electrical characterization of non conducting materials using reflection based

Electrical Characterization of Non-Conducting

Materials Using Reflection Based Microwave

Technique

B Y

PAL L AV I M AL AM E ( T P 2 F 1 2 1 3 0 0 1 )

G U I D E

D R . R AJ I V G U P TA

Submitted in partial fulfilment of the

requirements

of the degree of

Master of Engineering

by

Pallavi R. Malame

TP2F1213001Supervisor:

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


Introduction

Microwave Reflectometry

Features of FDR

Motivation

Problem Statement

Objectives


Motivation

Society for Applied Microwave Electronics Engineering & Research

Department of Electronics and Information Technology

Under the aegisof

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


ObjectivesTo 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

??


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


Electrical Characterization of Non-Conducting Materials Using Reflection Based MicrowaveTechnique

Electrical Characterization Non-Conducting Materials Reflection Based Microwave Technique

Figures Just for Illustration Purpose

Non Magnetic materials Products

Measuring Electrical Parameter only: Dielectric

S11ReflectionS21TransmissionEr’Dielectric ConstantEr’’ Loss Factor

C Band ( 5.81 GHz)

Why 5.81??


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. Fox2) Industrial Microwave Heating by A.C. Metaxas and R. Meredith

• 1980 -The dielectric properties of food materials in the microwave region can bedetermined 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 measurementmethods, namely, lumped circuit, resonator, transmission line, and free-spacemethods.


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-endedcoaxial-line probes have been used for broadband permittivity measurements [25-26].

• A similar technique is used for permittivity measurements on fresh fruits and vegetablesby 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]MilkUse of open ended coaxial probe technique for dielectric property measurement ofmilk is mentioned in Advanced Dairy Chemistry by McSweeney


• 1974 - Mudgett et.al.[32] has observed dielectric properties of skim milk over thetemperature range 25-55oC.

• 2006 - Nunes et al. [33] has examined the complex dielectric permittivity of UHT milk in afrequency 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 andsucrose 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/reflectionbased method which are open resonant structures are fabricated at the MassachusettsInstitute of Technology [11, 38].

• 1973,1983,1984 - Coaxial-line and rectangular wave-guide sample holders are used withvarious 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 coaland mineral samples [40].

• 1970 - Dielectric properties of grain samples are measured using a precision bridge overaudio frequencies from 250 Hz to 20 kHz with sample holders confined in a coaxial sampleholder and reported in [42].


Permittivity and Dielectric Mechanism

"'

0

rrrj

'

"

tanr

r

r

'

r

''

r

Complex RelativePermittivity

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.


Dielectric Theory

"'rrr j "'

rrr j

Electric Magnetic

Permittivity Permeability

FieldsFields

STORAGE

LOSS

MUT

STORAGE

LOSS

Non Magnetic Material!

1


Interaction of Medium with EM Waves


Dielectric Mechanism

Random Motion of water molecules

Orientation in Electromagnetic Field


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


Return

Relaxation time

11

10

100

10 100

Water at 20o C

f,

GHz

most energy is lost at 1/t

'r

"r

Cole Cole Plot


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


Vector Network Analyzer

N5221A PNA.


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.


Transmission/Reflection based Electrical Characterization of Non-Conducting Materials.

Sensor waveguide

Measured parameter S11 and S21

Features:

• Accuracy

• Best for solid materials.


Open Ended Coaxial Probe Technique

Sample thickness

d


Practical ViewCalibration 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


Oils

Result And Discussion

Sample oils:50 ml coconut oil50ml groundnut oil50ml sunflower


ε’

Low Frequency

ε"


Brix


Sample: 100g Water and Sugar Solution


Sugar content ε’ ε"σ : conductivity


Milk



Milk Adulteration Detection

Sample: Fresh untreated cow’s milktemperature is maintained at 250Cadulterants used are:water at room temperature, sugar, wheat flour as starch and sodium bi carbonate


Image Courtesy: Times of India (6/3/14)

ε’’ε’

Water

Water

ε’’

Water


Dielectric Response

Sugar

ε’


ε’

ε’’


Honey

Result And DiscussionA sample of honey from an apiary belonging to apis indica species of honeybee

Adulterants:distilled water and

corn syrup.


