s11 calibration of cut-off circular waveguide with three

9
IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 2021 93 PAPER S 11 Calibration of Cut-OCircular Waveguide with Three Materials and Related Application to Dielectric Measurement for Liquids Kouji SHIBATA a) , Member SUMMARY A method for the calibration of S 11 at the front surface of a material for a coaxial-feed type cut-ocircular waveguide with three refer- ence materials inserted and no short termination condition was proposed as a preliminary step for dielectric measurement in liquids. The equations for jig calibration of S 11 with these reference materials were first defined, and the electrostatic capacitance for the analytical model unique to the jig was quantified by substituting the reflection constant (calculated at frequencies of 0.50, 1.5 and 3.0 GHz using the mode-matching (MM) technique) into the equivalent circuit, assuming the sample liquid in the jig. The accuracy of S 11 measured using the proposed method was then verified. S 11 for the front surface of the sample material was also measured with various liq- uids in the jig after calibration, and the dielectric constants of the liquids were estimated as an inverse problem based on comparison of S 11 calcu- lated from an analytical model using EM analysis via the MM technique with the measured S 11 values described above. The eectiveness of the proposed S 11 calibration method was verified by comparison with dielec- tric constants estimated after S 11 SOM (short, open and reference material) calibration and similar, with results showing favorable agreement with each method. key words: dielectric measurement, liquid, cut-ocircular waveguide, S 11 , calibration 1. Introduction To comply with safety standards prescribing limits on expo- sure to EM (electromagnetic) waves, evaluation of the spe- cific absorption rates (SARs) of various radio systems has recently become necessary [1]. Against this background, M. A. Stuchly et al. (1980) overviewed dielectric measure- ment for various lossy media based on reflected and trans- mitted EM waves with a sample in the middle or at the tip of a transmission line [2]. In the above research, di- electric measurement based on reflection coecients with a sample in a cut-ocircular waveguide placed at the tip of a coaxial line was also examined, but no actual dielec- tric measurement example with this jig shape was included in the published paper [2]. O. G¨ ottmann et al. (1996) pro- posed dielectric measurement based on the reflection coef- ficient with a sample in both the coaxial line and the cut-ocircular waveguide, which is placed at the tip of the con- nector [3]. In this method, the jig must be mounted after S 11 calibration at the coaxial tip with a general SOL (short, Manuscript received May 13, 2020. Manuscript revised July 9, 2020. Manuscript publicized August 14, 2020. The author is with Hachinohe Institute of Technology, Hachinohe-shi, 031–8501 Japan. a) E-mail: [email protected] DOI: 10.1587/transele.2020ECP5025 open and load) calibration kit. Accordingly, measured S 11 values and estimated dielectric constant are greatly aected by small dierences in the length of the center conductor. Against this background, Shibata (2010) previously outlined the eectiveness of a high-precision broadband dielectric measurement method for small amounts of certain liquids based on S 11 using a cut-ocircular waveguide [4]. In this work, application of the mode-matching (MM) technique enabled calculation of S 11 for an analytical model more quickly than with other approaches. As part of eorts to develop this method, the potential for dielectric measure- ment in liquids in the low frequency band, estimation using a simple formula and methods for improving measurement accuracy have also been presented [5][10]. Meanwhile, the coaxial probe (flange) method is commonly adopted to de- termine complex permittivity in solid and liquid high-loss electrical materials [11][13]. However, the dielectric con- stant changes significantly in the coaxial method due to EM wave reflection from the vessel, which hinders determina- tion of uncertainty. As the sample in the proposed method is inserted into the cut-ocircular waveguide section, the con- finement of EM waves to this waveguide supports high mea- surement accuracy by eliminating the need to consider wave reflection from the vessel when the coaxial probe is used, thereby facilitating determination of permittivity in small amounts of scarce liquids. However, this method produces an error eect on S 11 and the dielectric constant caused by the dierence between the actual dimensions of the jig and the analytical model. In this study, a method for the calibration of S 11 based on the insertion of three reference materials with no short termination condition using a VNA (vector network ana- lyzer) was newly proposed as a preliminary step for dielec- tric measurement in liquids via the cut-ocircular wave- guide reflection method. A calibration equation for S 11 based on three impedance standards was first defined from the error model of the measurement system, and a theo- retical value for a reflection constant based on the inser- tion of the three reference materials was also defined for equivalent circuit analysis of the analytical model. Here, the electrostatic capacitance for the analytical model unique to the jig was quantified by substituting the reflection con- stant (calculated using EM analysis via the MM technique) into the equivalent circuit, assuming the sample liquid in the jig. The S 11 value for the jig was then calibrated from the Copyright c 2021 The Institute of Electronics, Information and Communication Engineers

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Page 1: S11 Calibration of Cut-Off Circular Waveguide with Three

IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 202193

PAPER

S11 Calibration of Cut-Off Circular Waveguide with ThreeMaterials and Related Application to Dielectric Measurement forLiquids

