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Characterizations of low-loss dielectric material properties, such as dielectric constant
The free-space measurement method is widely utilized for low-loss dielectric characterization at millimeter-wave frequencies and beyond, and this method is nondestructive, noncontacting, and broadband [1], [2], [11], [14]. This technique operates in a similar way to the above-mentioned transmission-line technique and uses the same methods to calculate dielectric constant and loss tangent. The free-space technique calculates the dielectric constant and loss tangent from the reflection and transmission S-parameters measured for a material that is placed between the transmit and receive antennas. Typically, either parabolic mirrors [2] or lenses [1] are employed (between these antennas) to prevent divergence of the beam. Time-domain spectroscopy (TDS) [15], [16] is another popular technique based on free-space measurement. TDS has several appealing advantages, including relatively low cost and the applicability of the measurement technique over a wide frequency range [17]. However, generally, the TDS method is less accurate than vector network analyzer (VNA)-based techniques that provide lower signal-to-noise ratios [3]. Such free-space techniques suffer from two main disadvantages. First, high-precision micrometer positioners are needed to carry out the relevant free-space calibrations that are typically nontrivial [2]. Second, the measurement system usually takes up a large amount of laboratory space [3].
Recently, new commercial material characterization kits (MCKs), developed by SWISSto12, have become available for waveguide frequency bands from 50 GHz to 1.1 THz. This broadband method is effectively a guided free-space approach. During measurement, the material is sandwiched between the two antennas that comprise the test ports of the MCK, as shown in Fig. 1. This minimizes the efforts needed for sample preparation. In contrast to most conventional free-space measurement setups, these MCKs eliminate the need for large parabolic mirrors or lens, and therefore, this significantly reduces the overall size of the measurement system. Note that these MCKs are not ideally suited to measure samples at varying temperatures—in these scenarios, the conventional free-space technique is likely to be more effective. An initial assessment of an MCK was described in [18]. However, only preliminary results were reported in [18], without any in-depth discussions or analyses. This article reports on a comprehensive investigation into material characterization using an MCK at WR-15 band (50–75 GHz). Common low-loss dielectric materials—PTFE, TPX, HDPE, Alumina, Silicon, Astra MT77 [19], and Rogers 3003 [20]—are measured with the MCK and the results are presented and compared with other sources of information. In addition, for PTFE, samples with different thicknesses are prepared, measured, and discussed, to explore the impact of sample thickness on achieved measurement quality. Finally, the uncertainties in the extracted dielectric constant and loss tangent values are calculated and reported. To the best of our knowledge, this is the first time that an in-depth study of material characterization using MCKs has been reported.
Photographs of the WR-15 (50–75 GHz) MCK-based experimental apparatus. (a) Overview of the whole measurement system, comprising VNA, WR-15 extension heads, and the WR-15 MCK. (b) Close-up view of the WR-15 MCK, showing a sample of PTFE sandwiched between the two MCK test ports.
This article is organized as follows. In Section II, the measurement technique is introduced. Section III describes the measurement results for the abovementioned dielectric samples. Section IV presents an uncertainty analysis for the extracted dielectric constant and loss tangent, which is followed by conclusions in Section V.
Fig. 1(a) shows the MCK measurement setup at NPL. A pair of Virginia Diodes Inc. (VDI) WR-15 frequency extenders are connected to a Keysight Technologies N5247A PNA-X network analyzer, enabling measurements of
During measurement, a dielectric material is placed in the gap between the two antennas, which can be gradually opened and closed using a gap adjustment mechanism. Similar to the conventional free-space measurement system, the MCK produces a Gaussian beam that provides plane-wave illumination of the sample [21]. However, compared to a conventional free-space measurement system, the MCK allows the electromagnetic wave to propagate within an enclosed low-loss environment and removes the need for bulky mirrors or lenses.
