PERMITTIVITY AND MEASUREMENTS 3693
00 0 PERMITTIVITY AND MEASUREMENTS tan de ¼ e =e . Mechanisms that contribute to the dielectric loss in heterogeneous mixtures include polar, electronic, atomic, and Maxwell–Wagner responses [7]. At RF and V. K OMAROV microwave frequencies of practical importance and cur- S. WANG rently used for applications in material processing (RF J. TANG Washington State University 1–50 MHz and microwave frequencies of 915 and 2450 MHz), ionic conduction and dipole rotation are domi- nant loss mechanisms [8]: 1. INTRODUCTION 00 00 00 00 s e ¼ ed þ es ¼ ed þ ð2Þ Propagation of electromagnetic (EM) waves in radio e0o frequency (RF) and microwave systems is described mathematically by Maxwell’s equations with corres- where subscripts ‘‘d’’ and ‘‘s’’ stand for contributions due to ponding boundary conditions. Dielectric properties of dipole rotation and ionic conduction, respectively; s is the lossless and lossy materials influence EM field distri- ionic conductivity in S/m of a material, o is the angular bution. For a better understanding of the physical frequency in rad/s, and e0 is the permittivity of free space processes associated with various RF and microwave or vacuum (8.854 10–12 F/m). Dielectric lossy materials devices, it is necessary to know the dielectric properties convert electric energy at RF and microwave frequencies of media that interact with EM waves. For telecommuni- into heat. The increase in temperature (DT) of a material cation and radar devices, variations of complex dielectric can be calculated from [9] permittivity (referring to the dielectric property) over a wide frequency range are important. For RF and micro- DT rC ¼ 5:563 10 11fE2e00 ð3Þ wave applicators intended for thermal treatments of dif- p Dt ferent materials at ISM (industrial, scientific, medical) frequencies, one needs to study temperature and moisture where Cp is the specific heat of the material in content dependencies of the permittivity of the treated Jkg 1 1 C 1, r is the density of the material in kg/m3, materials. E is the electric field intensity in V/m, f is the frequency in Many techniques have been developed for the measure- Hz, Dt is the time duration in seconds, and DT is the tem- ment of material permittivity. Some general descriptions perature rise in the material in 1C. It is clear from Eq. (3) of those methods are provided in the literature [1–4]. The that the rise in temperature is proportional to the mate- measurement results for diverse dielectric media are com- rial’s dielectric loss factor, in addition to electric field in- piled in the literature [5–7]. tensity squared, frequency, and treatment time. The objective of this article is to provide a brief descrip- In dielectric materials, the electric field strength de- tion of basic physical theory for the measurement of per- creases with distance z from the surface and is written as mittivity associated with three popular experimental az methods and to review the permittivities for different ma- E ¼ E0e ð4Þ terials. Most of these data are taken from the literature, but some of permittivity data were measured in Biological The attenuation factor a depends on the dielectric prop- Systems Engineering Department of Washington State erties of the material [5] and is given by University. The measurements were conducted by means 2 0sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 13 of open-ended coaxial probe method with commercial 1=2 00 2 instrumentation. 2p 41 0@ e A5 a ¼ e 1 þ 0 1 ð5Þ l0 2 e 2. THEORY OF PERMITTIVITY
where l0 is the free-space wavelength. Substituting Eq. (4) Permittivity is a quantity used to describe dielectric prop- into power equation Eq. (3), one obtains erties that influence reflection of electromagnetic waves at interfaces and the attenuation of wave energy within ma- 2az P ¼ P0e ð6Þ terials. In frequency domain, the complex relative permit- tivity e of a material to that of free space can be expressed Penetration depth of microwave and RF power is de- in the following form: fined as the depth where the power is reduced to 1/e (e ¼ 2.718) of the power entering the surface (Fig. 1). The e ¼ e0 je00 ð1Þ penetration depth dp in meters of RF and microwave en- ergy in a lossy material can be calculated by [5] The real part e0 is referred to as the dielectric constant and represents stored energy when the material is ex- vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffic 00 dp ¼ u 2sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi 3 ð7Þ posed to an electric field, while the dielectric loss factor e , u which is the imaginary part, influences energy absorption u e00 2 pffiffiffiffiffiffiffi 2pf t2e04 1 þ 15 and attenuation, and j ¼ 1. One more important para- e0 meter used in EM theory is a tangent of loss angle:
Encyclopedia of RF and Microwave Engineering, Edited by Kai Chang ISBN 0-471-27053-9 r 2005 John Wiley & Sons, Inc. 3694 PERMITTIVITY AND MEASUREMENTS
Lossy material factor (Fig. 2). For moist dielectric materials ionic conduc- tivity plays a major role at lower frequencies (e.g., o200 MHz), whereas both ionic conductivity and dipole Po Decay of EM power according to Lambert's law rotation of free water play a combined role at microwave frequencies. Maxwell–Wagner polarization arises from EM Po*1/e buildup of charges in the interface between components radiation in heterogeneous systems. The Maxwell–Wagner polariza- tion effect peaks at about 0.1 MHz [7], but in general, its dp Depth into the material z, m contribution is small compared to that of ionic conductiv- ity. For low-moisture media, bound water plays a major Figure 1. Typical penetration depth inside a large-sized material role in dielectric heating in the frequency range between (larger than the wavelength). 20 and 30 GHz [10,11] at room temperature (201C) [12]. For a pure liquid, the Debye model [13] describes the frequency-dependent dielectric properties in the rectan- where c is the speed of light in free space (3 108 m/s). gular form After obtaining the dielectric properties, the penetration depths of electromagnetic energy into selected materials e e ðe e Þot e ¼ e þ s 1 j s 1 ð8Þ can be calculated at the required frequency. Given fixed 1 1 þ o2t2 1 þ o2t2 dielectric properties, the penetration depth of a material is inversely proportional to frequency. It is, therefore, ex- where e1 is the infinite or high frequency relative permit- pected that in general deeper penetration corresponds to tivity, es is the static or zero-frequency relative permit- lower frequencies, and that higher frequencies result in tivity, and t is the relaxation time in seconds of the greater surface heating. It should be noted that the material. In general, the larger the molecules, the longer dielectric properties of lossy materials vary with frequen- the relaxation time. For a pure liquid, such as water, the cy but penetration depth does not vary exactly as 1/f. dielectric loss factor reaches the maximum at a critical Nevertheless, EM waves with short wavelength do not frequency related to the relaxation time ðfc ¼ 1=2ptÞ.Wa- penetrate deeply into most moist media [7], where the di- ter molecules are polar, and the most important constitu- electric constants and loss factors are relatively high. ent that contributes to the dielectric properties of moist dielectrics. Water molecules bound to the surface of polar materials in monolayers or multilayers have much longer 2.1. Frequency Effect relaxation times than do free water molecules. For exam- Dielectric properties of materials are affected by many ple, the relaxation time of bound water in different food factors, including frequency, temperature, and moisture materials at 201C is determined to be between 0.98 and content. Dielectric properties can vary significantly with 2.00 ns, corresponding to a peak in e00 at B100 MHz, frequency, which will be discussed in detail in this section. whereas the relaxation time t of free water in those foods The frequency-dependent trend of dielectric properties at 201C is between 0.0071 and 0.00148 ns, corresponding can provide important information of the material char- to a peak in e00 at around 16000 MHz [14]. Harvey and acteristics. In theory, electric conduction and various po- Hoekstra [10] found that e00 of monolayer bound water in larization mechanisms (including dipole, electronic, ionic, lysozyme at 251C peaked at 300 MHz and e00 for the second and Maxwell–Wagner) contribute to the dielectric loss layer bound water peaked at about 10000 MHz. The two