Kouji SHIBATA†a), Member

SUMMARY A method for the calibration of S11 at the front surface of amaterial for a coaxial-feed type cut-off circular waveguide with three refer-ence materials inserted and no short termination condition was proposed asa preliminary step for dielectric measurement in liquids. The equations forjig calibration of S11 with these reference materials were first defined, andthe electrostatic capacitance for the analytical model unique to the jig wasquantified by substituting the reflection constant (calculated at frequenciesof 0.50, 1.5 and 3.0 GHz using the mode-matching (MM) technique) intothe equivalent circuit, assuming the sample liquid in the jig. The accuracyof S11 measured using the proposed method was then verified. S11 for thefront surface of the sample material was also measured with various liq-uids in the jig after calibration, and the dielectric constants of the liquidswere estimated as an inverse problem based on comparison of S11 calcu-lated from an analytical model using EM analysis via the MM techniquewith the measured S11 values described above. The effectiveness of theproposed S11 calibration method was verified by comparison with dielec-tric constants estimated after S11 SOM (short, open and reference material)calibration and similar, with results showing favorable agreement with eachmethod.key words: dielectric measurement, liquid, cut-off circular waveguide, S11,calibration

1. Introduction

To comply with safety standards prescribing limits on expo-sure to EM (electromagnetic) waves, evaluation of the spe-cific absorption rates (SARs) of various radio systems hasrecently become necessary [1]. Against this background,M. A. Stuchly et al. (1980) overviewed dielectric measure-ment for various lossy media based on reflected and trans-mitted EM waves with a sample in the middle or at thetip of a transmission line [2]. In the above research, di-electric measurement based on reflection coefficients witha sample in a cut-off circular waveguide placed at the tipof a coaxial line was also examined, but no actual dielec-tric measurement example with this jig shape was includedin the published paper [2]. O. Gottmann et al. (1996) pro-posed dielectric measurement based on the reflection coef-ficient with a sample in both the coaxial line and the cut-offcircular waveguide, which is placed at the tip of the con-nector [3]. In this method, the jig must be mounted afterS11 calibration at the coaxial tip with a general SOL (short,

Manuscript received May 13, 2020.Manuscript revised July 9, 2020.Manuscript publicized August 14, 2020.†The author is with Hachinohe Institute of Technology,

Hachinohe-shi, 031–8501 Japan.a) E-mail: [email protected]

DOI: 10.1587/transele.2020ECP5025

open and load) calibration kit. Accordingly, measured S11

values and estimated dielectric constant are greatly affectedby small differences in the length of the center conductor.Against this background, Shibata (2010) previously outlinedthe effectiveness of a high-precision broadband dielectricmeasurement method for small amounts of certain liquidsbased on S11 using a cut-off circular waveguide [4]. In thiswork, application of the mode-matching (MM) techniqueenabled calculation of S11 for an analytical model morequickly than with other approaches. As part of efforts todevelop this method, the potential for dielectric measure-ment in liquids in the low frequency band, estimation usinga simple formula and methods for improving measurementaccuracy have also been presented [5]–[10]. Meanwhile, thecoaxial probe (flange) method is commonly adopted to de-termine complex permittivity in solid and liquid high-losselectrical materials [11]–[13]. However, the dielectric con-stant changes significantly in the coaxial method due to EMwave reflection from the vessel, which hinders determina-tion of uncertainty. As the sample in the proposed method isinserted into the cut-off circular waveguide section, the con-finement of EM waves to this waveguide supports high mea-surement accuracy by eliminating the need to consider wavereflection from the vessel when the coaxial probe is used,thereby facilitating determination of permittivity in smallamounts of scarce liquids. However, this method producesan error effect on S11 and the dielectric constant caused bythe difference between the actual dimensions of the jig andthe analytical model.

In this study, a method for the calibration of S11 basedon the insertion of three reference materials with no shorttermination condition using a VNA (vector network ana-lyzer) was newly proposed as a preliminary step for dielec-tric measurement in liquids via the cut-off circular wave-guide reflection method. A calibration equation for S11

based on three impedance standards was first defined fromthe error model of the measurement system, and a theo-retical value for a reflection constant based on the inser-tion of the three reference materials was also defined forequivalent circuit analysis of the analytical model. Here,the electrostatic capacitance for the analytical model uniqueto the jig was quantified by substituting the reflection con-stant (calculated using EM analysis via the MM technique)into the equivalent circuit, assuming the sample liquid in thejig. The S11 value for the jig was then calibrated from the

Copyright c© 2021 The Institute of Electronics, Information and Communication Engineers

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94IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 2021

reflection constant with three reference materials (pure wa-ter, methanol and air) inserted using a VNA over the fre-quency band of 0.50–3.0 GHz. The validity of the cali-brated S11 values obtained with the proposed method wasverified via comparison with the S11 value measured afterSOM (short/open and reference material (pure water)) cali-bration conditions [14]. S11 at the front surface of the samplewas measured with various liquids in the jig after calibrationwith three reference materials, and the dielectric constantsof various liquids were estimated from the above S11 basedon an inverse problem approach involving comparison withthe S11 value calculated using EM analysis via the MM tech-nique [4], [10]. The results were compared with the permit-tivity values estimated as an inverse problem after SOM cal-ibration conditions [14] and similar, with results showing fa-vorable agreement of values determined with each method.

