CN115465833A - Multi-channel heat sensor with micro-suspension structure and preparation method thereof - Google Patents

Multi-channel heat sensor with micro-suspension structure and preparation method thereof Download PDF

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Publication number
CN115465833A
CN115465833A CN202211138580.1A CN202211138580A CN115465833A CN 115465833 A CN115465833 A CN 115465833A CN 202211138580 A CN202211138580 A CN 202211138580A CN 115465833 A CN115465833 A CN 115465833A
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micro
channel
fluid channel
sensor
substrate
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CN202211138580.1A
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王竹卿
张亚男
殷鸿波
刘奇
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Sichuan University
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Sichuan University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
    • G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
    • G01N25/4873—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a flowing, e.g. gas sample
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
    • B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00261—Processes for packaging MEMS devices
    • B81C1/00301—Connecting electric signal lines from the MEMS device with external electrical signal lines, e.g. through vias
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
    • G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/05—Microfluidics

Abstract

The invention discloses a multi-channel heat sensor with a micro-suspension structure and a preparation method thereof, and the multi-channel heat sensor comprises a micro-channel inlet, a micro-channel and a micro-channel outlet, wherein a plurality of micro-channels are communicated between the micro-channel inlet and the micro-channel outlet, each micro-channel comprises a micro-fluid channel top cover, a micro-fluid channel wall and a micro-fluid channel bottom plate, a suspension bridge structure substrate is arranged at the bottom of the micro-fluid channel bottom plate, the edges of the micro-fluid channel top cover and the micro-fluid channel bottom plate are connected with the micro-fluid channel wall, a reference thermocouple and a main thermocouple are arranged inside a micro-fluid channel cavity, and a heater and a junction are respectively arranged on two sides of the top end of the micro-fluid channel bottom plate. The sensor comprises the microfluidic channel with the suspension bridge structure, so that the improvement of sensitivity and the reduction of heat loss are realized; the micro-fluidic measurement chamber is used for carrying out sensitive measurement on a small-volume liquid sample so as to reduce the loading dosage of the biological fluidic sample to the maximum extent, and the power-assisted portable medical care application is realized.

Description

Multi-channel heat sensor with micro-suspension structure and preparation method thereof
Technical Field
The invention relates to the field of heat sensors, in particular to a multi-channel heat sensor with a micro-suspension structure and a preparation method thereof.
Background
A thermal sensor is a device that can collect information for analyzing the temperature difference between a sample to be detected and a detection element. With the development of the disciplines of material science, electronic science and the like, the heat sensor becomes a research hotspot, in recent years, various novel heat detection sensors with excellent performance appear, and the requirements on the precision, the detection speed and the volume of the heat sensor are higher and higher. With the development of the integration technology, it is a trend to provide a sensor with small size, light weight and high detection precision.
With the development of Micro-Electro-Mechanical systems (MEMS), higher requirements are put on the performance and processing technology of various microstructures due to the requirements of the performance or structure of the Micro-System. The micro-suspension structure has a wide range of requirements because it can effectively avoid the influence between molecules and surfaces between the micro-suspension structure and the substrate and the heat transfer, and increase the contact area with the surrounding environment. Due to the fact that the suspension structure is isolated from the substrate relatively, heat flowing caused by other external factors can be reduced to the maximum extent, and detection precision of the sensor is improved. The suspended structure is combined with the heat sensor, so that heat dissipated in heat transfer can be effectively detected, and the detection accuracy and sensitivity of the sensor are improved.
The existing process for manufacturing a suspended structure between microstructures comprises bulk silicon process etching, an electrospinning process, chemical vapor deposition and the like, and because the required equipment or experimental conditions are higher, the process cost is higher, or accurate and firm mechanical bonding and effective electrical contact between the micro suspended structure and the microstructures are difficult to establish.
With the continuous improvement of the MEMS technical level, compared with the traditional heat sensor which is heavy, the micro-suspension structure heat sensor combines the micro-channel structure and the micro-suspension structure by means of the MEMS technology, and has the advantages of high performance, small volume, low cost, high stability and the like.
