Proceedings of the 40th European Microwave Conference

New Method for Dielectric Properties Characterization of Powder Materials: Application to Silicon Carbide
Q. Lu, L. Dubois, E. Paleczny, J-F. Legier, P-Y. Cresson, T. Lasri
Institut dElectronique, de Microlectronique et de Nanotechnologie UMR CNRS 8520, Avenue Poincar B.P. 60069 59652 Villeneuve dAscq Cedex France
tuami.lasri@iemn.univ-lille1.fr Abstract This article presents an original method of materials characterization. Our method is used for broad-band (30MHz-6GHz) determination of the complex dielectric permittivity of powder materials. This technique is based on the measurement of S parameters of two microstrip lines partially loaded with micrometric powder of silicon carbide (SiC). The results exhibit a good agreement with the very few other published values found in the literature. This method is investigated in the frame work of the study and realization of composite materials for microwave sintering operations.

I. INTRODUCTION The new materials of composite structures with high complexity, functionality and flexibility are more and more required for industry. They present a large interest for many industrial sectors (ceramics, polymers, industry of glass). In order to optimize their fabrication, it is important to evaluate their physical properties from the point of electromagnetic theory, which means dielectric permittivity and magnetic permeability. The nature of materials used for the realization of these composite materials, the size of the grains, the form, the arrangement, and the degree of compaction as well as the procedure of sintering will define the properties of the final material (solidity, state of surface, electrical and thermal conductivity, density) [1]. These parameters influence a lot the dielectric permittivity. Although, the lack of papers currently dealing with the field of powder materials characterization is observed, the exact knowledge of material permittivity is essential in the study of physical phenomena which govern interactions between electromagnetic waves and the tested material. Characterization of materials properties at microwave frequencies has a long history, dating from the early 1950s. Nowadays, the measurements of complex dielectric properties are classified in two different techniques: nonresonant methods (reflection method and reflection/transmission method) and resonant method (resonator method and resonant-perturbation method). Among these techniques, we use reflection/transmission methods, which have the significant advantage of application for wide frequency band. In this paper, the measurement cells using microstrip lines for the broad-band characterization of solid materials as well as powder materials are presented. We introduce the general

principle to obtain the complex dielectric permittivity r* of powder material on two steps: First, in our protocol, S - parameters are intermediate ones from which we extract the complex propagation constant of the partially loaded guiding structure with the help of home made de-embedding software [2]. All the widths and thicknesses, which are previously measured, act as data entries in our numerical tool based on the spectral domain approach (SDA) [3] [4] [5]. Real and imaginary parts of the dielectric permittivity of the test material are changeable parameters. Indeed, they are automatically adjusted, for each frequency, in such a way that the measured complex propagation constant matches the eigen value of our numerical problem which is the calculated complex propagation constant, as we know. After making a brief introduction of our method in the second section of the paper, the part III presents the simulation with home made and commercial software based on full-wave EM analysis. Finally, the section IV provides the application of this new measurement cells for broad-band characterization and gives results for the dielectric permittivity of silicon carbide powder and for solid material such as well known plexiglass. II. DESCRIPTION OF THE METHOD The determination of the complex dielectric permittivity r* with this measurement technique consists of two basic steps. The first one relies on the extraction of the propagation constant from S - parameter measurement through a deembedding procedure. In the second step, propagation constant matching procedure is optimized to give the complex permittivity of the material under test. A. The method of determination of the propagation constant The propagation constant for the fundamental mode of a uniform microstrip line, =+j, is not measured directly. , are the attenuation in nep/m and the phase constant in radian/m respectively. However, various techniques allow this determination from measurements of S - parameters by using a vector network analyzer. The work published by Bianco and Parodi proposes a skilful method of extraction of the propagation constant based on S parameters measurements of two

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microstrips lines witch differ only by their longitudinal dimension [6]. In this technique, two uniform microstrip lines of different lengths L1 and L2 (L1<L2) are needed, and also two identical launchers LA, LB for the connection to the measuring instrument. Obviously, it is requested that the propagation must be done over one mode (the quasi-TEM mode of the microstrip) without any other higher modes. The two microstrip structures are inserted between the launchers (Fig 1). In this case, the launchers-microstrip transition are normalized, Z0=50. Thanks to certain properties of matrix arrangement, the method we used will give the propagation constant which does not depend upon the launcher parameters, as soon as, they are identical on both sides of each port. Therefore, it is possible to extract the propagation constant (=+j) of the segment of line L by subtracting the influence of the transitions.
L1 L1/2 Line 1 LA w L1/2 LB

