Surface acoustic wave resonant sensor
11243189 · 2022-02-08
Inventors
- Aldo Jesorka (Gothenburg, SE)
- Kiryl Kustanovich (Gothenburg, SE)
- Ventislav Mitkov Yanchev (Vratsa, BG)
Cpc classification
G01N2291/0422
PHYSICS
G01N29/022
PHYSICS
G01N2291/0256
PHYSICS
International classification
Abstract
A surface acoustic wave resonant sensor for measuring a sample comprising a single port surface acoustic wave (SAW) resonator comprising an interdigital transducer and at least one reflective grating. The sensor is provided with a region for receiving the sample, said region being in communication with the at least one reflective grating and the IDT is separated acoustically and electrically from the region for receiving a sample such that the IDT is not mass sensitive to the sample. The sensor is especially suitable for bio sensing applications.
Claims
1. A surface acoustic wave (SAW) resonant sensor for measuring a sample, the sensor comprising: a one-port SAW resonator, including an interdigital transducer IDT; and at least one reflective grating; wherein the sensor is provided with a region for receiving the sample, said region being above and in direct contact with the at least one reflective grating, and the IDT is separated acoustically and electrically from the region for receiving the sample such that the IDT is not mass sensitive to the sample.
2. The surface acoustic wave resonant sensor according to claim 1, wherein the SAW resonator is provided with two reflective gratings arranged either side of the IDT.
3. The surface acoustic wave resonant sensor according to claim 1, wherein the at least one reflective grating is interdigitated such that a capacitor is formed at the interface of the region for receiving the sample and the reflective grating.
4. The surface acoustic wave resonant sensor according to claim 1, wherein the at least one reflective grating is adapted to receive a low frequency electric signal of from about 10 Hz to about 10 MHz.
5. The surface acoustic wave resonant sensor according to claim 1, wherein the sensor further comprises a fluidic layer in communication with the SAW resonator, wherein the fluidic layer is provided with a protective cap adapted to inhibit the ingress of the sample to be tested to the IDT, such that sample does not contact the IDT.
6. The surface acoustic wave resonant sensor according to claim 5, wherein the fluidic layer further comprises at least one microfluidic chamber arranged in communication with the at least one reflective grating such that said region for receiving a sample is formed by the at least one microfluidic chamber.
7. The surface acoustic wave resonant sensor according to claim 5, wherein the protective cap in the fluidic layer is provided with a recess such that an air gap is formed above the IDT.
8. The surface acoustic wave resonant sensor according to claim 1, wherein the at least one reflective grating comprises a plurality of thin film members arranged, periodically and substantially parallel to each other.
9. The surface acoustic wave resonant sensor according to claim 8, wherein the plurality of thin film members of the reflective gratings are arranged at a pitch of half a surface acoustic wavelength at resonance.
10. The surface acoustic wave resonant according to claim 1, wherein the SAW resonator is provided on a first surface of a piezoelectric substrate.
11. The surface acoustic wave resonant sensor according to claim 1, wherein an interlayer is provided above and in communication with the SAW resonator.
12. The surface acoustic wave resonant sensor according to claim 1, wherein the SAW resonator employs SH-SAW and/or Leaky SAW propagating along the X-axis of the piezoelectric substrate being selected from one of, Y-cut LiNbO3, 36° Y-cut LiNbO3, 41° Y-cut LiNbO3, 64° Y-cut LiNbO3, 163° Y-cut LiNbO3, 36° Y-cut LiTaO3, 42° Y-cut LiTaO3.
13. The surface acoustic wave resonant sensor according to claim 1, wherein the sample is a liquid sample.
14. A sensor assembly comprising a plurality of surface acoustic wave resonant sensors according to claim 1.
15. The sensor assembly according to claim 14, wherein the sensor assembly comprises a single fluidic layer.
16. A method for physical, biological, and/or chemical measurement comprising: providing a sample to be tested to a surface acoustic wave resonant sensor according to claim 1, providing a high frequency signal of greater than about 100 MHz to the IDT, and/or providing a low frequency signal of about 10 Hz to about 10 MHz, to the at least one reflective grating, measuring at least one shift in resonance frequency, change in amplitude of admittance and conductance near resonance, change in phase of the admittance near resonance, changes in resonator signal time of decay, and/or changes in complex electrical impedance of the SAW resonator.