In a micro-suspension thermal sensor, the sensor is usually prepared on a suspended thin film structure for improving the thermal insulation of the device to improve the high sensitivity of the sensor, and the micro flow channel is usually bonded directly above the sensor as a container and a reaction chamber of a reactant sample, so as to facilitate the manipulation of the reactant sample. The suspension structure can effectively improve the thermal insulation property of the device and reduce the heat capacity of the device, thereby increasing the heat sensitivity of the device. At present, different substrate materials such as silicon, glass, polymer, etc. have been applied to the fabrication of microfluidic structures. Silicon is a relatively common material with outstanding thermal stability, chemical inertness and good thermal conductivity, and a whole set of well-established processing technologies are available. The glass has the advantages of relatively low price, convenient processing and good biocompatibility. The polymer has the advantages of low cost, good processability, high optical transparency, simple processing steps, good biocompatibility and the like, and becomes a common microfluidic chip substrate material, such as a PDMS material and an SU-8 material. The PDMS material is resistant to high and low temperatures, does not harden at low temperatures, does not deform and soften at high temperatures, always keeps flexible characteristics, and has good dielectric properties and a certain ventilation effect. The SU-8 material has high transparency, large refractive index and low loss under a certain wavelength, and is considered to be a good material for optical waveguide application.
In the existing adopted microfluidic substrate materials, the preparation process of the silicon-based material is mature, but the etching process is relatively complicated, the requirement on the environment is severe, the processing period is long, and the large-scale application of the processing technology is limited. Furthermore, suspended membranes based on silicon materials are very fragile and complicated to manufacture. Glass, although transparent, has a great difficulty in etching a vertical cross section relative to a silicon wafer due to its amorphous nature. Although both silicon wafers and glass can be processed in bulk, the process of sealing the article needs to be performed in an ultra-clean environment and requires high voltage or high temperature. Compared with silicon-based materials, the polymer material has better tensile strength and lower thermal conductivity, and is easier to prepare into a thin film structure. However, polymer materials have the disadvantage that surface modifications are usually required and most are not resistant to high temperatures. While PDMS is an excellent material for making microfluidic systems, most organic solutions swell PDMS. In addition, while PDMS can replicate patterns with high fidelity, some geometries are not easily demolded. The prepared PDMS fluidic structures require an integrated bonding process with the sensor chip, which requires ensuring hermeticity and are difficult to bond to suspended microstructures. And the load force of the PDMS fluid system chip can damage the suspension structure of the thermal sensor, and the PDMS fluid system chip is applied to the suspension structure of a microsensor device.
The SU-8 based cantilever exhibits higher resistance to temperature changes than other cantilevers, which can reduce noise and improve sensitivity. Due to the high chemical resistance, microfluidic systems of microsensor devices are made with SU-8 polymers. The prepared microchannel with thin SU-8 cap enables the application of optical and fluorescence detection. The suspended microfluidic structure is integrated with thermocouple sensors, which can reduce heat loss and improve sensitivity compared to traditional bulky PDMS chambers.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a multi-channel thermal sensor with a micro-suspension structure and a preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a multi-channel heat sensor with a micro-suspension structure, which comprises a micro-channel inlet, a micro-channel and a micro-channel outlet, wherein a plurality of micro-channels are communicated between the micro-channel inlet and the micro-channel outlet, each micro-channel comprises a micro-fluid channel top cover, a micro-fluid channel wall and a micro-fluid channel bottom plate, a suspension bridge structure substrate is arranged at the bottom of each micro-fluid channel bottom plate, the edges of the micro-fluid channel top cover and the micro-fluid channel bottom plate are connected with the micro-fluid channel walls, a micro-fluid channel cavity is formed inside the micro-fluid channel top cover and the micro-fluid channel bottom plate, a reference thermocouple and a main thermocouple are arranged inside the micro-fluid channel cavity, and heaters and grounding parts are respectively arranged on two sides of the top end of each micro-fluid channel bottom plate.
As a preferred technical scheme of the invention, the micro-channels are uniformly distributed at intervals, and the spacing is 200um.
As a preferred technical scheme of the invention, the cavity of the micro-fluid channel is in a strip shape, the volume of the middle part is larger than that of the two sides, and the preparation material of the micro-fluid channel is SU-8 photoresist.
