CN113884542B - Wireless micro-fluidic sensor based on multilayer ceramic technology - Google Patents
Wireless micro-fluidic sensor based on multilayer ceramic technology Download PDFInfo
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/221—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance by investigating the dielectric properties
Abstract
The invention relates to a wireless microfluidic sensor based on a multilayer ceramic technology. The wireless microfluidic sensor based on the multilayer ceramic technology comprises: the micro-channel integrated waveguide resonator comprises a substrate integrated waveguide resonator, a slot antenna and a micro-channel structure integrated inside the substrate integrated waveguide resonator.
Description
Technical Field
The invention relates to a wireless microfluidic sensor based on a multilayer ceramic technology, and belongs to the fields of microfluidic technologies and sensor research.
Background
Microfluidic technology refers to the technology of manipulating fluids within micro-nano scale channels. Microfluidic technology has important applications in the fields of instant diagnosis, cell analysis, biosensing, drug metabolism, environmental detection, etc. As an important application field of microfluidic technology, the research of a chip-type microfluidic sensor has recently received extensive attention from academia and industry at home and abroad, and is a frontier research field involving the intersection of multiple disciplines such as analytical chemistry, fluid physics, biomedicine, electronic information, new materials and the like. The traditional microfluidic sensor is mainly used for detecting liquid to be detected by adopting a light detection method or a chemical analysis method, so that fluorescent marks or chemical modifications are required to be made in the sample preparation or test process, and in addition, professional operators and expensive professional analysis equipment are also required to be combined for detection, which becomes one of main bottlenecks for limiting the large-scale and wide use of the microfluidic sensor. With the rapid development of wireless communication technology and the rapid increase of demands of mobile medical and wearable devices, the technology integration of microfluidic liquid sensing and wireless communication has become one of hot spot directions in the development of microfluidic sensor technology.
The micro-flow sensor based on the microwave resonator utilizes the principle of dielectric perturbation to realize the sensing and analysis of the liquid to be detected by the change of the resonant frequency point and amplitude of the resonator caused by the change of the dielectric constants or the conductivities of different liquids in the micro-flow channel. Compared with the traditional microfluidic sensor, the microfluidic sensor based on the microwave resonator can realize label-free and noninvasive rapid detection. Common resonator types in microwave sensors mainly include split ring resonators (split ring resonators), cross-coupled ring resonators (cross split ring resonators), dielectric resonators (dielectric resonators), and substrate integrated waveguide (SubstrateIntegratedWaveguide, SIW) resonators. The SIW is a novel waveguide-like structure integrated in a medium, and is a resonator structure formed by connecting upper and lower metal surfaces of a substrate on a low-loss dielectric substrate by using a periodically metallized through hole array. Because the SIW resonance structure inherits the advantages of high Q value and low loss of the traditional metal waveguide and has the advantages of small size, easy processing and low cost of the microstrip circuit, under the traction of the requirements of miniaturization and integration of the whole sensor and the detection system, the SIW-based sensor starts to be widely focused by academia and industry. For example, chinese patent 1 (application No. 202010044452.5) discloses a reconfigurable quarter-mode substrate integrated waveguide microwave microfluidic sensor, in which a PTFE-based dielectric material is used as a sensor substrate, but a PDMS organic material is used as a liquid channel and is independently placed outside the sensor. Meanwhile, microwave signal excitation needs to be tested by means of an SMA connection network analyzer. Although the organic material has the advantages of flexibility, low cost and good processability, the thermal stability is relatively poor, the organic material is not suitable for high-temperature or corrosive liquid detection, and the organic material can be subjected to chemical reaction with a microfluidic solvent to cause swelling, deformation and the like of a microfluidic channel. Compared with organic materials, the low-temperature co-fired ceramic (LTCC) and high-temperature co-fired ceramic (HTCC) materials have the advantages of high melting point, high strength, chemical inertness, corrosion resistance and the like, and have incomparable advantages in the application of extreme chemical reactions and test conditions of high temperature, high pressure, corrosion and the like. In addition, multilayer ceramic technology, represented by LTCC and HTCC, is also one of the technological approaches to the fabrication of various types of microwave resonators and sensors. For example, chinese patent 2 (publication No. CN109374690 a) discloses a wireless microfluidic sensor, but the working principle is that the sensor relies on the near-field magnetic induction coupling of an inductance coil, the test distance is short, and the detection limit is not high due to the limitation of the inductance coil, for example, the detection limit is only 10% (volume concentration) of ethanol aqueous solution. For example, chinese patent 3 (publication No. CN107677707 a) discloses a LTCC-based substrate integrated waveguide type wireless passive gas sensor and a method for manufacturing the same, but a cylindrical hole for supporting a gas sensitive material is provided at the center of the substrate integrated waveguide structure, and a conductive gas sensitive material is coated on the metal surface of the cylindrical sidewall, which is equivalent to introducing a conductive material into the substrate integrated waveguide resonator, thereby reducing the Q value of the substrate integrated waveguide resonator, and in addition, the slot position of the slot antenna is selected at a position close to the through hole of the substrate integrated waveguide array, thereby reducing the reflection of microwave signals, and affecting the sensitivity and the test distance of the sensor. Most importantly, this patent discloses a gas sensor that is incapable of microfluidic liquid detection.