17. The method according to claim 16, wherein the high frequency signal is provided to the IDT and the low frequency signal is provided to the at least one reflective grating concurrently.
18. A system for measuring a sample comprising: a surface acoustic wave resonant sensor according to claim 1, a high frequency electrical signal generator for providing a high frequency signal of greater than about 100 MHz to the IDT, a low frequency electrical signal generator for providing a low frequency electrical signal of from about 10 Hz to about 10 MHz to the at least one reflective grating.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) These and other aspects, features and advantages of which the invention is capable will be apparent and elucidated from the following description of embodiments of the present invention, reference being made to the accompanying drawings, in which
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DETAILED DESCRIPTION
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(17) The sensor 1 is adapted such that the IDT 8 is not mass sensitive to the sample. The region for receiving the sample 20, and/or the sample, is shielded, that is, it is not in communication with the IDT 8. Further, in the sensor 1, the sample to be measured does not contact the IDT 8. Not in communication as used herein refers to the sample not being in acoustic communication nor electric communication with the IDT 8. That is, the IDT 8 is separated acoustically and electrically from the region for receiving a sample 20. This surprisingly enables reliable measuring of a variety of samples, especially liquid, viscous, and/or conductive samples. In some of the aspects disclosed herein, the sensor further comprises a fluidic layer 2 adapted to inhibit the ingress of the sample to be tested to the IDT 8.
(18) The region for receiving the sample 20, and/or the sample, may be confined to the at least one reflective grating 9.
(19) Confining the region for receiving the sample 20, and/or the sample, to the at least one reflective grating 9, has traditionally not been attempted as reflectors in classic one-port resonators do not contain a lot of energy, but serve to reflect and confine the energy to the resonator IDT. Most sensitivity comes from mass loading of the IDT, reflectors are only to a very minor part involved in the sensing, as they do not contain much energy.
(20) The SAW resonator is provided on a piezoelectric substrate 6. The SAW resonator is provided on a first surface 7 of the piezoelectric substrate 6. The first surface 7 is adjacent to, and in communication with the fluidic layer 2. The SAW resonator is also in communication with the fluidic layer 2.
(21) The single port SAW resonator, formed on the first surface 7 of the piezoelectric substrate 6, comprises an IDT 8 and at least one, such as two, reflective gratings 9. The reflective gratings 9 are provided on laterally opposing sides of the IDT 8, The single port SAW resonator is provided with a single IDT 8, that is, not a plurality of IDTs. The sensor 1 is not provided with an input and output IDT pair.
(22) The IDT 8 is formed by a plurality of metallic thin film members 81, such as bars, arranged in an array. The thin film members 81 of the IDT 8 are arranged in substantially parallel alignment to each other. The IDT 8 has a longitudinal axis which is substantially parallel with longitudinal axis of alignment of the thin film members 81 of the IDT 8. The array of thin film members 81 of the IDT 8 extends laterally towards the reflective gratings 9.
(23) The reflective gratings 9 are also formed by a plurality of metallic thin film members 91, such as bars, arranged in an array. The thin film members 91 of the reflective gratings 9 are arranged in substantially parallel alignment to each other. The array of thin film members 91 of the reflective gratings 9 extends laterally in alignment with the lateral axis of the IDT 8. Each of the thin film members 91 of the reflective gratings 9 extend substantially perpendicular to the alignment of the array. As shown in
(24) The thin film members 81, 91 of the IDT 8 and the reflective gratings may be described as being a periodic strip grating.