The gated-reflect-line (GRL) calibration technique [23] is carried out at the ends of the antennas prior to making measurements of S-parameters. The GRL method requires a simple zero-length “Thru” standard and a metallic reflecting plate as the “Reflect” standard [23]. The “Thru” standard is realized by closing the gap between the two halves of the corrugated antennas. The “Reflect” standard is realized by placing a short circuit (a 1-mm-thick metal shim, provided with the MCK) between the two halves of the antennas. Time-domain gating, a useful technique for free-space measurements, is employed here to separate the wanted signals from the spurious reflections generated elsewhere in the measurement system (e.g., due to the connections between the MCK and the test ports of the VNA, and so on). In this article, the time-gating window is set to 400 ps, i.e., the value recommended by the manufacturer of the MCK [21].
S-parameter measurements were taken after the abovementioned calibration. The VNA was set to measure at 501 frequency points with an intermediate-frequency (IF) bandwidth of 50 Hz. No VNA averaging was used for the measurements. All measurements were carried out at a laboratory temperature of 23°C ± 1°C. As with conventional free-space methods or other traveling-wave methods, the dielectric constant (
Seven different kinds of common dielectric material were measured using the MCK over the frequency range 50–75 GHz. These materials are PTFE, TPX, HDPE, Alumina, Silicon, Astra MT77, and Rogers 3003. The latter two are popular low-loss dielectric materials for substrates of millimeter-wave printed circuits.
Software is supplied with the MCK for data analysis, which allows computation of the dielectric constant and loss tangent directly from measured
A further comparison between the MCK software and the NIST precision model was undertaken using two other samples: silicon (of thickness 3.06 mm) and alumina (of thickness 10.18 mm). The results are shown in Figs. 4 and 5, respectively. Again, excellent agreement between these two approaches is achieved. A magnified view of a part of the extracted dielectric constant for silicon (shown in the inset in Fig. 4) shows steps in the results obtained using the MCK software. This is due to the limited numerical precision specified in the MCK software. The comparison of algorithms demonstrates that the results extracted from MCK software are consistent with those obtained using the NIST precision model based on transmission only.
The key equations in the NIST precision model [24] are briefly described next. The absolute permittivity
where
Fig. 6 shows the extracted dielectric constant and loss tangent for Astra MT77 sample (thickness 1.60 mm) and Rogers 3003 sample (thickness 1.50 mm) over the frequency range of 50–75 GHz. Similarly, Fig. 7 shows the extracted dielectric constant and loss tangent for the HDPE sample (thickness 5.97 mm) and TPX sample (thickness 2.81 mm). Tables I and II summarize the results extracted using the MCK. Tables I and II also show the selected values reported in the literature. The values of dielectric constant, presented in Table I, show good agreement between the MCK measured values and the values found in the literature. The values of loss tangent, presented in Table II, also show acceptable agreement, although some of these values from the literature are very close to zero. Apart from the different thicknesses of the samples, sample measurement angle, and test frequency, the differences between our results and values found in the literature may be attributed to factors, such as measurement setup, extraction process, surface roughness of the samples, and differences in sample manufacturing/preparation. The uncertainties in the extracted dielectric constant and loss tangent values may account for these differences. This will be discussed in Section IV.
The extracted dielectric constant and loss tangent values, reported in Tables I and II, are subject to several sources of error. These errors will cause the extracted values to differ from the underlying true values of these quantities. In order to quantify the extent of the difference between the extracted values and the true values, it is useful to provide an estimate of the likely uncertainty in the extracted values.
This section provides the preliminary estimates of the uncertainty due to the main sources of error, which include the insertion repeatability of the sample into the sample holder, the sample thickness, the measurement of the sample thickness, and the measured S-parameters of the sample. These estimates will be used to establish a preliminary assessment of the overall uncertainty of the MCK in the WR-15 waveguide band. This is not intended as a rigorous assessment of uncertainty, as this is beyond the scope of this article—rather, the intention is to provide an indication of the typical size of uncertainty that could be expected for these MCKs.
Random processes contribute to some errors in the extracted results. In this article, we consider two potential sources of such errors: 1) insertion repeatability of the sample, without changing the orientation of the sample in the MCK and 2) insertion repeatability that also includes changing the orientation of the sample with respect to its position in the sample holder. The former evaluation was performed on all samples; the latter evaluation was performed on just two of the PTFE samples of different thicknesses (i.e., 2.96 and 11.95 mm). Six repeated measurements were carried out on each individual sample, for both types of error evaluation (i.e., with and without changing the sample orientation between reinsertions). The two PTFE samples were marked so that their orientation could be changed in a systematic way (i.e., by introducing a rotation of 60° between each reinsertion).
