Transmission lines of various types, such as microstrip lines, coplanar waveguides and hollow waveguides, have been used to measure or characterize material properties, including dielectric and magnetic properties. The materials can be in solid, liquid or gas phases. These materials can be placed on transmission lines, in direct contact or with no direct contact. For liquids, microfluidic and nanofluidic channels are promising to be powerful methods for real-time and in-situ measurement. Coated with absorbing materials, such as polymers, can also be performed for high sensitivity measurements, including gas measurements. In addition to significantly reducing sample volumes in traditional dielectric spectroscopy measurements, such as studying the structure and dynamics of protein and polymer, measuring cells in suspension, developing drugs, characterizing petroleum fluids and biodiesel, evaluating food and beverage quality, and analyzing biopharmaceutical processes, the method can enable real-time monitoring of liquids and particle-suspensions.
In all the measurements, however, calibrations are necessary in order to remove measurement uncertainties so quantitative material properties can be obtained. The calibrations can be performed with standard devices, such as Matching Load, Open and Short, which have pre-determined electrical impedance values, or reference materials, which have known properties. Accurate calibration is especially important when material volume is small, such as minute amount of liquids in microfluidic devices, or the targeted material property change is small. Accurate removal of the effects of measurement cables, connectors and test fixtures as well as operation uncertainties, such as cable connection repeatability, is necessary but challenging and inconvenient.
Many calibration techniques have been developed. Thru-Reflect-Line (TRL) is considered the most accurate calibration method and it only requires the single Line standard that has an accurate characteristic impedance, in addition to two approximately known standards. The multiline method uses redundant Line standards to minimize the effects of random errors, including variations from Line fabrications. Thus, calibration accuracy and bandwidth are improved over single Line TRL method. These methods, among others, have been adopted for microwave microfluidics applications. However, the use of standard components requires multiple connection-disconnection operations, which could result in significant measurement uncertainties that could be especially important for small volume samples. The single-connection method addresses the multi-connection issue, but multiple reference materials, such as air and water, are needed. As a result, measurement accuracy depends on reference quality. In addition to measurement complications and costs, the need for reference materials or standard calibration components makes it difficult for real-time and in-situ applications, such as inline process monitoring where reference materials are not available or the calibration operation is cumbersome. Therefore, self and auto-calibration methods are desired. There are a few reported self-calibration methods or “calibration-independent” methods. Our previous studies show that by use of a reservoir, the property of liquids can be quantitatively measured without external calibration standards or reference materials. Nevertheless, the method is inconvenient since accurate measurement of liquid volumes is necessary. At the same time, the method is difficult to use for solid or gas measurement. The single-length method uses a single measurement fixture to avoid additional parasitic elements that would produce errors in multi-line or multi-length efforts. Nevertheless, the method requires a reasonable initial guess of the sample dielectric constant for root-searching algorithm to work. The guess may be difficult when measuring unknown liquids. The calibration-independent methods use either air as a reference material or the material-under-test for self-reference. But multiline or repeated connection-disconnection operations are needed therein. Thus, a need exists for a simple methodology that can quantitatively measure material properties accurately.
The aspects and advantages of the invention will be set forth in part in the following description, or may be obvious from the description, or may be learned through practice of the invention. One exemplary aspect of the present disclosure is directed to broadband measurement of liquid permittivity without using liquid reference materials or calibration standards. The method uses a single transmission line and a single microfluidic channel which intercepts the line twice. As a result, two transmission line sections are formed where intercepts occur. The lengths of the two transmission line sections can have a given ratio, such as 2:1, for convenient material property extraction from measurements. A plurality of measurements can be made with a vector network analyzer (VNA) or a device that has a transmitter and a receiver and configured for scattering parameter measurements. The two transmission line sections can be empty, or one is filled with liquid under measurement (LUM), or both are filled. A unique algorithm with closed-form formulas can be used to obtain quantitative liquid properties, such as permittivity or permeability. In another aspect, two separate microfluidic channels can be used in conjunction with a single transmission line. Then, the two channels can be filled with liquid or gas which are to be measured. In yet another aspect, solids, including films, can be characterized when the transmission line section ratio, such as 2:1 mentioned above, is satisfied.
The present method also relates to the use of nanofluidic channels for material property measurement. Additionally, the method can involve using interferometry approach to couple the transmission line to a VNA for high sensitivity measurement.
A full and enabling disclosure of the present invention, including the best mode thereof, directed to one of ordinary skill in the art, is set forth in the specification, which makes reference to the appended figures, in which:
Repeat use of reference characters throughout the present specification and appended drawings is intended to represent same or analogous features or elements of the invention.
Reference now will be made in detail to embodiments of the invention, one or more examples of which are illustrated in the drawings. Each example is provided by way of explanation of the invention, not limitation of the invention. In fact, it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the scope or spirit of the invention. For instance, features illustrated or described as part of one embodiment can be used with another embodiment to yield a still further embodiment. Thus, it is intended that the present invention covers such modifications and variations as come within the scope of the appended claims and their equivalents.
Generally, the present application relates to automatic and self-calibration of devices for quantitative material measurement. The device described herein simultaneously addresses the need for calibration standards or reference material and the uncertainty of multiple connections. In actual embodiment, the transmission line does not need to be straight. Any type of transmission lines, including waveguides, can be used. The materials to be measured can be solid, such as thin films, gas, such as volatile organic chemicals (VOC, which can be absorbed with polymers for stronger signals), and liquids, including liquids with suspended particle.