(25) The thin film members 81, 91 of the IDT 8 and the reflective gratings 9 may comprise a suitable metal patterned on the first surface 7 of the piezoelectric substrate 6. Such suitable metals include for example, Au, Pt, Al, Cu. The thin film members 81, 91 may be formed by a plurality of deposited metals, for example, the thin film members 81, 91 may comprise a first adhesion layer of Ti, a second load layer of Au, and a final adhesion and capping layer of Ti. The provision of the adhesion layers increases adhesion of any subsequently provided layers.
(26) As can be seen in
(27) The thin film members 81, 91 of the IDT 8 and the reflective gratings 9 may be arranged in a row.
(28) As shown in
(29) The IDT 8 may have a periodical array of thin film members 81 with a pitch p.sub.0≈V.sub.SAW/(2.sub.f0), where V.sub.SAW is the phase velocity of the surface acoustic wave, while f0 is the resonance frequency.
(30) The thin film members 91 of the reflective gratings 9 form a periodic grating structure with a pitch of p.sub.0 as described above. The thin film members 91 of the reflective gratings may be electrically connected as shown in
(31) In the arrangement of reflective gratings 9 shown in
(32) The at least one reflective grating 9 may be designed such that energy at resonance is increased within a portion of the reflective grating 9 adjacent the region for receiving the sample 20. This may be achieved by reducing the reflectivity to transmitted waves of a portion of the at least one reflective grating 9 relative to adjacent portions. That is, a portion of low reflectivity is provided between two portions of normal or increased reflectivity. One technique for reducing the relative reflectivity of a portion of the at least one reflective grating 9 is to decrease the metallisation ratio of the low reflectivity portion. Such a design is shown in
(33) The fluidic layer 2 is a structured fluidic layer for inhibiting the ingress of sample to the IDT 8. The fluidic layer 2 may comprise at least one microfluidic chamber 3 in communication with feeding channels 4. The fluidic layer 2 may provide a structure for the provision of sample to the region of the resonator for receiving a sample. The fluidic layer 2, and in particular the at least one microfluidic chamber 3, is arranged in communication with the one port SAW resonator. At least a portion of the at least one microfluidic chamber 3 is provided above a portion of the reflective gratings 9. The at least one microfluidic chamber 3 may be provided such that it covers a portion of the IDT 8. An example of such an arrangement can be seen in
(34) As shown in
(35) The fluidic layer 2 may be provided with a region acting as a protective cap 5 which is in communication with and ensures that neither the microfluidic chambers 3, nor the feeding channels 4 are in communication with the IDT 8. The protective cap 5 is provided adjacent to the at least one microfluidic chamber 3. The protective cap may be provided adjacent and between two microfluidic chambers 3.
(36) The fluidic layer 2 may be formed by a polymer, glass or any suitable known material for the provision of a structured fluidic layer. The fluidic layer 2 in the sensor 1 as described in the experimental section comprise the polymer polydimethylsiloxane (PDMS).
(37) In the arrangement shown in
(38) Whilst the description has focused on a sealed system where a sample to be measured is provided via the microfluidic chambers 3 and microfluidic channels 4 this is not necessary for the sensor 1 to function. An open arrangement is shown in
(39) As can be seen in
(40) The piezoelectric substrate 6 comprises either a bulk piezoelectric crystal, for example, LiTaO.sub.3, LiNbO.sub.3, Quartz etc. or thin piezoelectric film composite substrate formed by a piezoelectric thin film layer, for example, ZnO, AlN, LiTaO.sub.3, LiNbO.sub.3, PZT etc. deposited or transferred on top of a non-piezoelectric bulk substrate, for example, e.g. Si, Sapphire, Fused Silica; YAG etc. The substrate may be a Y-cut substrate having a rotation of between about 30° and about 50° around the Y-axis. Such as Y-cut LiNbO.sub.3, 36° Y-cut LiNbO.sub.3, 41° Y-cut LiNbO.sub.3, 64° Y-cut LiNbO.sub.3, 163° Y-cut LiNbO.sub.3, 36° Y-cut LiTaO.sub.3, 42° Y-cut LiTaO.sub.3, The substrate is suitable for propagation of surface acoustic waves.