2. Dielectric Measurement Method and Related S11

Calibration Theory

In this method, the dielectric constant is estimated fromthe S11 value measured with various liquids in the cut-offwaveguide with a coaxial feed-type SMA connector (Fig. 1).Here, a novel S11 calibration method involving the use ofthree reference liquids and no short termination is proposedas a preliminary step for dielectric measurement. The esti-mation procedure is as follows:

1. The measurement jig (a coaxial-feed-type cut-off circu-lar waveguide with an SMA connector) is attached to ameasurement cable connected to a VNA.

2. S11 is calibrated at the front surface of the sample of thejig with the three reference material inserted.

3. S11 at the front of the sample material is measured withvarious liquids in the jig.

4. The dielectric constant is estimated as an inverse prob-lem so that the calculated S11 value for the jig-relatedanalytical model corresponds to the measured value foreach frequency.

The proposed S11 calibration method with three ref-erence materials is outlined here. Calibration for S11 witha short condition – as applied in the previous stage of di-electric measurement of materials based on reflection co-efficient differences with different samples in the jig – haspreviously been proposed (e.g., Ref. [15]). This procedure isapplied in commercial products such as dielectric measure-ment kits involving the use of coaxial probes from Keysight

Fig. 1 Jig cross-section

Technologies [16]. However, there is concern regarding theinstability of electrical contact with the inner surface of theouter conductor of the coaxial line using this structure, andrelated uncertainty in measured values of S11 and complexpermittivity.

In this study, a reference material is used instead ofload termination as a calibrator. S11 is also not determinedwith the coaxial tip short-circuited, but is measured with asecond reference material inserted. Based on the above, S11

values determined with the three reference liquids in the jigare used for S11 calibration with this method. Accordingly,the theoretical values of S11 at the front surface of the sam-ple with the three termination conditions must also be cal-culated from equivalent circuit analysis. Meanwhile, actualS11 values with these materials inserted are measured usingthe VNA. The S11 value for the front surface of the samplewith insertion of an unknown material is then calibrated viasubstitution of these values into the equation described later.The equation for calibration of the coaxial line S11 valuewith the proposed method and the three reference materialsis derived as outlined below. Equation (1) is first satisfied forthe reflected wave b1 observed with the EM wave a1 incidentfrom the measuring instrument in the two-terminal pair cir-cuit of Fig. 3, which corresponds to the analytical model ofFigs. 1 and 2.[

b1

b2

]=

[S11 S12

S21 S11

]·[

a1

a2

](1)

The reflection coefficients for Ref. (Ports) 1 and 2 in Fig. 3are then defined as ρi and Γi in Eqs. (2) and (3), correspond-ing to the these termination conditions:

ρi =b1

a1(2), Γi =

a2

b2(3)

Here, three termination conditions and one unknown mate-rial are then defined with insertion into the jig depending onsubscripts 1, 2 and 3 for Γi and ρi.

Accordingly, the reflection coefficient ρi for Ref. 1(Port 1) is calculated using Eq. (4) with systematic errorterm settings of EDF = S11, ESF = S22, ERF = S12 andS21 = 1 in Eqs. (1)–(3).

ρi = EDF +Γi · ERF

1 − ESF · Γi(4)

The reflection coefficient Γi for Ref. 2 (Port 2) is thus cal-culated as per [15] based on the following equation with re-placement of Γi in Eq. (4):

Γi =a2

b2=

ρi − EDF

ESF · ρi + ERF − ESF · EDF(5)

Fig. 2 Analytical model Fig. 3 Equivalent circuit

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SHIBATA: S11 CALIBRATION OF CUT-OFF CIRCULAR WAVEGUIDE WITH THREE MATERIALS95

Fig. 4 Equivalent circuit

Here, Γi in Eq. (5) can be determined from the three un-knowns of EDF, ESF, ERF and γ by placing the denominatorof Eq. (5) as γ and adapting the equation based on compari-son of the association among Eqs. (1)–(3) and (4), (5) as inthe following equation:

ESF =ρ2 − ρ3 + γ · (Γ3 − Γ2)

Γ2 · ρ2 − Γ3 · ρ3(6)

EDF = ρ1 − Γ1 · (ESF · ρ1 + γ) (7)

ERF = EDF · ESF + γ (8)

γ=(ρ2−ρ1)·(Γ2 ·ρ2−Γ3 ·ρ3)+(ρ2−ρ3)·(Γ1 ·ρ1−Γ2 ·ρ2)

(Γ3−Γ2)·(Γ2 ·ρ2−Γ1 ·ρ1)+(Γ1−Γ2)·(Γ3 ·ρ3−Γ2 ·ρ2)(9)