Conductivity
Effect of increasing temperature Log (ε")
Free water Effect of Maxwell-Wagner increasing effect temperature Bound water
Figure 2. Contributions of various mecha- nisms of the loss factor ðe00Þ of moisture mate- 0.1 100 20,000 MHz. rials as a function of frequency (f) [12]. Log (f) PERMITTIVITY AND MEASUREMENTS 3695
15 Frequency-dependent characteristics of complex biological materials, including moist foods, cannot be described with simple mathematical expressions. 10 ' 2.2. Temperature Effect 5 Temperature of a material has a significant effect on the dielectric properties. Generally, the loss factor increases 0 with increasing temperature at low frequencies due to ionic conductance and decreases with increasing temper- 5 ature at high frequencies due to free-water dispersion " (Fig. 2). In multidispersion materials, for example, the 0 transition is gradual because of the combined effects of 107 33108 109 331010 relaxation and the ionic conduction and there is a U-shape 00 Frequency (Hz) frequency response in e (Fig. 6). Debye related the relax- ation time for the spherical molecule to viscosity and tem- Figure 3. Dielectric constant ðe0Þ and loss factor ðe00Þ as a function perature as the result of randomizing agitation of the of frequency for packed lysozyme samples containing nearly two layers of bound water at 251C [10]. Brownian movement [5]
3n t ¼ V ð10Þ dispersions observed in Fig. 3 correspond to the first and kT second layers of bound water, respectively. Figure 4 shows a good example of Debye dielectric re- where n is the viscosity, T is the absolute temperature, V is laxation for butyl alcohol at 201C with single relaxation the volume, and k is a constant. For nonspherical water time measured with an open-ended coaxial probe connect- molecules, we may have the following relation ed to an impedance analyzer [19]. At low frequencies, in a n static region, where the dipoles have time to follow the t 1 ð11Þ variations of the applied field, the dielectric constant of T butyl alcohol has a value of B17. The loss factor is small while the viscosity of all fluid decreases with increasing for both high and low frequencies and reaches a peak at temperature [16] the relaxation frequency of B250 MHz. Similar frequency-dependent permittivity can be found Ea=RgT in water, methanol, and ethanol and can be expressed in v ¼ v0e ð12Þ the following relationships, respectively [15]: where Ea is activation energy and Rg is the universal gas constant. Therefore, as temperature rises, relaxation time 74:59 ¼ þ ð Þ for water decreases. The shifting of the relaxation time e 5:62 9 water 1 þ jf =17:0 10 toward a lower value (thus the frequency at the maximum 00 27:89 e shifts toward a higher value as temperature increases) e ¼ 5:76 þ ðmethanolÞ ð9Þ 00 1 þ jf =2:709 109 reduces the value of e for water at a fixed microwave fre- quency (Fig. 5). For example, as the relaxation time t 20:84 decreases with increasing temperature, the dispersion e ¼ 4:44 þ ðethanolÞ 1 þ jf =0:826 109 peak moves to higher frequencies and the loss factor of pure water at 2450 MHz decreases with increasing tem- perature. The dielectric constant e0 of free water also de- creases with increasing temperature as the result of 20 increased Brownian movement. 00 ' The dielectric loss factor es due to conduction decreases 16 " with increasing frequency as shown in Eq. (2). The 00 contribution of es to the overall loss factors is smaller at 12 2450 MHz than at 915 Hz (Fig. 6). The electric conductiv- ity s in ionic solutions increases with temperature due to 8 decreased viscosity and hence increased ion mobility [17]. 00 Therefore, based on Eq. (2), es also increases with temper-
Dielectric properties 4 ature (Fig. 6). At 915 MHz the dielectric constant of ionic solutions generally increases with temperature. 0 The dielectric properties of high-moisture-content sub- 1 10 100 1000 10000 stances change with temperature [19]. An example of the Frequency (MHz) dielectric loss factor ðe00Þ of fifth-instar codling moths mea- Figure 4. Dielectric constant ðe0Þ and loss factor ðe00Þ of butyl al- sured at five temperatures is shown in Fig. 7. The loss cohol at 201C [19]. factor decreases with increasing frequency, reaching 3696 PERMITTIVITY AND MEASUREMENTS