Disclosure of Invention
Aiming at the problems that the integration level of a micro flow channel and a resonator of the traditional micro flow control sensor based on a microwave resonator is low, and an SMA wire connection test is needed, the invention aims to provide a wireless micro flow control sensor based on a multilayer ceramic technology, realize the integration of liquid sensing and wireless communication and provide a new thought for the design of the wireless micro flow control sensor.
In one aspect, the present invention provides a wireless microfluidic sensor based on multilayer ceramic technology, comprising: the micro-channel integrated waveguide resonator comprises a substrate integrated waveguide resonator, a slot antenna and a micro-channel structure integrated inside the substrate integrated waveguide resonator. The invention relates to a novel wireless microfluidic sensor with a simple structure.
In the invention, the substrate integrated waveguide resonator and the micro-channel structure are creatively integrated on the same multilayer ceramic substrate through co-firing of the multilayer ceramic material and the metal electrode material for the first time, thereby realizing the integrated integration of the microwave resonator, the antenna and the micro-channel. In addition, the invention has the further advantage that the micro-flow channel structure is introduced into the substrate integrated waveguide resonator, which is equivalent to introducing air medium, and the dielectric loss of air is approximately 0 and is far smaller than that of ceramic medium material, so that the Q value of the resonator can be obviously improved by integrating the substrate integrated waveguide resonator and the micro-flow channel structure together through the multilayer ceramic technology, and the sensitivity of the sensor is further effectively improved. Because different fluid types and different concentrations of fluids have different dielectric constants and conductivities, the sensing and analysis of different liquids to be detected are realized by utilizing the principle of dielectric perturbation of the resonator and by changing the resonant frequency point and amplitude of the resonator caused by the change of the dielectric constants or conductivities of different liquids in the microfluidic channel. The method has the advantages of no marking, wireless detection, high sensitivity, good stability and the like.
Preferably, the substrate integrated waveguide resonator is composed of a ceramic substrate, a first metal electrode surface and a second metal electrode surface which are positioned on the upper surface/the lower surface of the ceramic substrate, and a periodic array of metal through holes.
Preferably, the shape of the substrate integrated waveguide resonator is square, round or triangular.
Preferably, the slot antenna is formed by slotting on the first metal electrode surface or the second metal electrode surface; the slotting position of the slot antenna is arranged at a right middle position within a range formed by surrounding the periodically-arrayed metal through holes; the slot antenna is rectangular in shape, the length-to-width ratio is 7-9:1, and the distance between the broadside and the metal through hole is kept to be more than 1 time of the broadside length.
Preferably, the micro-channel structure is located inside a ceramic substrate constituting the substrate integrated waveguide resonator, and the micro-channel structure has at least an inlet and an outlet capable of penetrating to the first metal electrode surface or the second metal electrode surface.
Still preferably, the wireless microfluidic sensor further comprises: an inlet hose sealed at the inlet for introducing the fluid to be tested, and an outlet hose sealed at the outlet.
Preferably, the wireless microfluidic sensor based on the multilayer ceramic technology is prepared by integrated cofiring through the multilayer ceramic technology; the multilayer ceramic technology can be a low temperature co-fired ceramic technology or a high temperature co-fired ceramic technology.
In another aspect, the invention provides an application of a wireless microfluidic sensor based on multilayer ceramic technology in liquid detection, wherein the liquid is liquid or solution with conductivity less than 0.001S/m, and is selected from ethanol water solution and glucose water solution. Preferably, the concentration detection limit of the ethanol aqueous solution is 5vol% (volume concentration), and the concentration detection limit of the glucose aqueous solution is 50mg/dL. It should be understood that the sensitivity of the sensor can be further improved by changing the size and micro-channel structure of the substrate integrated waveguide resonator, and it can be seen from the figure that the existing sensor also responds to the concentration below 50mg/dL, and the theoretical detection limit of the sensor to the glucose aqueous solution can reach 1.42mg/dL according to the calculation result.