(41) The sensor 1 may be provided with electrical contacts 12, or contact pads 12, for the provision of a signal to the SAW resonator. A first contact 12 may be arranged in communication with the IDT 8. A second contact 12 may be arranged in communication with the at least one reflective grating 9. If′ the SAW resonator is provided with two reflective gratings 9, then the second contact may be arranged in communication with both reflective gratings 9.
(42) The sensor 1 as described herein enables one-port sensing measurements at high frequencies. High frequencies may be around or greater than 100 MHz, Such measurements include measurement of shift in resonance frequency, change in amplitude of admittance and conductance near resonance, change in phase of the admittance near resonance, changes in resonator signal time of decay etc. High frequency signals may be provided to the IDT 8.
(43) Low frequency signals may be provided to the at least one reflective grating 9. Low frequency signals may be from around 10 Hz to about 100 Hz. The low frequency signals may be used to measure complex electric impedance of the sample, High frequency and low frequency signals may be provided substantially simultaneously, that is concurrently. The reflective gratings provided with low frequency signals enable electrical impedance spectroscopy.
(44) The sample to be measured may be a liquid sample. The liquid sample may be electrically conductive.
(45) The principle of operation allows the use of this device in physical, chemical and biological sensing applications. The devices 1 has a small form factor, uses small volumes of samples and provides for robust integration in to a sensing array.
(46) Also provided herein is a sensor assembly comprising a plurality of devices 1 according to that described above. The sensor assembly may comprise a single fluidic layer 2. The plurality of regions for receiving a sample in each of the respective devices in the sensor assembly may be accessible by a plurality of microfluidic chambers 3 provided in the single microfluidic layer 2. The microfluidic channels 4 present in the fluidic layer 2 may be arranged in a fluidic gradient generator as is known in the art. In such a way simultaneous and parallel analysis of a variety of samples can be achieved with the sensor assembly. The complexity of measurement of a variety of samples is thus greatly reduced.
(47) Also provided herein is a method for physical, biological, and/or physical measurement comprising: providing a sample to be tested to a sensor 1 according to the description above. The method further comprises providing a high frequency signal of greater than about 100 MHz to the IDT 8, and/or providing a low frequency signal of about 10 Hz to about 10 MHz, to the interdigitated reflective grating 9. Thereafter, measuring at least one of: shift in resonance frequency, change in amplitude of admittance and conductance near resonance, change in phase of the admittance near resonance, changes in resonator signal time of decay, and/or changes in complex electrical impedance in the low frequency range. As described above high frequency signals are suitable for measuring frequency shifts of resonance in the resonator. The low frequency signals can be used to measure complex permittivity of the sample to be tested. The low frequency signals are generally employed when the reflective gratings 9 are arranged interdigitally and when the impedance of the SAW resonator is measured. The high frequency signals and low frequency signals may be provided concurrently, such as substantially simultaneously. The at least one reflective grating 9 is specifically designed to be capacitive such that the provision of low frequency signals enables measuring of parameters not possible in previous SAW based sensor systems.