The open-ended coaxial line shown in Figs. 1 and 2 can berepresented as the equivalent circuit shown in Fig. 4, whereCf and εri · C0 are defined as the fringing capacitance at thetip of the coaxial line and the sample insertion section at thecoaxial tip, respectively. Here, CT = Cf + εri ·C0 is satisfied.Accordingly, the input impedance ZΓi for Ref. 2 (Port 2) isexpressed by

ZΓi =1

jω ·CT=

1jω · (C f + εri ·Co)

(10)

Thus, the reflection constant Γi for Ref. 2 (Port 2) can becalculated [15] by

Γi =ZΓi − Z0

ZΓi + Z0=

1 − jωC0 · εri · Z0 − jωC f · Z0

1 + jωC0 · εri · Z0 + jωC f · Z0(11)

Here, Z0 is the characteristic impedance of Port 1, definedas Z0 = 50 Ω. Accordingly, the theoretical reflection coeffi-cient Γi for Ref. 2 (Port 2) with the assumption of the refer-ence material in the jig is then determined based on Eq. (11)by substituting the Cf and C0 values of the equivalent cir-cuit shown in Fig. 4. In the proposed S11 method, to im-prove accuracy in measurement of S11 against the conven-tional method [15], [17]–[19], Cf and C0 in Eq. (10) are de-termined by substituting the input impedance calculated viathe MM technique for the analysis model of Fig. 2 at eachfrequency into ZΓi on the left side. Here, ZΓi for open termi-nation is determined by substituting εri = 1.0 (air) into εri inEq. (10). Accordingly, EDF, ERF and ESF (system errors inEq. (5)) are determined based on Eqs. (6)–(9) from the the-oretical value of the reflection constant Γi (where i = 1, 2and 3) under the three termination conditions in Ref. 2 andthe measured value of the reflection coefficient ρi in Ref. 1.Equation (5) is also transformed as below based on the re-lationship between the measured reflection coefficient ρmeas

from Ref. 1 and the reflection coefficient Γcorr from Ref. 2 ascalibrated from the theoretical value of the reflection coeffi-cient Γi.

Γcorr =ρmeas − EDF

ESF · ρmeas + ERF − ESF · EDF(12)

From the above relationship, the calibrated reflection coeffi-cient Γcorr for Ref. 2 (Port 2) is obtained by substituting themeasured ρmeas value for Ref. 1 (Port 1) and the EDF, ERF

and ESF values determined from the three termination con-ditions into Eq. (12).

In this method, the S11 value of the jig is calibrated withthree reference materials (including air) using Eq. (12). Theprocedure for S11 calibration with the jig based on substitu-tion of the electrostatic capacitance value determined fromthe equivalent circuit is outlined below.

1. The electrostatic capacitance Cf of the coaxial part isdetermined by comparing the input impedance calcu-lated via EM analysis to the analytical model assumingthe complex permittivity of the sample as εri=1.0 (air).

2. The electrostatic capacitance C0 value for the circularcavity section at each frequency is determined from theabove Cf value, the complex permittivity for each ref-erence material inserted and the reflection constant cal-culated via EM analysis.

3. The theoretical value of the reflection coefficient Γi forRef. 2 (Port 2) with assumed insertion of the three ref-erence materials is determined based on Eq. (11) bysubstituting the complex permittivity for each materialand the Cf and C0 values.

4. The theoretical value of the reflection constant Γi forRef. 2 as determined above and the measured reflectionconstant ρi for Ref. 1 are substituted into Eqs. (6)–(9).

5. EDF, ERF and ESF in the measurement system are deter-mined based on Eqs. (6)–(9).

6. The measured S11 value for Ref. 2 after calibration isdetermined from Eq. (12) by substituting the aboveEDF, ERF, ESF values and the measured reflection con-stant ρmeas for Ref. 1

The procedure for determination of actual electrostatic ca-pacitance is outlined in the next chapter.

3. Quantification of Electrostatic Capacitance at theMeasurement Jig Tip

The capacitance of the coaxial tip is first quantified for cal-ibration of the coaxial line S11 value using a VNA in theabove procedure. To this end, the input impedance assum-ing insertion of the three reference materials with corre-spondence to the analytical model of Fig. 2 is first calcu-lated based on EM analysis via the MM technique. Here,pure water, methanol and air were used as the three standardmaterials as necessary for S11 calibration. Next, for calcu-lation of the reflection constant based on equivalent analy-sis, the calculated values of input impedance for each in-sertion condition for Ref. 2 from the MM technique were

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96IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 2021

Table 1 Determination of Cf with Eq. (14) based on εri = 1.0 − j 0.0

substituted into the left side of Eq. (10). The electrostaticcapacitance Cf and the C0 value of the equivalent circuitshown in Fig. 4 were then determined based on the proce-dure outlined below.

