUT STORAGE LOSS Non Magnetic Material! 1 27-02-2015 TERNA COLLEGE : ME THESIS 13
  • 14. Interaction of Medium with EM Waves 27-02-2015 TERNA COLLEGE : ME THESIS 14
  • 15. Dielectric Mechanism Random Motion of water molecules Orientation in Electromagnetic Field 27-02-2015 TERNA COLLEGE : ME THESIS 15
  • 16. Frequency response of Dielectric Mechanisms Microwave frequency region } Microwave frequency Loses are introduced at low frequency Parameters contributing to permittivity Conduction: ionic Dipolar relaxation Atomic polarization Electronic polarization 27-02-2015 TERNA COLLEGE : ME THESIS 16 Return
  • 17. Relaxation time 1 1 10 100 10 100 Water at 20o C f, GHz most energy is lost at 1/t ' r " r Cole Cole Plot 27-02-2015 TERNA COLLEGE : ME THESIS 17
  • 18. Measurement Techniques Parallel Plate Low Frequency Best for thin flat sheets Coaxial Probe Broadband Best for liquids, semi-solids Transmission Line Broadband Best for machine-able solids Transmission Free Space Broadband, mm-wave Non-contacting Resonant Cavity Single frequency High accuracy, Best for low loss, or very thin samples 27-02-2015 TERNA COLLEGE : ME THESIS 18
  • 19. Vector Network Analyzer N5221A PNA. 27-02-2015 TERNA COLLEGE : ME THESIS 19 Image Courtesy : Agilent Technologies
  • 20. Reflection based Electrical Characterization of Non- Conducting Materials. Sensor Probe, waveguide, patch antenna Measured parameter S11 reflection coefficient Features: Best for lossy MUTs, liquids or semi-solids.  Broadband.  Convenient and non-destructive.  Require no machining of the sample, easy sample preparation, after calibration, the dielectric properties of a large number of samples can be routinely measured in a short time.  Measurement can be performed in a temperature controlled environment. 27-02-2015 TERNA COLLEGE : ME THESIS 20
  • 21. Transmission/Reflection based Electrical Characterization of Non-Conducting Materials. Sensor waveguide Measured parameter S11 and S21 Features: • Accuracy • Best for solid materials. 27-02-2015 TERNA COLLEGE : ME THESIS 21
  • 22. Open Ended Coaxial Probe Technique Sample thickness d 27-02-2015 TERNA COLLEGE : ME THESIS 22
  • 23. 27-02-2015 TERNA COLLEGE : ME THESIS 23
  • 24. Practical View Calibration and Measurement Technique • Agilent Technologies N5221A PNA network analyser • Agilent Technologies 85070E open ended coaxial- line probe • 85070E software • reflection coefficient was measured • PNA Port OSL calibration • Probe Calibration open, short and deionised water • Temperature maintained at 250C • Ecal Module 27-02-2015 TERNA COLLEGE : ME THESIS 24
  • 25. Oils Result And Discussion Sample oils: 50 ml coconut oil 50ml groundnut oil 50ml sunflower 27-02-2015 TERNA COLLEGE : ME THESIS 25
  • 27. Brix Result And Discussion Sample: 100g Water and Sugar Solution 27-02-2015 TERNA COLLEGE : ME THESIS 27
  • 28. Sugar content ε’ ε"σ : conductivity 27-02-2015 TERNA COLLEGE : ME THESIS 28
  • 29. Milk Result And Discussion 27-02-2015 TERNA COLLEGE : ME THESIS 29
  • 30. Milk Adulteration Detection Sample: Fresh untreated cow’s milk temperature is maintained at 250C adulterants used are: water at room temperature, sugar, wheat flour as starch and sodium bi carbonate 27-02-2015 TERNA COLLEGE : ME THESIS 30 Image Courtesy: Times of India (6/3/14)
  • 34. Honey Result And Discussion A sample of honey from an apiary belonging to apis indica species of honeybee Adulterants: distilled water and corn syrup. 27-02-2015 TERNA COLLEGE : ME THESIS 34
  • 37. Rectangular Waveguide as Fixture: Simulation in HFSS 27-02-2015 TERNA COLLEGE : ME THESIS 37
  • 38. 27-02-2015 TERNA COLLEGE : ME THESIS 38 S11 vs Frequency S11= -19.927 at 5.81GHz
  • 39. Permittivity 1 27-02-2015 TERNA COLLEGE : ME THESIS 39Video
  • 40. Permittivity 10 27-02-2015 TERNA COLLEGE : ME THESIS 40Video
  • 41. SIMULATION RESULTS 27-02-2015 TERNA COLLEGE : ME THESIS 41
  • 42. Experimental Setup 27-02-2015 TERNA COLLEGE : ME THESIS 42
  • 43. Coax to Waveguide Adaptor 27-02-2015 TERNA COLLEGE : ME THESIS 43
  • 44. SAMPLE HOLDER AND SAMPLE 27-02-2015 TERNA COLLEGE : ME THESIS 44
  • 45. 85071E Software 27-02-2015 TERNA COLLEGE : ME THESIS 45
  • 46. Waveguide Fixture S11 S21 Coax to waveguide adapter 1 -21.79dB - Coax to waveguide adapter 2 -25.85dB - Combined waveguide -24.85dB -0.94dB Material Teflon 2.1 2.53 UHM 2.4 2.66 Wood 1.2-5 5.43 Wet-Wood - 12.58 27-02-2015 TERNA COLLEGE : ME THESIS 46