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Materials and Fabrication
Substrate and SAW Resonator Fabrication
(49) A typical surface acoustic resonant device, as disclosed here, is fabricated on a 4″ (Ø) 525 μm thick Y-cut X-propagation black LiNbO.sub.3 piezoelectric substrate (Precision Micro-Optics Inc., USA) using standard lift-off lithography. First, the substrate is cleaned with oxygen plasma (PS300AL PC, PVA TePla AG, Germany), followed by sonication in mr-Rem 400 remover (Micro Resist Technology GmbH, Germany), rinsed in ethanol and deionized water (DI), and dried with N.sub.2 stream. The substrate is then primed with HMDS (MicroChemicals GmbH, Germany) vapor (QS V 200 BM, solar-semi GmbH, Germany). Following that the image reversal photoresist (Merck AZ 5214 E, MicroChemicals GmbH, Germany) is applied by spin-coating (resulting thickness of 1.5 him) and baked at 110° C. for 1 minute. Pattern transfer into the resist is done by laser direct writer (λ=405 nm, exposure dose 24 mW, DWL 2000 by Heidelberg Instruments Mikrotechnik GmbH, Germany). Reversal bake at 125° C. for 1 minute and flood exposure of the resist (λ=365 nm, 60 seconds at 6 mW/cm.sup.2, MA/BAG by SÜSS MicroTec AG, Germany) is followed by development step in Merck AZ 351B general purpose developer (MicroChemicals GmbH, Germany) for 35 seconds (1-part developer to 5 parts DI). To remove residues of the photoresist and HMDS, an O.sub.2 plasma descumming step is performed (30 seconds at 50 W, 250 mTorr, 10 SCCM, BatchTop m/95 by Plasma-Therm LLC, USA). Metallization by e-beam evaporation (PVD225, Kurt J. Lesker Company Ltd., USA) consists of 25 mu Ti adhesion layer, 260 mu Au load and 15 mu Ti cap layer. The top Ti layer allows for native oxidation of the material to form TiO.sub.2, that significantly improves the adhesion of SiO.sub.2 passivation and prevents its delamination in case when bare Au is used without any capping. Lilt-off of excess metallization is done in acetone using sonication followed by a washing step in mr-Rem 400 remover, ethanol and DI. 100 mu of SiO.sub.2 passivation layer is deposited by reactive magnetron sputtering (MS 150, FHR Anlagenbau GmbH, Germany) in order to protect the electrodes from corrosion and short-circuiting effects, as well as to increase bonding energy between the device and a PDMS slab that contains the micro fluidic channels. To etch the contact pad 12 opening another lithography step is performed. The substrate is again treated with HMDS vapor, and approximately 1.2 μm of Merck AZ 1512 HS (MicroChemicals GmbH, Germany) photoresist is subsequently applied via spin-coating, and baked at 100° C. for 1 minute. Definition of an etch mask is done with direct laser writing (λ=405 nm, exposure dose ≈24 mW), followed by a development step in Dow Microposit MF CD-26 developer (MicroChemicals GmbH, Germany) for 45 seconds. An additional descumming step in O.sub.2 plasma is then performed to remove residues of the photoresist and HMDS. Openings in SiO.sub.2 are dry etched in NF.sub.3 plasma (Plasmalab System 100, Oxford Instruments plc, UK). The etch mask is then removed by sonication in mr-Rem 400 remover, ethanol and DI wash. In the final step the chips are diced and packaged.
Fluidic Layer Fabrication
(50) A microfluidic analyte delivery system is fabricated in PDMS, using standard soft lithography. The master mould is fabricated by applying approximately 50 μm of MicroChem Corp. SU-8 3035 negative photoresist (Micro Resist Technology GmbH, Germany) on a 4″ (Ø) 525 μm thick Si wafer (MicroChemicals GmbH, Germany) via spin-coating (GYRSET® equipped RCD8 by SÜSS MicroTec AG, Germany). Prior to resist application, the substrate is cleaned using buffered oxide etch solution (to remove the native oxide and to improve wetting of the polymer), rinsed in DI and blow-dried in an N.sub.2 stream. Soft-baking is performed at 95° C. for 15 minutes. Subsequently edge beads are removed by solvent jetting on the periphery of a wafer. Microfluidic circuits are defined by photolithography (2=365 nm, 42 seconds at 6 mW/cm.sup.2, MA/BA 6 by SÜSS MicroTec AG, Germany) using vacuum contact exposure. To finalize resist polymerization, it is post-baked for 1 minute at 65° C. and 5 minutes at 95° C. Development follows, using mr-Dev 600 (Micro Resist Technology GmbH, Germany) for 8 minutes. An additional descumming step in O.sub.2 plasma is performed to remove residues of the photoresist, followed by a hard baking step to reduce pattern stress and remove cracks in polymer, employing temperature ramping of the wafer to 200° C. (about T.sub.g of polymerized SU-8) and back to room temperature. To passivate the surface of the master mould, trichloro(1H,1H,2H,2H-perfluorooctyl)silane (Sigma-Aldrich Co. LLC, USA) vapor is used. Finally, silicon elastomer prepolymer is prepared from a Dow SYLGARD® 184 kit (Sigma-Aldrich Co. LLC, USA), cast in a 10:1 base/catalyst mixture, and cured at 80° C. for an hour. The cured PDMS replica is released from the master mould for post-processing that includes cutting out of individual chips and punching inlets and outlets.