ε’

Water

ε’’

Water


ε’

cornsyrup

ε’’

cornsyrup


Rectangular Waveguide as Fixture: Simulation in HFSS



S11 vs Frequency

S11= -19.927 at 5.81GHz

Permittivity 1

27-02-2015 TERNA COLLEGE : ME THESIS 39Video

Perm1.avi

Permittivity 10

27-02-2015 TERNA COLLEGE : ME THESIS 40Video

Perm_10.avi

SIMULATION RESULTS


Experimental Setup


Coax to Waveguide Adaptor


SAMPLE HOLDER AND SAMPLE


85071E Software


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


Frequency 5.71GHz

0.2

0.1


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


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.



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.


[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 dehydratedcarrots”, Journal of Physical Chemistry , vol. 49: pp. 601-622, 1945.[14] T.M. Shaw, and J. A. Galvin, “High frequency heating characteristics of vegetabletissues determining from electrical conductivity measurements”, In ProceedingsInstitution of Radio Engineering, Institute of Radio Engineering and ElectronicsPublication, Chaberska, Prague: IREE, vol. 37, pp. 83-86. 1949.[15] W.E. Pace, W.B. Westphal and S.A. Goldblith. “Dielectric properties of commercialcooking 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 selectedvegetables and fruits at 0.1 - 10 GHz”, Journal of Microwave Power, vol. 19, no.4, pp.


[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 othermaterials with high water contents at microwave frequencies”, Journal of FoodTechnology, vol. 1, pp.313-322, 1966.[20] N.E. Bengtsson, and P.O. Risman, “Dielectric properties of food at 3 GHz asdetermined 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 PowerEngineering 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 WaterContaining 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 openendedcoaxial line sensor technique for RF and microwave complex permittivity measurements”, Journal of Physics: Electronics and Scientific Instrument, vol. 22, pp.757-770, 1989.


[26] D.V. Blackham, and R.D. Pollard, “An improved technique for permittivitymeasurements using a coaxial probe”, IEEE Transactions of Instrumentation andMeasurement , vol. 46 , no. 5, pp.1093-1099. 1997.[27] S.O. Nelson, “Measurement of microwave dielectric properties of particulatematerials”, Journal of Food, 1994.[28] H. Lizhi, K. Toyoda, and I. Ihara, “Dielectric properties of edible oils and fatty acidsas 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 withvegetable 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 andanti-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, “Dielectricbehaviour of semi-solid food at low, intermediate and high moisture contents”, Journalof 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 1and 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, “Electromagneticproperties of milk and its constituents at 2.45 MHz”, Journal of Microwave Power andElectromagnetic Energy, vol. 27 , no.4 , pp. 199–204,1992.


[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 withsucrose 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 andloss 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 materialspulverized 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 constantof 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, “Determiningdielectric properties of grain and seed in the audio frequency range”, Transactions of theASAE , vol.13, no.3 , pp.348-351, 1970.[43] Agilent, 2006. Basics of measuring the dielectric properties of materials. ApplicationNote:32, USA.


[44] D.M. Slaten,; B.N. Scott,; Gordon, B. Lloyd, “ Techniques and applications ofpermittivity measurements”, Electrical Insulation and Dielectric Phenomena, IEEE1996 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, “MicrowaveElectronics 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: Compositionalquality. 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 inUSA, June 14, 2012

Thank You


electrical characterization of non conducting materials using reflection based

Engineering

microwave method

terna college

microwave technique

homogeneous materials

magnetic materials products

electrical parameter

rapid measurement system

electrical conductivity