  • 48. Conclusion The experimental results on oil and brix content are close to the values specified in Literature and Theory Open ended coaxial technique can be utilised for oil adulteration detection-More experimentation with TDR required The Technique can satisfactorily used in Sugar Industries for measurement of brix due to wide variation in S11 data Milk and Honey adulteration detection methods are proved reliable and accurate Transmission/Reflection based method using software 85071E gives a very accurate Result compared to reflection based method. The fabricated waveguide design proves very useful in wood, paper and pulp industries for wood moisture measurement for instant results 27-02-2015 TERNA COLLEGE : ME THESIS 48
  • 49. Scope for Future Work Dielectric spectroscopy of oil Investigations for fat content measurement Cheese Industry Instead of Rectangular waveguide a circular waveguide can be used. More materials like metamaterials can be studied for their dielectric and magnetic property Different sensors including Patch antennas ,horn antennas etc. can be explored. 27-02-2015 TERNA COLLEGE : ME THESIS 49
  • 50. 27-02-2015 TERNA COLLEGE : ME THESIS 50 References [1] W. Skierucha; A. Wilczek, and A. Szyplowska, “Dielectric spectroscopy in agro physics”, Int. Agrophys., pp. 187-197, 2012. [2] T.W. Athey, M.A. Stuchly and S.S. Stuchly, “Measurement of radio-frequency permittivity of biological tissues with an open-ended coaxial line - Part I”, IEEE Transactions on Microwave Theory and Techniques, vol. 30 ,no.1, pp.82-86. 1982. [3] D. Bérubé, F.M. Ghannouchi, and P. Savard, “A comparative study of four open-ended coaxial probe models for permittivity measurements of lossy dielectric biological materials at microwave frequencies”. IEEE Transactions on Microwave Theory and Techniques, vol. 44, no.10, pp. 1928-1934, 1996. [4] M.M. Brady, S.A. Symons, and S.S. Stuchly, “Dielectric behaviour of selected animal tissues in vitro at frequencies from 2 to 4 GHz”, IEEE Transactions on Biomedical Engineering, vol. 28, no.3, pp.305-307, 1981. [5] R. ZAJÍČEK, L. OPPL, J. VRBA, “Broadband Measurement of Complex Permittivity Using Reflection Method and Coaxial Probes”,Technická 2, Prague. [6] Xiong Yu, Vincent P. Drnevich, and Robert L. Nowack Ref.: Yu, Xiong, Drnevich, Vincent P. and Nowack, Robert L., “Improvements of Soil Dielectric Mixing Model for Inversion Analysis of Time Domain Reflectometry Measurements", Proc. TDR 2006, Purdue University, West Lafayette, USA, vol 4, pp.19 , Sept. 2006. . New York, NY: The Chemical Catalog Company. 1929.
  • 51. 27-02-2015 TERNA COLLEGE : ME THESIS 51 [7] Scott B. Jones, Jon M. Wraith and Dani or, “Time domain reflectometry measurement principles and applications” Hydrol. Process., Vol 16, pp.141–153, 2002. [8] S.O. Nelson, “Dielectric properties of agricultural products - Measurements and applications”, IEEE Transactions of Electrical Insulation, vol. 26, no.5, pp.845-869. 1991. [9] J. W. Choi, J. Cho, Y. Lee, J. Yim, B. Kang, K. Oh, et al., “Microwave detection of metastasized breast cancer cells in the lymph node; potential application for sentinel lymphadenectomy,” Breast Cancer Research and Treatment, vol. 86 , no.2, pp. 107-115, 2004. [10] P. Debye, Polar Molecules. New York, NY: The Chemical Catalog Company. 1929. [11] A. Von Hippel, Dielectrics and Waves. New York, NY: John Wiley and Sons. 1954. [12] S.O. Nelson, “Dielectric properties measuring techniques and applications”, ASAE ,No. 983067. St. Joseph, MI: ASAE. 1998. [13] W.C. Dunlap,and B. Makower, “Radio frequency dielectric properties of dehydrated carrots”, Journal of Physical Chemistry , vol. 49: pp. 601-622, 1945. [14] T.M. Shaw, and J. A. Galvin, “High frequency heating characteristics of vegetable tissues determining from electrical conductivity measurements”, In Proceedings Institution of Radio Engineering, Institute of Radio Engineering and Electronics Publication, Chaberska, Prague: IREE, vol. 37, pp. 83-86. 1949. [15] W.E. Pace, W.B. Westphal and S.A. Goldblith. “Dielectric properties of commercial cooking oils”, Journal of Food Science, vol. 33, pp. 30-36, 1968. [16] V.N. Tran, S.S. Stuchly and A.W., “Kraszewski. Dielectric properties of selected vegetables and fruits at 0.1 - 10 GHz”, Journal of Microwave Power, vol. 19, no.4, pp.