90 0°C 20°40°C 0°C 80 40 ° 0°C 25 ° 70 20 C 50° 30 40°C 60 75° 50 " " ' 20 "t d 40 "d " 30 10 ( ")t =+"d " 20 " 0 10 108 109 1010 1011 0 Frequency (Hz) 109 1010 1011 1012 1013 Figure 6. Effect of temperature on dielectric loss factor ðe00Þ of (a) 0.5 N aqueous sodium chloride at three temperatures [18]. 50 0°C 40 25° 50° which a preferentially heated subject in an EM field ac- 30 ° celerates heating as its temperature rises. " 75 20 Figure 8 shows the loss factor of a typical dry nut (wal- nut kernels) over the frequency range from 1 to 1800 MHz 10 at five temperatures. The e00 values are less than 1 at fre- 00 0 quencies below 50 MHz. The e values peak in the range 109 1010 1011 1012 1013 between 500 and 1000 MHz. The peak value of e00 for wal- nut kernels decreases with increasing temperature, while (radians/s) the frequency corresponding to the peak e00 shifts to a (b) higher value. This temperature-dependent trend is typical Figure 5. Effect of temperature on dielectric constant ðe0Þ and of polar molecules [20]. At any selected frequency in the loss factor ðe00Þ of free water (o ¼ 2pf, where f is frequency in Hz) tested range, the loss factor of the walnut kernel generally [22]. decreases with increasing temperature; that is, for a given EM field intensity, higher temperature walnuts will ab- about 12 at 1800 MHz. The loss factor of codling moth lar- sorb less energy than cooler ones, resulting in improved vae increases with temperature, especially at low frequen- heating uniformity. cies. This is due mainly to the increase in ionic conduction Ice is almost transparent to microwaves (Table 1). at high temperatures [12]. Increasing dielectric loss factor When a lossy material is frozen, both dielectric constant with temperature often results in a well-known phenom- and loss factor are significantly reduced; the degree of re- enon, commonly referred to as ‘‘thermal runaway’’ [7], in duction depends, to a large extent, on the amount of water
500 20°C 30°C 40°C 400 50°C 60°C
300 Effect of increasing temperature
Loss factor 200
100
0 Figure 7. Dielectric loss factor of codling 1 10 100 1000 moth larvae (slurry) at five temperatures [19]. Frequency (MHz) PERMITTIVITY AND MEASUREMENTS 3697
5
20°C 30°C Effect of ° 4 40 C increasing 50°C temperature 60°C ")
ε 3
2 Loss factor ( Loss factor
1
0 Figure 8. Dielectric loss factor of walnut ker- 1 10 100 1000 nels as a function of frequency at five temper- Frequency (MHz) atures [19]. in the unfrozen state and the ionic conductivity of the free dielectric permittivity of many materials. Nondestructive, water. broadband (RF and microwave ranges), and high-temper- ature (r12001C) measurements can be preformed with 2.3. Moisture Effect this method using commercially available instrumenta- tion. Its well-developed theory makes it possible to obtain Moisture content is one of the major components of most sufficiently accurate results for both medium-loss and biological materials. In general, the higher the moisture high-loss media [24–26]. content, the larger the dielectric constant and loss factor Figure 10 illustrates an OCP system used at Washing- of the materials [20, 22, 23]. Water in moist dielectric ma- ton State University. It consists of an automatic network terials can be divided, in descending mobility, into (1) wa- analyzer (ANA) with a calibration kit, custom-built test ter held in intercellular space or capillaries, (2) multilayer water, and (3) monolayer water that is tightly bound to the polar sites. The free-water molecules have dielectric prop- erties similar to those of liquid water, while the bound water exhibits icelike dielectric properties. Dielectric properties of biomaterials, in general, decrease rapidly with decreasing moisture content to a critical moisture level. Below this moisture level, the reduction in loss fac- tor is less significant because of the bound water (Fig. 9). During microwave drying, the wetter parts of biomaterials absorb more microwave energy and tend to level off the Rate of evaporation uneven moisture distribution.