The beneficial effects are that:
(1) Compared with the common organic matrix material in the existing microfluidic device, the LTCC material has high chemical stability, and can be co-fired with the silver electrode material with high conductivity, so that the device loss caused by the sensor material is reduced;
(2) Compared with the existing microfluidic technology, the wireless microfluidic sensor provided by the invention has the advantages that the detection is in a low-cost, label-free and non-invasive detection mode, and a detection junction can be quickly and conveniently obtained;
(3) According to the invention, the micro-flow channel is embedded in the substrate integrated waveguide resonator, which is equivalent to introducing an air cavity in the substrate integrated waveguide resonator, so that the Q value of the substrate integrated waveguide resonator is obviously improved from 353 without the micro-flow channel to 1205, the improvement is more than 3 times, and the sensor has higher sensitivity;
(4) Because the LTCC has the advantage of multi-layer technology, various functional components can be integrated, so that the sensor has more functions, and the sensor is beneficial to realizing miniaturization and functional integration.
Drawings
FIG. 1 is a schematic diagram of the structure of a wireless microfluidic sensor according to the present invention
Fig. 2 is a schematic front view of a wireless microfluidic sensor of the present invention;
FIG. 3 is a schematic back view of a wireless microfluidic sensor according to the present invention
FIG. 4 is a schematic diagram of a portion of a micro-fluidic channel structure of a wireless microfluidic sensor according to the present invention;
FIG. 5 shows the results of wireless tests of the wireless microfluidic sensor of the present invention on ethanol aqueous solutions with different concentrations, wherein the detection limit of the sensor of the present invention on ethanol aqueous solutions can reach 5vol%;
FIG. 6 shows the results of wireless tests of the wireless microfluidic sensor of the present invention on glucose aqueous solutions of different concentrations, wherein the detection limit of the sensor of the present invention on glucose aqueous solutions can reach 50mg/dL;
fig. 7 is a schematic exploded view of a wireless microfluidic sensor according to the present invention.
Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
In the invention, the substrate integrated waveguide resonator, the slot antenna and the micro-channel are combined for the first time, and the wireless detection of the type and concentration of the fluid is realized by receiving and transmitting the sensor signal through the slot antenna by utilizing the principle that the dielectric constant and the conductivity of the fluid in the micro-channel cause the resonance frequency point and the amplitude of the resonator to change.
In an embodiment of the present invention, the structure of the wireless microfluidic sensor is shown in fig. 1 and 7, and the wireless microfluidic sensor comprises a multilayer ceramic substrate 1, a substrate integrated waveguide resonator formed by periodic array metal through holes 2 (the diameter D can be 0.1-0.5 mm and the distance p between adjacent metal through holes can be 0.2-1 mm) and a first metal electrode surface (upper electrode 3) and a second metal electrode surface (lower electrode) 4 which are positioned on the multilayer ceramic substrate, and a slot antenna 5 formed by slotting in the upper electrode 3. The slotting position is arranged within the range formed by surrounding the periodically arrayed metal through holes and has a specified distance from the metal through holes. The slot antenna is rectangular in shape, and has a length (L) to width (W) ratio of (7-9): 1, and a distance (Wp) between the broadside and the metal through hole is maintained to be 1 time or more the broadside length, so as to reduce the influence on the sensor sensitivity and the test distance. A micro flow channel structure 6 for containing the liquid to be measured is also provided within the resonator and between the upper electrode 3 and the lower electrode 4. Wherein the micro flow channel structure 6 has at least an inlet 7 and an outlet 8 (see fig. 3) penetrating the surface of the upper electrode 3. The liquid to be measured is introduced into the micro flow channel structure 6 in the multilayer ceramic substrate 1 from the inlet 7 for detection, and then flows out from the outlet 8.
The multilayer ceramic substrate 1 may be an LTCC or HTCC material, preferably an LTCC material. The total thickness of the multilayer ceramic matrix may be 0.5 to 2mm.
The resonator shape surrounded by the periodically-arrayed metal through holes 2 in the substrate integrated waveguide resonator can be square (the side length a can be 10-50 mm), triangular (the side length a can be 10-50 mm) or circular (the diameter a can be 20-60 mm), and is preferably square. The resonant frequency of the substrate integrated waveguide resonator is regulated by the side length dimension, namely the shape dimension of the resonator surrounded by the periodic array metal through holes 2 is also designed by combining the initial working frequency of the resonator.