  • 52. 27-02-2015 TERNA COLLEGE : ME THESIS 52 [17] M.A. Stuchly, and S.S. Stuchly, “Dielectric properties of biological substances – Tabulated”, Journal of Microwave Power, vol. 15, pp.19-26,1980. [18] M. Sucher and J. Fox, Handbook of Microwave Measurements. New York, NY: Polytechnic Press Institute. 1963. [19] G.P. de Loor, and F.W. Meijboom, “The dielectric constant of foods and other materials with high water contents at microwave frequencies”, Journal of Food Technology, vol. 1, pp.313-322, 1966. [20] N.E. Bengtsson, and P.O. Risman, “Dielectric properties of food at 3 GHz as determined by a cavity perturbation technique. II. Measurements on food materials”, Journal of Microwave Power, vol. 6 , no.2, pp. 107-123, 1971. [21] A.C. Metaxas and R. Meredith. Industrial Microwave Heating (IEEE Power Engineering Series). Piscataway, NJ:Peter Peregrinus. 1983. [22] A.W. Kraszewski, “Microwave aquametry - A review”, Journal of Microwave Power, vol. 15, no.4, pp. 209-220, 1980. [23] A. Kraszewski, Microwave Aquametry – Electromagnetic Interaction with Water Containing Materials, Piscataway, NJ: IEEE Press. 1996. [24] E. Nyfors, and P. Vainikainen, Industrial Microwave Sensors, chapter 2. Boston, MA: Artech House, Norwood. 1989. [25] J.P. Grant, , R.N. Clarke, G.T. Symm and N.M. Spyrou, “A critical study of the openended coaxial line sensor technique for RF and microwave complex permittivity measurements”, Journal of Physics: Electronics and Scientific Instrument, vol. 22, pp. 757-770, 1989.
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  • 54. 27-02-2015 TERNA COLLEGE : ME THESIS 54 [35] W Guo, X Zhu, H Liu, R Yue, S Wang, “Effects of milk concentration and freshness on microwave dielectric properties”, Journal of Food Engineering, vol. 99, pp. 344-350, 2010. [36] W Guo, X Zhu, Y Liu, H Zhuang ,Sugar and water contents of honey with dielectric property sensing, Elsevier: Journal of Food Engineering, vol. 97, no. 2, pp. 275–281 , March 2010. [37] W Guo, Y Liu, X Zhu, S Wang, “Dielectric properties of honey adulterated with sucrose syrup”, Elsevier: Journal of Food Engineering, Vol. 107, no.1, pp. 1-7, 2011. [38] S. Roberts, and A. von Hippel, “A new method for measuring dielectric constant and loss in the range of centimetre waves”, Journal of Applied Physics, vol. 17, pp.610-616, 1946. [39] S.O. Nelson, “Electrical properties of agricultural products - A critical review”, Transactions of the ASAE , vol.16, no. 2, pp. 384- 400, 1973. [40] S.O. Nelson, “Density dependence of the dielectric properties of particulate materials pulverized coal, flour, wheat samples”, Transactions of the ASAE , vol.26, no.6 , pp.1823-1825, 1983. [41] S.O. Nelson, “Moisture, frequency, and density dependence of the dielectric constant of shelled, yellow-dent field corn”, Transactions of the ASAE , vol. 30, no. 5, pp. 1573- 1578, 1984. [42] P.T. Corcoran, S.O. Nelson, L.E. Stetson and C.W. Schlaphoff, “Determining dielectric properties of grain and seed in the audio frequency range”, Transactions of the ASAE , vol.13, no.3 , pp.348-351, 1970. [43] Agilent, 2006. Basics of measuring the dielectric properties of materials. Application Note:32, USA.
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