3. MEASUREMENT PRINCIPLES AND METHODS
3.1. Open-Ended Coaxial Probe Method Open-ended coaxial probe (OCP) method is currently one of the most popular techniques for measuring of complex Loss factor Table 1. Dielectric Properties of Water and Ice at 2450 MHz Relative Dielectric Loss Factor Loss Tangent State of Water Constant ðe0Þðe00Þðtan dÞ 1 Water (25 C) 78 12.5 0.16 Mc Mean moisture content, M Ice 3.2 0.0029 0.0009 Figure 9. Rate of evaporation and dielectric loss factor as affect- Source: Ref. 21. ed by food moisture content [7]. 3698 PERMITTIVITY AND MEASUREMENTS
Coaxial cable
Thermometer Probe
Sample Jacket
Figure 10. Schematic diagram of experimen- tal setup realizing open-ended coaxial probe method [19]. Impedance analyzer Temperature sensor Spring Water bath cell, a programmable circulator, a coaxial cable, and a per- terms of S parameters of the connector: sonal computer connected to the ANA through a special bus. The material under study is placed in a stainless steel a ¼ S ; a ¼ S S e 2gz; a ¼ S e 2gz ð15Þ pressureproof test cell. The probe is kept in close contact 11 11 12 12 21 22 22 with the sample during the measurements via a stainless steel spring and piston. A thin rigid stainless steel ther- In the inverse coaxial probe model, it is assumed that a mocouple probe passes onto the center of the sample to sample has a semiinfinite size. A few additional conditions measure sample temperature. The programmable circula- must be satisfied to avoid measurement error in the OCP tor pumps a temperature-controlled liquid (90% ethylene method: glycol and 10% water by volume) through the water jacket of the test cell, allowing the sample inside to be heated and * Minimize thermal expansion of both conductors of cooled. coaxial line at high temperatures. The sensing element of an OCP system is an open-end- * Intimate contact between the probe and the sample; ed cylindrical coaxial line that is excited by transverse liquid sample may flush the probe and the surface electromagnetic (TEM) wave. Parameters (amplitude and roughness of solid sample should be less than 0.5 mm phase) of incident and reflected signals are detected by the [28]. ANA. The complex dielectric permittivity is determined * according to the reflected coefficient ðG ¼ G0 jG00Þ as fol- Minimize disturbance caused by temperature, vibra- lows [27] tion, or any other external factors after calibration and during measurement. 2G00 0 ¼ð Þ 1 e Aef 0 2 002 ; The OCP method is very well suited for liquids or soft solid ð1 þ G Þ þ G samples. It is accurate, fast, and broadband (from 0.2 to up ð13Þ 02 002 to 20 GHz). The measurement requires little sample prep- 00 1 1 G G e ¼ðAef Þ aration. A major disadvantage of this method is that it is ð1 þ G0Þ2 þ G002 not suitable for measuring materials with low dielectric property (plastics, oils, etc.). where Ae is the empirical coefficient dependent on char- acteristic impedance of the probe and sample size. In order to eliminate the influence of reflections caused by trans- 3.2. Transmission-Line Method mission-line discontinuities, a calibration procedure is uti- The transmission-line method (TLM) belongs to a large lized. The EM characteristics of the measurement system group of nonresonant methods of measuring complex di- are analyzed using three standard terminations (open, electric permittivity of different materials in a microwave short, and 50 O). Then any material with well-known di- range [7,51]. Several modifications to this method exist, electric properties such as deionized water, for example, is including the free-space technique [29], the open- tested. The actual reflection coefficient differs from reflec- circuit network method (see previous section), and the tion coefficient measured using ANA (G ) [25] m short-circuited network method. Usually three main types of transmission lines are used as the measurement cell in G a G ¼ m 11 ð14Þ TLM: rectangular waveguide, coaxial line, and microstrip a22ðGm a11Þþa12 line. Consider the distribution of the TEM wave in a short- where a11 is the directivity error, a12 is the frequency re- circuited coaxial line partially filled with a lossy material sponse error, a22 is the source match error. Taking into under study (Fig. 11). Analyzed sample is placed near the account propagation constant (g) and distance from the short-circuited end of the transmission line. The dielectric connector to the probe head (z) we can calculate aij in properties of the sample are determined using the follow- PERMITTIVITY AND MEASUREMENTS 3699
Short circuit end
d Lossy sample Coaxial line