The upper electrode 3 and the lower electrode 4 are arranged in parallel and are communicated up and down through the periodically arrayed metal through holes. The upper electrode 3, the lower electrode 4, and the periodically-arrayed metal vias 2 may be made of a conductive metal material such as gold, silver, or copper, preferably silver.
The micro flow channel structure 6 is disposed in the multilayer ceramic substrate 1, and may be distributed between the upper electrode 3 and the lower electrode 4 in a straight line, a bent shape, or a multilayer communication staggered manner. In a preferred example, the micro flow channel structures 6 are parallel to the upper electrode 3 and/or the lower electrode 4 and distributed in a zigzag manner in a plane. The inlet 7 and the outlet 8 are preferably provided on the upper surface of the multilayer ceramic substrate 1 and distributed within the resonator shape enclosed by the periodically arrayed metal vias 2. In an alternative embodiment, the cross-sectional shape of the micro flow channel structure is rectangular or square, and the side length c can be 0.2-2 mm. The top view of the micro-flow channel structure is S-shaped, and the unidirectional maximum length a of the S-shaped micro-flow channel 0 Can be 5-40 mm.
In an alternative embodiment, the wireless microfluidic sensor further comprises an inlet hose sealed at the inlet for introducing the fluid to be measured, and an outlet hose sealed at the outlet.
It should be understood that the present invention preferably employs LTCC technology to make wireless microfluidic sensors, but does not exclude wireless microfluidic sensors made using HTCC or other methods.
In another embodiment of the present invention, when the wireless microfluidic sensor detects fluid, the fluid to be detected can be introduced from the inlet (fluid inlet) 7 through the external electric pump, then the fluid to be detected flows into the micro-channel structure 6 along the inlet, when the fluid to be detected flows through the micro-channel structure 6 and passes through the areas of the upper electrode 3 and the lower electrode 4, the resonance frequency and the S11 amplitude of the substrate integrated waveguide resonator will change, and the frequency offset of the LC resonant antenna is different due to different dielectric constants and conductivities of different fluids to be detected or different concentrations of the same fluid, so as to realize detection of the type and concentration of the fluid.
The invention creatively combines the substrate integrated waveguide resonator/antenna integrated structure with the micro-flow channel by adopting a multilayer ceramic technology, and obtains the wireless micro-flow control sensor. The principle that the dielectric constant of the fluid in the micro-channel changes to cause the resonant frequency of the substrate integrated waveguide resonator is utilized, and wireless transmission is carried out on the liquid sensitive signals through the slot antenna, so that wireless detection of the type and concentration of the fluid is realized.
Compared with the traditional microfluidic sensor based on a spectrum method and an electrochemical method, the invention realizes the integration of liquid sensing and wireless microwave communication, has the advantages of being passive, wireless, miniaturized, portable, high in sensitivity, good in stability and the like, and has wide application prospects in the fields of instant diagnosis, water body monitoring, biochemical analysis, drug screening, environmental monitoring and the like.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1: preparation of wireless microfluidic sensor
(1) In this example 1, a wireless microfluidic sensor (square SIW, side length a=28 mm, total thickness h of ceramic matrix 0.8mm; diameter d=0.2 mm of metal through holes, pitch p=0.4 mm, length l=17 mm, width w=2 mm, W) of slot antenna was prepared by LTCC technology p =13 mm). Firstly, punching holes on the surface of LTCC green ceramic tape material, wherein the holes comprise metal through holes, lamination alignment holes and micro-channel holes (a) 0 =20 mm) and fluid inlet and outlet; printing silver electrode slurry on the surface of LTCC green ceramic tape material with holes according to a slotting pattern and a pattern of a full electrode through a screen printing process, and then drying in an oven at 80 ℃ for later use;
(2) The above punched and printed green tiles were laminated in order of green tile carrying upper electrode, green tile with micro flow channel structure, and green tile carrying lower electrode (see fig. 1). In order to keep the micro-channel structure smooth, single-axis pressure lamination is adopted, the lamination pressure is 1MPa, and the lamination temperature is 60 ℃; then, filling holes in the back film of the silver electrode at the through holes (namely, preparing through hole electrodes) so as to communicate the upper electrode and the lower electrode, thereby obtaining a sensor biscuit;
(3) Placing the sensor biscuit into a high-temperature electric furnace, heating to 450 ℃ at 1 ℃/min, preserving heat for 60 minutes to remove organic matters in the LTCC green ceramic tape material, and then continuously heating to 900 ℃ at 5 ℃/min, preserving heat for 20 minutes, and sintering to obtain a LTCC wireless microfluidic sensor sample;
(4) And firmly sealing and bonding the peek conversion interface for flowing in and out fluid at the fluid inlet and outlet (inlet and outlet) of the surface of the sintered sensor sample by using double-component glue, thereby completing the preparation of the LTCC wireless microfluidic sensor.