Two capacitances are connected in parallel at the frontof the transmission line expressed by the equivalent circuitas shown in Fig. 4 with correspondence to the analyticalmodel of Fig. 2. Here, Cf and C0 are the electrostatic (fring-ing) capacitances of the coaxial line and the sample inser-tion section. It is also assumed that Cf ≡ εrA · C0 is satisfiedfor εri = 1.0 − j 0.0. The total capacitance of Cf and C0

is then calculated as CT = Cf + εri · C0. Based on the re-sults, the total capacitance at the coaxial tip is defined asCT ≡ Cf + Cf/εrA. Input impedance for Ref. 2 is expressedas ZΓi = RΓi + jXΓi using Eq. (10), and RΓi = 0Ω is satisfiedin the case of εri = 1.0 − j 0.0. Accordingly, ZΓi is simpli-fied to a pure imaginary value, and input impedance can beexpressed as

ZΓi = jXΓi =1

jω ·CT≡ εrA

jω ·C f · (εrA + 1)(13)

Cf is thus expressed as follows by manipulating Eq. (13)with focus on Cf:

C f ≡ εrA

j2 · ω · (1+εrA) · XΓi = −εrA

ω · (1+εrA) · XΓi (14)

The electrostatic capacitance Cf of the coaxial line sec-tion can be calculated via the above procedure. Mean-while, RΓi = 0 is also determined from input impedance(ZΓi = RΓi + jXΓi) based on EM analysis via the MM tech-nique, as the real part of input impedance is 0Ωwith an opencoaxial tip. As a result, ZΓi = jXΓi is satisfied. Cf was thendetermined by substituting the value of ZΓi calculated usingthe MM technique and εrA into Eq. (14). The frequenciesfor calculation were set as 0.50, 1.5 and 3.0 GHz from pastresearch results. The ZΓi [Ω] values for input impedance cal-culated using the MM technique with 2a = 4.10 mm, 2b =1.30 mm, d = 5.00 mm and εrA = 2.05 (Fig. 1) are shown inTable 1. The electrostatic capacitance Cf of the coaxial linesection for each frequency was also calculated as shown inTable 1 by substituting the above ZΓi = jXΓi into Eq. (14).

Next, the electrostatic capacitance C0 at the circularcavity (sample insertion) section was determined from thefringing capacitance Cf value for the coaxial line section asdetermined from the above procedure. For this purpose, thefollowing equation is determined by manipulating Eq. (11)related to the theoretical value of the reflection coefficient Γi

for Ref. 2, the electrostatic capacitances Cf and C0, the lineimpedance Z0 and the dielectric constant of the sample εri

with focus on C0:

Table 2 C0 values based on substitution of ZΓi calculated using the MMTechnique assuming the insertion of pure water in Eq. (15)

Table 3 C0 values based on substitution of ZΓi calculated using the MMtechnique assuming the insertion of methanol in Eq. (15)

C0 =1εri·[

1jω · Z0

(1 − Γi

1 + Γi

)−C f

](15)

In the proposed method, S11 is calibrated by substitutingΓi (the theoretical value of the reflection coefficient forRef. 2 with the assumption of each sample in the jig anal-ysis model) and ρi (the actual measurement value of thereflection coefficient for Ref. 1) into Eqs. (5) to (9). Here,the theoretical value of the reflection coefficient for Ref. 2is calculated using Eq. (11) corresponding to the equivalentcircuit shown in Fig. 4 to shorten the computation time. Theelectrostatic capacitance C0 of the sample insertion part nec-essary for calculation of the reflection coefficient based onthe above equivalent circuit is also calculated using Eq. (15).In [15], the VNA-measured value was substituted as the re-flection coefficient Γi in Eq. (15). Here, the value calcu-lated (exact solution) using the MM technique is substi-tuted into Γi to improve the accuracy of the S11 calibra-tion value. The theoretical value (i.e., the calculated com-plex number) determined using the Debye dispersion equa-tion [11], [20], [21] is substituted as the complex permittiv-ity part εri of Eq. (15) for each sample. Accordingly, ca-pacitance C0 is also calculated as a complex number withits imaginary part uniquely corresponding to the dielectricloss tangent of the sample. Here, pure water (εr1), methanol(εr2) and air (εr3 = 1.0) were the three reference materials.In this study, the complex permittivity of the reference mate-rial used to determine C0 was calculated from the theoreticalvalue using the Debye dispersion equation [11], [20], [21].Moreover, various investigations were carried out with com-plex permittivity calculated using the Debye dispersion for-mula corrected from on past evaluation conducted by the au-thor. Specifically, based on Eq. (27) in Ref. [21], the valuesof ε0 = 37.2, εinf = 4.49 and τ = 4.78 · 10−11 were used tocalculate complex permittivity for methanol at a liquid tem-perature of 25.0◦C based on previous measurements madeby the author [14]. The results of calculation to determineinput impedance ZΓ1 using the MM technique with a condi-tion of complex permittivity εri using the Debye-dispersion

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SHIBATA: S11 CALIBRATION OF CUT-OFF CIRCULAR WAVEGUIDE WITH THREE MATERIALS97

equation [21] at a liquid temperature of 25.0◦C for each fre-quency are shown in Tables 2 and 3. Accordingly, electro-static capacitance C0 at the sample insertion section was cal-culated by substituting the values of Cf, Z0, εri and ZΓi (Γi)into Eq. (15). The results with the insertion of pure waterand methanol are shown in Tables 2 and 3.