The invention also provides a preparation method of the multi-channel heat sensor with the micro-suspension structure, which comprises the following steps;
s1: preparing a processing substrate, taking an insulating silicon wafer as a substrate, and doping silicon dioxide in the silicon substrate by using an ion implantation process to reduce the resistance of the sensor;
s2: preparing a separation layer, depositing a silicon dioxide film on a substrate as the separation layer by using a chemical vapor deposition technology, etching the silicon dioxide layer by using buffered hydrofluoric acid etching solution, and opening a window for a thermocouple electrode;
s3: realizing electrode patterns of a heater and a sensor, coating photoresist on the front surface of silicon dioxide, forming the electrode patterns of the heater through photoetching, and defining the area of the heater electrode;
s4: preparing a port of a thermocouple electrode, depositing a chromium/gold layer on the top of the port by a sputtering deposition technology after a photoetching process, and manufacturing electrode patterns of a heater and a sensor by using an Au/Cr stripping process;
s5: preparing a micro-channel supporting wall, designing a micro-channel with the same structure, making the micro-channel wall and a separation layer from SU-8 photoresist, and making a top cantilever structure into a bridging structure by BHF etching and silicon etching;
s6: realizing micro-channel covering patterns, covering SU-8 dry films on a substrate by controlling force and temperature, and manufacturing covering film patterns on channels by a photoetching method;
s7: and preparing a silicon dioxide layer bottom cavity structure, and etching the bottom of the silicon dioxide to form a bottom cavity.
S8: stripping the photoresist at the bottom of the silicon dioxide layer to finish the preparation of the MEMS thermal sensor with the suspension structure cavity
As a preferred embodiment of the present invention, in step S1, the ion implantation conditions of the silicon substrate are 100kev voltage and 1020cm -3 Concentration of carrier
Compared with the prior art, the invention has the following beneficial effects:
1: the sensor of the invention comprises a micro-fluid channel with a suspension bridge structure, thus realizing the improvement of sensitivity and the reduction of heat loss.
2: the invention carries out sensitive measurement on the small-volume liquid sample through the microfluidic measuring chamber so as to reduce the loading dosage of the biological fluidic sample to the maximum extent and apply the assisted portable medical care.
3: the sensor provided by the invention comprises a plurality of micro-fluid channels, can realize quick response and small-volume sample detection, can simultaneously process a plurality of solutions for component detection, and solves the problems of less detection information and long processing time of the traditional MEMS thermal sensor.
4; the sensor can be produced in a large scale at one time by adopting a standard MEMS process, has low manufacturing cost, can be produced without complex equipment, and has the potential of wide use.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of the structure of a MEMS thermal sensor of the present invention;
FIG. 2 is a schematic diagram of a multi-channel thermal sensor of the present invention;
FIG. 3 is an exploded view of the structure of a single microfluidic channel of a multi-channel thermal sensor of the micro-suspension structure of the present invention;
FIG. 4 is a process diagram for preparing a multi-channel thermal sensor of a micro-suspension structure according to the present invention;
FIG. 5 is a response time of a microfluidic channel of a multi-channel thermal sensor of the present invention;
FIG. 6 is a result of a sensitivity test of a microfluidic channel of a multi-channel thermal sensor of a micro-suspension structure of the present invention;
in the figure: 1. a microchannel inlet; 3. a micro flow channel; 4. a microchannel outlet; 6. a heater; 7. a microfluidic channel upper cap; 8. a microfluidic channel wall; 9. grounding; 10. a microfluidic channel floor; 11. a reference thermocouple; 12. a main thermocouple; 13. a microfluidic channel cavity.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
As shown in fig. 1-3, the present invention provides a multi-channel thermal sensor with a micro-suspension structure, which comprises a micro-channel inlet 1, a micro-channel 3 and a micro-channel outlet 4, wherein a plurality of micro-channels 3 are communicated between the micro-channel inlet 1 and the micro-channel outlet 4, each micro-channel 3 comprises a micro-fluid channel top cover 7, a micro-fluid channel wall 8 and a micro-fluid channel bottom plate 10, a suspension bridge structure substrate is arranged at the bottom of the micro-fluid channel bottom plate 10, the micro-fluid channel wall 8 is connected to the edges of the micro-fluid channel top cover 7 and the micro-fluid channel bottom plate 10, a micro-fluid channel cavity 13 is formed inside the micro-fluid channel top cover 7 and the micro-fluid channel bottom plate, a reference thermocouple 11 and a main thermocouple 12 are arranged inside the micro-fluid channel cavity 13, and a heater 6 and a grounding part 9 are respectively arranged at two sides of the top end of the micro-fluid channel bottom plate 10.