Example 2: application of wireless microfluidic sensor
(1) Because different fluids and the same fluid with different concentrations have respective characteristic dielectric constants, the invention mainly utilizes the working principle that the change of the dielectric constant and the conductivity of the fluid to be detected flowing through the micro-channel causes the change of the resonant frequency and the S11 amplitude of the sensor, and realizes the wireless detection of the type and the concentration of the fluid to be detected by collecting and analyzing the S parameter of the wireless microfluidic sensor through an external reading antenna;
(2) The liquid to be measured is discharged from the fluid outlet (outlet) after flowing through the micro-channel structure of the sensor, and the test results are shown in fig. 5, and it can be seen that the ethanol water solutions with different concentrations all show different resonance frequencies after flowing into the sensor, so as to realize wireless detection of different liquids;
(3) The glucose aqueous solution with different concentrations is respectively introduced into the sensor from the fluid inlet of the wireless microfluidic sensor, the liquid to be detected is discharged from the fluid outlet after flowing through the micro-channel structure of the sensor, and the test result is shown in fig. 6.
Claims (7)
1. The wireless microfluidic sensor based on the multilayer ceramic technology is characterized by comprising a substrate integrated waveguide resonator, a slot antenna and a micro-channel structure integrated in the substrate integrated waveguide resonator; the wireless microfluidic sensor based on the multilayer ceramic technology is prepared by integrally co-firing the multilayer ceramic technology;
the substrate integrated waveguide resonator consists of a ceramic matrix, a first metal electrode surface and a second metal electrode surface which are positioned on the upper surface/the lower surface of the ceramic matrix, and a periodic array of metal through holes;
the slot antenna is formed by slotting a first metal electrode surface or a second metal electrode surface, and the slotting position of the slot antenna is arranged at a right middle position within a range formed by surrounding a periodically-arrayed metal through hole;
the micro-channel structure is positioned in a ceramic matrix forming the substrate integrated waveguide resonator and is at least provided with an inlet and an outlet which can penetrate to the first metal electrode surface or the second metal electrode surface; the section of the micro-channel structure is rectangular or square, and the side length c is 0.2-2 mm; the top view of the micro-flow channel structure is S-shaped, and the unidirectional maximum length a of the S-shaped micro-flow channel 0 5-40 mm.
2. The wireless microfluidic sensor based on multilayer ceramic technology according to claim 1, wherein the shape of the substrate integrated waveguide resonator is square, circular or triangular.
3. The wireless microfluidic sensor based on multilayer ceramic technology according to claim 1, wherein the slot antenna is rectangular in shape with an aspect ratio of (7-9): 1, and the distance between the broadside and the metal through hole is maintained to be more than 1 time of the broadside length.
4. The wireless microfluidic sensor based on multilayer ceramic technology according to claim 1, further comprising: an inlet hose sealed at the inlet for introducing the fluid to be tested, and an outlet hose sealed at the outlet.
5. The wireless microfluidic sensor based on multilayer ceramic technology according to any one of claims 1 to 4, characterized in that the multilayer ceramic technology is a low temperature co-fired ceramic technology or a high temperature co-fired ceramic technology.
6. Use of a wireless microfluidic sensor based on multilayer ceramic technology according to any one of claims 1 to 5 for liquid detection, characterized in that the liquid is a liquid or a solution with conductivity < 0.001S/m, selected from aqueous ethanol or aqueous dextrose.
7. The use according to claim 6, wherein the aqueous ethanol solution has a concentration detection limit of 5 vol.% and the aqueous glucose solution has a concentration detection limit of 50mg/dL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111039902.2A CN113884542B (en) | 2021-09-06 | 2021-09-06 | Wireless micro-fluidic sensor based on multilayer ceramic technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111039902.2A CN113884542B (en) | 2021-09-06 | 2021-09-06 | Wireless micro-fluidic sensor based on multilayer ceramic technology |
Publications (2)
| Publication Number | Publication Date |
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