The electrostatic capacitance C0 of the sample inser-tion part was also calculated for air (εr3 = 1.0). The to-tal value at the tip of the coaxial line was determined us-ing CT ≡ Cf + εr3 · C0, and Cf ≡ εrA · C0 was assumedfor εr3 = 1.0. Thus, C0 ≡ Cf/εrA was set. The value forthe sample insertion section can thus be immediately deter-mined by substituting the values of Cf and εrA into aboveequation, and the results of calculation to determine C0 foreach frequency with sample insertion of air are shown inTable 4.

The input impedance ZΓi (where i = 1, 2 and 3) forRef. 2 was also calculated using Cf and C0 values deter-

Table 4 C0 values based on the assumption of an open termination con-dition (εr3 = 1.0)

Table 5 Input impedance with the complex permittivity values in Ta-ble 2, Cf and C0 substituted into Eq. (11) (pure water)

Table 6 Input impedance with the complex permittivity values in Ta-ble 3, Cf and C0 substituted into Eq. (11) (methanol)

Table 7 Input impedance with the complex permittivity values in Ta-ble 4, Cf and C0 substituted into Eq. (11) (air)

mined via the above procedure. Here, pure water, methanoland air were assumed as reference materials for jig inser-tion. The input impedance ZΓi for Ref. 2 was calculated bysubstituting the values of Table 2–4 for complex permittiv-ity and the values of Cf and C0 into Eq. (11). These valueswere compared with those from the MM technique (see Ta-bles 5 to 7). The values calculated from Eq. (11) correspondexactly to those of the MM technique, indicating that inputimpedance on the front surface of the sample can be accu-rately calculated by substituting Cf and C0 for the equivalentcircuit as determined from Eqs. (14) and (15) into Eq. (11)with a coaxial-feed type cut-off circular waveguide as withthe measuring jig.

4. Verification of S11 Calibration Accuracy

The validity of reflection coefficient Γcorr calibration basedon Eqs. (6)–(15) via the procedure described in Sects. 2and 3 was verified at frequencies of 0.50, 1.5 and 3.0 GHzwith pure water, methanol and air as reference materialsat a liquid temperature of 25.0◦C. Here, dielectric constantsetting is required in calculation of the theoretical reflec-tion coefficient Γi for the reference material. The calculatedvalue from the Debye dispersion equation [20] was thus setfor pure water, the equation corrected from the value mea-sured by the author [14] was set for methanol, and the the-oretical value (1.0 − j0.0) was set for air (open) as shownin Tables 2–4. The dimensions and electrical constants ofthe analytical model as shown in Figs. 1 and 2 were set as2a = 4.10 mm, 2b = 1.30 mm, d = 5.00 mm and εra = 2.05.The theoretical reflection constant Γi based on the equiva-lent circuit for Ref. 2 with the insertion of each referencematerial and setting of the above dielectric constant εri wasused based on extraction from the values calculated usingEq. (11) (Tables 5 to 7). Meanwhile, the S11 value at the tipof the coaxial cable connected to the VNA was calibrated us-ing a general SOL (short, open and loaded) calibration kit,and the jig shown in Fig. 1 was connected to the tip of thecable for actual S11 measurement. The reflection constanton the SOL calibration plane (Ref. 1) for substitution into ρi

(where i = 1, 2 and 3) in Eqs. (6)–(9) (as necessary for S11

calibration at the front of the sample (Ref. 2) using the mea-surement system) was measured in the frequency range of0.50 to 3.0 GHz with pure water, methanol and open termi-nation conditions. Results of input impedance measurementat 0.50, 1.5 and 3.0 GHz are shown in Table 8.

Table 8 Input impedance measurement values with reference materialinsertion (25.0◦C) for the SOL calibration plane (Ref. 1) in S11 calibration

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98IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 2021

Table 9 Input impedance measurement values for the SOL calibrationplane (Ref. 1) for S11 calculation at the front of the sample (Ref. 2)

Input impedance on the SOL calibration plane (Ref. 1)was also measured for the tip of the jig with open, purewater, methanol and ethanol as unknown materials forsubstitution of the value as the reflection constant (ρmeas)in Eq. (12) to calibrate S11 at the front surface of the sam-ple (Ref. 2) under various conditions after jig mounting (Ta-ble 9), and S11 calibration for the sample front of the jigwas performed using these values. Here, the relationshipbetween complex permittivity estimated using the proposedmethod and the accuracy (uncertainty) of input impedancemeasurement values was examined. As an example, thevariation of measured input impedance with respect to Zin =