In operation, a vector network analyzer (VNA) can be configured to measure the four scattering parameters or S-parameters (S11, S12, S21, S22), under three different states: there is no material-under-measurement (MUM, e.g. liquid), there is MUM on one transmission line section, and there is MUM on both transmission line sections. Then, the S-parameters are transformed to ABCD matrices. After processing the ABCD matrices, the propagation constant of the MUM line section can be calculated with analytical formulas when the length ratio of the two line-channel sections is 2:1 (or 1:2). When the ratio is not 2:1, numerical root-searching algorithms can be used to obtain the propagation constant of the MUM line section. The use of two line-channel sections, instead of one, can facilitate the searching process. Finally, the permittivity or permeability of MUM can be extracted by use of geometry and material specific models.
Referring to the drawings,
Full S-parameters for the three states can be recorded in a single-connection measurement while the vector network analyzer performs measurement operations continuously.
Referring to the drawings,
Referring now to
Referring now to
The two TL sections have the same cross section geometry, thus identical propagation constant, γI=γII=γ=α+jβ, and characteristic impedance ZI=ZII=Z when air or MUM filled both sections and when MUM is at the same temperature as the system in
M
Left
M
i
I
M
Center
M
i
II
M
Right
=M
i (2)
where subscript i denotes one of the three states of sections 202, 206.
At (700), the measurement procedure for an exemplary embodiment in the present disclosure is demonstrated. The measured scattering parameters of the device in three states are described as the following:
1) At (702), both section 202 and section 206 are full of air.
M
Left
M
air
I
M
Center
M
air
II
M
Right
=M
1 (3)
2) At (704), section 202 is filled with MUM while section 206 with air.
M
Left
M
liquid
I
M
Center
M
air
II
M
Right
=M
2 (4)
3) At (710), both sections 202, 206 are full of MUM.
M
Left
M
liquid
I
M
Center
M
liquid
II
M
Right
=M
3 (5)
Multiply matrix M1 (M2) by the inverse matrix of M2 (M3), we obtain:
M
Left
M
air
I(Mliquid)−1(MLeft)−1=M1M2−1 (6)
(MLeftMliquidIMCenter)MairII(MliquidII)−1(MLeftMliquidIMCenter)−1=M2M3−1 (7)
Notice that M1M2−1(M2M3−1) and MairI(MliquidI)−1(MairII(MliquidII)−1) are similar matrices. According to trace matrix theory, we can obtain:
For generality, we define the length ratio of section 202 and section 206 is always larger or equal to 1, i.e.
After collecting the S-parameters of the first two states, we need to determine if the length ratio is equal to 2 at (706). For the case
at (708), root-searching algorithm techniques can be used to solve eq. (8) or (9) for γliquid. For the case
at (710), the S-parameters of the third state allows the removal of term
in eqs. (8) and (9) by using the sums of arguments rule of hyperbolic function:
Since
can be calculated with eq. (13) below when device dimensions and air permittivity are known, eq. (10) can be considered as a quadratic equation of
Then, the transmission-line propagation constants can be obtained from the measured S-parameters in three states with the following formulas at (712):
where γ1 and γ2 are two eigenvalue solutions from
They describe and incident and a reflected wave with γ1=−γ2. Furthermore, the physically meaningful propagation constant needs to be identified from γliquid1,2 and γliquid,21,2. Some educated, but often obvious, rules can be exploited from the obtained and |α| and |β|. For a reasonable γ solution, its αliquid is expected to be larger than αair and have the same sign as βliquid for each frequency.
With the obtained γ values, MUM permittivity can be obtained by use of geometry and material specific models at (714). Many of which are available in literature, such as the following one:
where c is the speed of light in vacuum, εeff is the effective permittivity, ε1 is the relative permittivity of MUM, and q and C0 are constants that can be derived from conformal mapping (CM) or single layer reduction techniques. Conductor loss (αc) can also be considered for better accuracy.
The equations to calculate γ from measured S-parameters are applicable to any type of transmission lines even though different transmission lines have different models to extract MUM permittivity from γ.
Referring to
Referring to
to describe spectrum accuracy, where N is the number of measured frequency points over the spectrum.
Referring to
Referring now to
Experimental Measurement
A coplanar waveguide (CPW) with two microfluidic channels in
In embodiment I, where the two channels are not connected together, de-ionized (DI) water, methanol, ethanol and 2-propanol (IPA) from Sigma-Aldrich (US), are measured separately. For each of the sample liquids, the S-parameters of the three states are obtained. Each measurement is repeated three times. The measured data are then processed by use of eqs. (11) and (12) to obtain γliquid. The complex permittivity of the MUM is obtained from eq. (5).
In embodiment II, where the two microfluidic channels are connected together with a silicone tubing to form a single channel, DI water and IPA are measured in succession. The 100 mm long tubing has a 0.51 mm inner diameter and provides 60s delay time. The obtained S parameters, such as S21 magnitude, are plotted in
In addition to measuring material properties, the present methodology has significant applicability in the development of portable, quantitative and fast RF/microwave probes that are easy to operate.
Such probes can be used to characterize various materials in-situ and on-line for real-time monitoring.
While the present subject matter has been described in detail with respect to specific embodiments thereof, it will be appreciated that those skilled in the art, upon attaining an understanding of the foregoing may readily produce alterations to, variations of, and equivalents to such embodiments. Accordingly, the scope of the present disclosure is by way of example rather than by way of limitation, and the subject disclosure does not preclude inclusion of such modifications, variations and/or additions to the present subject matter as would be readily apparent to one of ordinary skill in the art.