So, as soon as of this segment is determined, we obtain the r* of our test sample because all the other geometrical and physical parameters of our line L are well known. In the next section of the paper we present the protocol employed to extract the complex permittivity. B. The method of determination of the dielectric permittivity We should mention that the relations between the propagation constant and the permittivity r* of material under test are not analytic. The calculation of r*=r-jr as a function of the calculated needs a numerical analysis method. We have developed home made de-embedding procedure and full wave electromagnetic software, to retrieve the complex permittivity. The spectral domain approach (SDA) is used for the hybrid mode analysis of the microstrip device. The procedure is given in Fig 3.
Convertor Bianco & Parodi

measured calculated
+ -

Same transition L1/2 Line 2 LA w

L2 L1/2

Same transition

measured-calculated
yes stop

=0
LB

r* material

no Choice of a new physical parameter (r, tan)

r *
L=L2-L1

Fig. 1 Microstrip structure, lines with different lengths L1 and L2.

is then deduced from the measured Sij,L1, Sij,L2 parameters by the following relation:
2 cosh( L) =
2 2 S12 ,L1 + S12,L2 + S11,L1S22,L2 + S11,L2 S22,L1 S11,L1S22,L1 S11,L2 S22,L2

Calculation of the new propagation constant relative to the new definite physical

SDA

Fig. 3 Flow chart for the complex permittivity determination.

S12,L1S12,L2

The indices L1 and L2 are respectively dedicated to the S parameters relating to line 1 and line 2. Inspired from this method, we may place directly the powder material onto the microstrip lines, hence we can extract the constant of propagation for the line L covered by a certain amount of powder material (Fig 2).
L1 l w LB Sample holder Test sample l Line 1 LA

The software must be considered as an expert one, especially dedicated to dielectric or magnetic characterization; the material being, independently, made of thick or thin solid or powdered layer. So, it gives the complex permittivity or permeability of any layer of finite thickness. Through this procedure, the complex dielectric permittivity (r*=r-jr) of powdered test sample is obtained in a broad frequency band. III. SIMULATION RESULTS High Frequency Structure Simulator (HFSS, ANSYS Inc.) is a very popular commercial tool that can provide very accurate results for 3D electromagnetic field simulation of high-frequency and high-speed components. The software is based on the resolution of the Maxwell's equations by the finite element method. The 3D study of the structure makes it possible to take into account the discontinuities of the cell and to calculate the electromagnetic field in any point of the structure [7]. Thus, the simulator determines the [S] parameters matrix distribution of the support as well as the propagation constant. In order to apply the Bianco-Parodi method for our structure and also to find out the effects of the sample holder on the whole structure, we established several models of microstrip lines by means of HFSS (Fig 4). The two

Same transition

L2

Same transition

Line 2

LA l

w l L=L2-L1

LB

Fig. 2 Measurement configuration (two microstrip lines with different lengths L1 and L2 covered by the test sample).

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lines are both designed for Z0=50 to match the cables and the vector network analyzer used to perform the S-parameter measurements. The microstrip lines are specified as RT Duroid5880 (r=2.2, tan=0.0009) for substrate material; copper for the center conductor; plexiglass for the sample holder. The microstrip lines are covered with the sample holder which is filled with the powder. We begin our investigations by considering that the permittivity of the sample is known from Baeraky measurements, ie r*=6-0.5j [8]. This is done to test the robustness of the protocol.
Line 2 Sample holder Sample holder Test sample Test sample Line 1

microstrip line. We can also verify that propagation constant does not depend upon the launcher parameters. The extraction is consequently very well done. Thus, the robustness is confirmed. IV. MEASUREMENT RESULTS Our experimental measurement cells used for this study are presented in Fig 6. Two microstrip lines are made on substrate RT Duroid5880 with thickness=508m, center conductor thickness=17.5m, center conductor width=1.54mm. The two microstrip lines lengths are respectively L1=101.5mm and L2=76mm. The sample holders are made from plexiglass with 5mm thickness. The S - parameters measurements are preformed using a Rhode&SchwarzZVL6 vector network analyzer. In order to compensate for the symmetric and random errors, the network analyzer and cables are calibrated. The test was carried out in laboratory with SiC powder samples (Norton type F100HD); the grain size was approximately 100m and the sample is filled symmetrically in the holder.
Sample holder Test sample: powder of SiC

(a)

Wave port

(b)

Fig. 4 Modeling of the test structure with HFSS (a) 2D view (b) 3D view.

What we do, now, consists in the calculation of the S parameters response of a 3D cell containing line1, and a 3D cell containing line2 with known values. These two data sets named Sij,L1, Sij,L2 are injected in Bianco-Parodi formula in order to extract the propagation constant. We compared this data (,) with those directly given by the 2D FEM analysis (HFSS). Fig 5 shows a very good agreement of the constant propagation (,) between the 3D HFSS simulation associated to Bianco-Parodi de-e-embedding (propagation constant calculated from S-parameters considering Fig. 4.b plus Bianco-Parodi equation) and classical two dimension full wave method (Fig. 4.a). Let us note that the material chosen for the sample holder presents a low dielectric permittivity (r=2.5) and very low losses (tan=0.005).
(Rad/m)
250 200 150 100 50 0 0 1 2 3 Frequency (GHz) 4 5 6

(a)

(b)

Fig. 6 Measurement cell with (a) empty sample holder and (b) filled with SiC powder.