2.0416 − j 106.54 at a frequency of 0.50 GHz with pure wa-ter inserted as shown in Table 9 was first considered. Forthese sample insertion conditions, variations of 0.05 for thereal part and 0.2 for the imaginary part are assumed dueto the uncertainty (accuracy) of the VNA used in measure-ment. The variation in the estimated value of complex per-mittivity (78.50 − j 1.922) associated with the variation inthe measured value of Zin was calculated as an inverse prob-lem via the MM technique. The results showed changes of0.187 in the real part and 0.054 in the imaginary part. Thereal part of complex permittivity also changed by 0.098 andthe imaginary part by 0.002 with the variation of the outer-conductor’s inner diameter (2a) of 0.05 mm in Ref. [4]. Ac-cordingly, complex permittivity in each table was unified tofour significant digits for both the real and imaginary parts.Input impedance was also unified to five significant digitsfor both parts.

S11 at the front surface of the sample (Ref. 2) with thejig for permittivity measurement attached to the tip of thecoaxial cable of the measurement system was calibrated us-ing the input impedance value measured on the SOL cal-ibration plane (Ref. 1) as described above. Here, the the-oretical input impedance in Ref. 2 converted to the reflec-tion coefficient Γi with pure water, methanol and open con-ditions calculated using Eq. (11) (Tables 5 to 7) was firstsubstituted into Eqs. (6) to (9). Input impedance measuredon the SOL calibration plane (Ref. 1) converted to the re-flection coefficient ρi with pure water, methanol and openconditions on the sample front (as required for S11 calibra-tion of the jig) (Table 8) was also substituted into the ρi partof Eqs. (6) to (9). EDF, ESF and ERF, representing the er-ror term of the measurement system and the auxiliary func-tion γ of the above values, are then calculated (as required

Table 10 Input impedance at the front of the sample (Ref. 2) after cali-bration with three termination conditions (25.0◦C)

for S11 calibration at the front surface of the sample in thejig). Moreover, input impedance measured on the SOL cal-ibration plane (Ref. 1) converted to the reflection coefficientρmeas on the sample front (as required for S11 calibration ofthe jig) with pure water, methanol and ethanol inserted asunknown materials (Table 9) was substituted into the ρmeas

part of Eq. (12). The reflection coefficient at the front ofthe sample after calibration (Ref. 2) under each terminationcondition was thus calibrated as Γcorr using Eq. (12) at eachfrequency from the above procedure. The measured reflec-tion constants Γcorr after calibration based on Eqs. (5)–(12)at frequencies of 0.50, 1.5 and 3.0 GHz and a liquid tem-perature of 25.0◦C were then verified. The input impedancemeasurement results for various liquid types after calibra-tion with the three materials are shown in Table 10, whichalso indicates measured values after SOM calibration (short,open and reference material (pure-water)) conditions. Theerror of the results based on Eq. (12) was within 0.02% withpure water as the unknown material, 2.0% with methanoland 1.1% with air (open). Comparison of measured inputimpedance after calibration with the three reference mate-

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rials and insertion of methanol with the results obtainedafter SOM calibration indicated a slight difference for thereal part at 3.0 GHz. This may be attributed to variationsobserved in repeated measurement of S11. Errors in inputimpedance measurement after calibration based on Eq. (12)were also within 2.0% with ethanol as the unknown mate-rial, which differed from outcomes observed with the refer-ence materials. These details indicate that input impedancecan be calibrated at a calculation accuracy within 2% evenwith various liquids assumed as unknown materials usinga VNA with the proposed method. The results showed cali-bration values close to those observed from SOM conditionswith the three reference materials. In addition, realizationof a short condition in a coaxial feed-type cut-off circularwaveguide is challenging. Specifically, the measured valueof S11 after calibration is affected by the unstable nature ofelectrical contact with the coaxial tip with the short elementin the jig with S11 calibration based on SOM. Here, insta-bility factors relating to short termination with placementin the cut-off circular waveguide are eliminated by S11 cal-ibration with three reference materials and no short termi-nation. Such calibration is considered to enable measure-ment of permittivity with higher accuracy than SOM-basedcalibration.

5. Dielectric Measurement with Various Liquids

The dielectric constants of various liquids were estimated asan inverse problem based on comparison of 1. the S11 valuemeasured with an unknown material in the jig, and 2. thatcalculated using the MM technique with a similar analyticalmodel [4] from input impedance measured with liquids inthe jig after S11 calibration at the front of the sample usingthree termination conditions. The effectiveness of the pro-posed S11 calibration method was verified by comparing theabove estimated values with otherwise obtained outcomesafter SOM calibration [14] and the theoretical value fromthe Debye relaxation equation [11], [14], [20], [21]. The re-sults of dielectric constant estimation for pure water aftercalibration are shown in Table 11 (a). Values estimated asan inverse problem via the MM technique after calibrationwith the three reference materials were also compared withtheoretical values obtained using the Debye dispersion for-mula, with results showing an exact match for all frequen-cies. The results from estimation as an inverse problem viathe MM technique after SOM calibration were also com-pared with those calculated using the Debye dispersion for-mula, with differences of no more than 1.5% for all frequen-cies. This is attributed to the fact that the calibration proce-dure for S11 based on the three reference materials and SOMboth involved the complex permittivity of pure water calcu-lated using the Debye dispersion formula. The estimated di-electric constants of methanol (Table 11 (b)) also indicate anexact match between values estimated after calibration withthe three reference materials and calculated using the Debyedispersion equation. This is attributed to the fact that cali-bration for S11 based on these materials involved the com-