Further, the microchannels 3 are evenly spaced and spaced at a distance of 200um.
Further, the micro-fluid channel cavity 13 is a long strip, the volume of the middle part is larger than that of the two sides, the square cavity is arranged in the middle, the side length is 500um, the height is 50um, and the preparation material of the micro-fluid channel 3 is SU-8 photoresist.
Specifically, the heater 6 is matched with the grounding part 9 and used for evaluating after the sensor is produced and simulating the generated reaction heat; when the heat sensor starts to work, firstly, the eye fluid of a patient to be detected is injected into the inlet 1 of the micro-flow channel by a titration method, and is respectively injected into each micro-flow channel 3 by shunting, so that the whole cavity 13 and the flow channel of the micro-flow channel are filled with the solution; at this time, 5 chambers are filled with various types of enzymes, the enzymes are placed in the middle area of the microfluidic channel cavity 13, 1 of the chambers is an experimental group, the remaining 4 chambers are control groups, different enzymes react with the solution to generate reaction heat, then the reference thermocouple 11 and the main thermocouple 12 sense the heat and detect the released heat, and finally the electric signals are transmitted to a computer for processing.
As shown in fig. 4 to 6, the present invention further provides a method for preparing a multi-channel thermal sensor with a micro-suspension structure, comprising the following steps:
s1: referring to fig. 4 (a), a processing substrate is prepared, and a silicon-on-insulator (SOI) substrate having a device layer of N-type silicon is used, the silicon-on-insulator (SOI) substrate having a thickness of 10 μm, 1 μm, and 400 μm, respectively;
s2: referring to FIG. 4 (b), a separation layer was prepared by mixing 500nm of SiO 2 The thin film is deposited on the substrate by chemical vapor deposition as a separate layer of silicon dioxide (SiO) at 500nm 2 ) Etching the layer by buffered hydrofluoric acid (BHF) etching solution to open an ion injection window so as to prepare a PN junction;
s3: referring to fig. 4 (c), electrode patterns of the heater and the sensor are implemented, photoresist is coated on the front surface of silicon dioxide, the electrode patterns of the heater are formed by photolithography, and the area of the heater electrode is defined;
s4: referring to fig. 4 (d), preparing a port of a thermocouple electrode, depositing a 200nm chromium/gold (Cr-Au) layer on the top of the port by a sputtering deposition method after a photolithography process, specifically, sputtering a 40nm chromium (Cr) layer on the front surface of 500 μm thick silicon dioxide by using a sputtering device, then sputtering a 160nm gold (Au) layer on the chromium (Cr) layer, finally completing the deposition of a chromium/gold (Cr-Au) layer metal film, removing the chromium/gold (Cr-Au) layer which is not covered by a photoresist mask by using a chromium/gold (Cr-Au) etching solution, heating the substrate to 450 ℃ and maintaining the substrate for 1 minute to realize ohmic contact of the thermocouple sensor;
s5: referring to fig. 4 (e), a microchannel support wall was prepared, microchannels had the same structure according to design, microchannel walls and a separation layer were made of SU-8 photoresist, 50 μm was photo-etched, and after a cleaning process of a substrate, SU-8 walls were fabricated on a substrate by a photo-etching process, microchannel having a width of 50 μm and a height of 50 μm. Manufacturing the top cantilever structure into a bridging structure by buffered hydrofluoric acid (BHF) etching and silicon etching;
s6: referring to fig. 4 (f), a micro flow channel covering pattern was realized, and the thickness of the channel cover was prepared from a dried SU-8 thin film (50 μm), first, the dried SU-8 thin film with a support film was covered on the channel at 55 ℃ for 3 minutes, after exposure for 80 seconds, the substrate was pre-baked at 85 ℃ for 30 seconds, after which the support film was moved, and the substrate was heated at 95 ℃ for 5 minutes to harden the pattern on the substrate;
s7: referring to fig. 4 (g), preparing a silicon dioxide layer bottom cavity structure, etching the bottom of silicon dioxide to form a bottom cavity, developing the SU-8 thin film by using SU-8 developing solution, washing off the developing solution after 10min, and completing the preparation of the hollow structure on the substrate;
s8: referring to fig. 4 (h), the photoresist at the bottom of the silicon dioxide layer is stripped, and the MEMS thermal sensor having the bridge structure is prepared through a back silicon etching and buffered hydrofluoric acid (BHF) etching process.