In order to illustrate the experimental results obtained with our broad-band characterization method, we give, in Fig 7 the propagation constant (,) determined with the Bianco-Parodi method. For the tests, we have first considered empty sample holders and then a Plexiglass sample (thickness=15mm) and a layer of SiC powder (thickness=5mm)
(Nep/m)
14 12 10 8

(Nep/m)
10 8

2D HFSS simulated 3D Bianco-Parodi simulated

6 4

measured SiC

2 D HFSS simulated 3D ianco-Parodi simulated

2 0

4 2 0 0 1 2 3 Frequency (GHz) 4 5 6

measured Plexiglass

measured Empty

Fig. 5 Simulated results: comparison between 3D + Bianco-Parodi and 2D HFSS propagation constants (, ) in a frequency band of 0.1 GHz to 6 GHz.

(a)

We clearly see that this kind of sample holder does not perturb the determination of the propagation constant of the

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 (Rad/m)
250 200 150 100 50 0 0 1 2 3 Frequency (GHz) 4 5 6

0,6 0,5

measured SiC measured Plexiglass measured Empty

tan

0,4 0,3 0,2 0,1

SiC Substrate Plexiglass

2 3 4 5 6

0 0 1 Frequency (GHz)

(b) Fig. 7 SiC. Propagation constant measured with Bianco-Parodi method in a frequency band of 30 MHz to 6 GHz  RT Duroid5880, Plexiglass,

(b) Fig. 8 Measured dielectric constant and loss tangent (r, tan) in a frequency band of 30 MHz to 6 GHz  RT Duroid5880, Plexiglass, SiC

Using our hybrid mode analysis (SDA), the dielectric constant and loss tangent can be calculated from the propagation constant data (,). The comparison results are shown in Fig 8. We characterize successfully the dielectric permittivity of Duroid5880 substrate: rsubstrate=2.11-2.16, tansubstrate=0.001-0.005; plexiglass: rplexiglass=2.4-2.6, tanplexiglass=0.01-0.03. The results agree with the measured data from the dielectric constant reference guide [9]. In the case of the SiC powder, we observe an agreement between our measured permittivity and the results obtained for the same material by other laboratory using a different characterization technique (the cavity resonator technique) [7]. We find out that the dielectric permittivity of SiC decreases slightly in the investigated frequency band . Thus, we estimate the value for SiC powder to: rSiC=6-7, tanSiC=0.12-0.2.
9 8 7 6

V. CONCLUSIONS The measurement technique on a broad frequency band (30 MHz to 6 GHz) for powder materials characterization has been developed in this paper. Compared to the data found in the literature, our results present a high accuracy in a large frequency band. From the experimental point of view, our measurements method is fast and easy to implement. The measurement process repeatability has been checked and has shown a high level of confidence. This characterization method that is valid for a very large class of powder materials is also well suited for solid materials (thick or thin). REFERENCES
[1] C. Beaucamp-Ricard, L. Dubois, S. Vaucher, P.Y. Cresson, T. Lasri, and J. Pribetich, Temperature measurement by microwave radiometry: application to microwave sintering, IEEE Trans. Intrum. Meas., vol. 58, no. 5, pp 1712-1719, May 2009. F. Ponchel, J. Midy, J.F. Legier, C. Soyer, D. Rmiens, T. Lasri, and G. Guguan Dielectric microwave characterization of BSTfilm depositedon high resistivity silicon substrate: analysis by 2D tangential finite element method, J. Appl. Phys., accepted for publication, 2010. N. Tentillier, B. Splingart, J.F. Legier, E. Paleczny, C. Legrand, Application des cristaux liquides aux circuits microondes accordables, in 11me Colloque Francophone sur les Cristaux Liquides, Dunkerque, 23-25 septembre 2003. T. Itoh, R. Mittra, Spectral domain approach for calculating the dispersion characteristics of microstrip lines, IEEE Trans. Microw. Theory Tech.,, vol. MTT 21, no. 7, pp 496-499, Jul 1973. P. Pribetich, Contribution ltude dun applicateur microonde de type fente, excit par une ligne microruban, PhD. thesis, Universit des sciences et technologies de Lille, Lille, France, Jun. 1984. B. Bianco, and M. Parodi, Determination of the propagation constant of uniform microstrip lines, Alta Frequenza XIV, no. 2, pp. 107110, Feb. 1976. (2010) The ANSYS, INC. website. [Online]. Available: http://www.ansoft.com/products/hf/hfss T. A. Baeraky, "Microwave measurements of the dielectric properties of silicon carbide at high temperature," Egyptian Journal of Solids, vol. 25, pp. 263-273, 2002. (2010) The RF Cafes website. [Online]. Available: http://www.rfcafe.com/references/electrical/dielectric-constantsstrengths.htm

[2]
SiC

r 4
3 2 1 0 0 1 2 3 Frequency (GHz) 4 5 6

[3]

Plexiglass

[4]
Substrate

[5]

[6]

(a) [7] [8]

[9]

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