Fig. 8 shows the calculated standard uncertainty in the extracted dielectric constant and loss tangent values, for the first investigation (i.e., for the random errors associated with the repeated measurements without changing the orientation of the sample). The standard uncertainty [34] for the extracted dielectric constant value
Similarly, the standard uncertainty for the loss tangent
The standard uncertainty values shown in Fig. 8 are less than 0.007 for the dielectric constant and less than 0.0008 for the loss tangent, at all frequencies and for all seven dielectric materials.
The investigation into changing the orientation of the two PTFE samples produced standard uncertainties of comparable size to those calculated for PTFE from the repeated measurements shown in Fig. 8. This indicates that the impact of changing the orientation of the PTFE sample in the MCK has negligible additional effect of the extracted values of dielectric constant and loss tangent for PTFE. This may not be the case for other materials (e.g., materials that exhibit some form of inhomogeneity) and so this type of assessment should be considered for all materials measured using the MCK.
In order to quantify the impact of sample thickness on the extracted dielectric constant and loss tangent values, measurements were made on four PTFE samples of different thicknesses: 2.96, 5.99, 8.99, and 11.95 mm. These samples were machined in the NPL workshops using a single PTFE rod and therefore were made from the same batch of material. The wavelength was calculated to be approximately 4.23 mm at 50 GHz, using a value of 2.008 for the dielectric constant of PTFE, as given in Table I. In general, characterization techniques based on free space or transmission line methods require that the samples under test should be thick enough to contain at least 20° of phase at the wavelength
Fig. 9 shows the extracted dielectric constant and loss tangent values for these four PTFE samples. Fig. 9 shows that there is no obvious correlation (i.e., systematic dependence) between the extracted dielectric constant and loss tangent values, and the thickness of the sample is measured. This suggests that this effect can be neglected for this material. This may not be the case for other materials (e.g., materials that exhibit either very high or very low loss) and so this type of assessment should be considered for all materials measured using the MCK.
Part of the procedure for using the MCK requires a measurement of the thickness of the sample being measured. This is achieved using a digital micrometer that is included as part of the MCK. This thickness determination will be subject to error due to the accuracy of this digital micrometer. The digital readout on the micrometer introduces a digitizing error that is effectively half the resolution of the digital readout. For this MCK, the resolution of the micrometer is 0.01 mm and so the uncertainty due to this digitizing error is 0.01/2 mm
The impact due to the uncertainty in the measured sample thickness on the extracted dielectric constant and loss tangent is evaluated by perturbing the measured value for the thickness of the sample by the standard uncertainty and then reextracting the dielectric constant and loss tangent values. The difference between the two sets of extracted values (i.e., those obtained using the original value and the perturbed value for the sample thickness) is considered to represent the uncertainty due to the error in determining the sample thickness.
To illustrate this, the technique has been applied to the 5.99-mm-thick sample of PTFE. The impact of the standard uncertainty in the thickness determination on the extracted dielectric constant and loss tangent is shown in Fig. 10, where the associated standard uncertainty in the extracted dielectric constant and loss tangent is approximately 0.004 and 0.0001, respectively. Fig. 10 also shows the standard uncertainty due to the insertion repeatability (discussed previously) and the measured S-parameters (to be discussed next) for this sample.
The MCK also makes use of measured values for
At WR-15 band, a single, typical, value of standard uncertainty for the measured
The impact of the uncertainty in
As mentioned earlier, this technique has been applied to the 5.99-mm-thick sample of PTFE. The impact of the standard uncertainty in the real and imaginary components of
Having evaluated the standard uncertainty due to each of the main sources of error, these uncertainty contributions can be combined to provide an overall uncertainty in the extracted dielectric constant and loss tangent values.
For
The use of this equation assumes that
Having established a value of
For a given combined standard uncertainty
Fig. 11 shows the expanded uncertainty with a 95% coverage probability
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