Table 11 Results of complex permittivity estimation for various liquids

plex permittivity of methanol calculated using the Debyedispersion formula. Values estimated as an inverse prob-lem via the MM technique after calibration with the threereference materials were also compared with values esti-mated as an inverse problem via the MM technique after

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100IEICE TRANS. ELECTRON., VOL.E104–C, NO.2 FEBRUARY 2021

SOM calibration and theoretical values obtained using theDebye dispersion formula. The values showed differencesof no more than 1.4% at all frequencies. Estimation resultsfor the dielectric constant of ethanol are shown in Ta-ble 11 (c). In this case, the complex permittivity of ethanolwas also estimated via the coaxial-probe method [12], [13].Values estimated as an inverse problem via the MM tech-nique after calibration with the three reference materialswere compared with those estimated as an inverse problemvia the MM technique after SOM calibration. The valuesshowed differences of no more than 2.01% for all frequen-cies. However, differences among values were found to in-crease with frequency. Next, values estimated as an inverseproblem via the MM technique after calibration with thethree reference materials and SOM calibration were com-pared with those estimated as an inverse problem via thecoaxial probe method [12], [13]. The values showed differ-ences of no more than 5.83% for the real part for all frequen-cies. However, differences among values for the imaginarypart were found to increase with frequency. However, theclose agreement between estimation values after calibrationwith the three reference materials and those after SOM cali-bration indicates the validity of the proposed S11 calibrationand permittivity estimation.

6. Conclusion

This study involved verification of an S11 calibration methodfor jigs to improve measurement accuracy in the estimationof dielectric constants from measured S11 values with var-ious liquids in an open-ended cut-off waveguide. Specifi-cally, termination conditions with three reference materialswere used for calibration at the front surface of the mate-rial for the jig with the material inserted for estimation ofthe complex permittivity of various liquids. Moreover, theelectrostatic capacitance for the analytical model unique tothe jig was quantified by substituting the reflection constant(calculated using the mode-matching (MM) technique) intothe equivalent circuit, assuming the sample liquid in the jig.With pure water, methanol and air as the reference materi-als, S11 was calibrated at the front of the sample in the jigwithin the frequency band of 0.50–3.0 GHz, and S11 wasmeasured at the front of the sample with various liquids inthe jig after calibration. The validity of the calibrated S11

values obtained with the proposed method was verified viacomparison with the S11 value measured after SOM cali-bration conditions. S11 at the front surface of the samplewas measured with various liquids in the jig after calibra-tion with three reference materials, and the dielectric con-stants of various liquids were estimated from the above S11

based on an inverse problem approach involving comparisonwith the S11 value calculated using EM analysis via the MMtechnique. The results were compared with the permittivityvalues estimated as an inverse problem after SOM calibra-tion conditions and similar, with results showing favorableagreement of values determined with each method. Futurework will involve evaluation of actual liquids and their tem-

perature dependence along with extension of the methodto examination of liquids in the millimeter range. Round-robin testing at different institutions is also necessary inassociation with standardization of this method.

Acknowledgements

This work was partly supported by a Grant-in-Aid forScientific Research (No. 20K04522; Establishment of aBroadband Dielectric Measurement Method for Liquids inTemperature-Change Environments for Synthesis of Func-tional Materials) from the Japan Society for the Promotionof Science (JSPS).

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Kouji Shibata was born in Shimada City,Shizuoka Prefecture, Japan, in 1970. After grad-uating from the Engineering Department at theKanazawa Institute of Technology in Ishikawa,Japan, in 1993, he took up employment withSPC Electronics (Shimada Physical & ChemicalIndustrial) Co., Ltd. in Chofu, Japan. His rolesthere included designing and developing passivecircuits such as filters, couplers, diplexers andantennas in the microwave/millimeter band. In2001 and 2004, respectively, he completed the

Master’s and Doctoral Programs of Aoyama Gakuin University GraduateSchool in Tokyo, Japan, and holds Doctor of Engineering status. In 2004he took up a position as a lecturer at Hachinohe Institute of Technology inJapan and became an associate professor in 2015. He is currently engagedin research on electrical constant measurement for passive components inthe high-frequency band and the development of a small sensor informa-tion mobile Internet communication system using an ARM microcomput-ers running on Linux.