Preparation and Bonding of Layers
(51) Thereafter both the resonator chip and PDMS structure are exposed to O.sub.2 plasma for 45 seconds (0.2 mBar, 30 SCCM, 100 W, Atto Plasma Chamber, Diener Electronic GmbH, Germany), To align the two parts, Milli-Q water (18.2 MΩ) is applied onto the surface of the SAFE sensor, preventing immediate bonding with the PDMS chip when brought into contact. Alignment is performed under a stereo microscope. Once aligned, the complete assembly 1 is rested for 10 minutes, so that the Milli-Q water can dry and allow for delayed covalent bonding of the components. The process if finalized by a baking step at 80° C. for 10 minutes, after which the sensor 1 are inspected and packaged.
Experimental Section
A Fabricated Sensor 1
(52) A sensor 1 was prepared according to the fabrication methods described above. In
Demonstration of SH-SAW Confinement to the Surface by the Said Periodic Strip Gratings Comprising the IDT (8) and the Reflective Gratings (9)
(53) To show the principle of energy confinement near the interface between the periodic strip gratings and the liquid, a Finite Element Method (FEM)-simulation of the SH-SAW displacement was performed. A periodic strip grating along the X-axis on the surface of Y-cut LiNbO.sub.3 is considered to have 270 nm thick. Au strips with pitch p.sub.0=10 μm. As evident from
(54) Characterization of the Fabricated Device
(55) This embodiment describes a method for close-in resonance characterisation of the fabricated device. Sensitivity towards exposing the sensor to a liquid is demonstrated while retaining the characteristic device performance features. In
(56) Conclusions from Experimental Section
(57) One-port resonant sensor platforms as described herein are characterized by lower toss of signal, thus maintaining a moderate to low electric impedance at resonance. The device Q×f product (Q— the Q factor, f— the resonance frequency) in liquid remains on the order of 1.710.sup.10 Hz, while the acoustic wave transducer is naturally protected from the short-circuiting effect of the liquids. Sensor response is represented by changes in resonance frequency, phase, resonator dissipation, or combinations thereof.
(58) The thin film technological platform has demonstrated sensing resolution comparable to QCM, while offering robust integration in sensing arrays and small sample volumes. The obtained benefits arise from the ability of one-port measurement, and the high frequency of operation which led to significantly reduced size, as compared to QCM.
(59) The integrated resonant SAW sensor, presented in this invention, is a high frequency equivalent of the QCM in view of the ability to perform as one-port resonator loaded with liquid and biochemical deposits on the sensing surfaces.
(60) Although, the present invention may have been described above with reference to specific embodiments, it is not intended to be limited to the specific form set forth herein. Rather, the invention is limited only by the accompanying claims.
(61) In the claims, the term “comprises/comprising” does not exclude the presence of other elements or steps. Furthermore, although individually listed, a plurality of means, elements or method steps may be implemented by e.g. a single unit or processor. Additionally, although individual features may be included in different claims, these may possibly advantageously be combined, and the inclusion in different claims does not imply that a combination of features is not feasible and/or advantageous. In addition, singular references do not exclude a plurality. The terms “a”, “an”, “first”, “second” etc do not preclude a plurality. Reference signs in the claims are provided merely as a clarifying example and shall not be construed as limiting the scope of the claims in any way.