After step S8, performing simulation test on the MEMS thermal sensor by using simulation software, as shown in fig. 5, performing response time test on the multi-target detection MEMS thermal sensor according to the embodiment; it can be seen that when a step temperature is input, the sensor can quickly respond to the temperature change, and in less than 200ms, the thermocouple detects the temperature change and outputs a response signal, and then converts the response signal into an electric signal output, so that the thermal sensor has quick response and good thermal characteristics.
As shown in FIG. 6, the sensitivity test of the multi-target detection MEMS heat sensor of the embodiment shows that the sensor has extremely high thermal characterization precision, which confirms that the prepared micro sensor can measure the catalytic reaction heat of the enzyme, and the suspension bridge structure provided by the invention can improve the sensitivity of the heat detection.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. The utility model provides a multichannel heat sensor of little suspension structure, its characterized in that, includes microchannel entry (1), microchannel (3) and microchannel export (4), it has a plurality of microchannels (3) to put through between microchannel entry (1) and microchannel export (4), microchannel (3) include microfluidic channel top cap (7), microfluidic channel wall (8) and microfluidic channel bottom plate (10), the bottom of microfluidic channel bottom plate (10) is provided with suspension bridge structure substrate, the border department of microfluidic channel top cap (7) and microfluidic channel bottom plate (10) is connected with microfluidic channel wall (8), inside microfluidic channel cavity (13) that forms simultaneously, the inside of microfluidic channel cavity (13) is provided with reference thermocouple (11) and main thermocouple (12), the top both sides of microfluidic channel bottom plate (10) are equipped with heater (6) and ground connection department (9) respectively.
2. A multi-channel thermal sensor of a micro-suspension structure according to claim 1, wherein the micro-channels (3) are uniformly spaced and spaced at a distance of 200um.
3. The multi-channel thermal sensor with a micro-suspension structure as claimed in claim 2, wherein the micro-fluid channel cavity (13) is a strip with a volume in the middle larger than that on two sides, and the micro-fluid channel (3) is made of SU-8 photoresist.
4. A preparation method of a multi-channel heat sensor with a micro-suspension structure is characterized by comprising the following steps;
s1: preparing a processing substrate, doping silicon dioxide in a silicon substrate by using an ion implantation process and taking an insulating silicon wafer as the substrate, and reducing the resistance of the sensor;
s2: preparing a separation layer, depositing a silicon dioxide film on a substrate as the separation layer by a chemical vapor deposition technology, etching the silicon dioxide layer by buffered hydrofluoric acid etching solution, and opening a window for a thermocouple electrode;
s3: realizing electrode patterns of a heater and a sensor, coating photoresist on the front surface of silicon dioxide, forming the electrode patterns of the heater by photoetching, and defining the area of the heater electrode;
s4: preparing a port of a thermocouple electrode, depositing a chromium/gold layer on the top of the port by a sputtering deposition technology after a photoetching process, and manufacturing electrode patterns of a heater and a sensor by using an Au/Cr stripping process;
s5: preparing a micro-channel supporting wall, designing a micro-channel with the same structure, making the micro-channel wall and a separation layer from SU-8 photoresist, and making a top cantilever structure into a bridging structure by BHF etching and silicon etching;
s6: realizing micro-channel covering patterns, covering SU-8 dry films on a substrate by controlling force and temperature, and manufacturing covering film patterns on channels by a photoetching method;
s7: and preparing a silicon dioxide layer bottom cavity structure, and etching the bottom of the silicon dioxide to form a bottom cavity.
S8: and stripping the photoresist at the bottom of the silicon dioxide layer to finish the preparation of the MEMS thermal sensor with the suspension structure cavity.
5. The method as claimed in claim 4, wherein in step S1, the silicon substrate is implanted at 100kev voltage and 1020cm -3 The carrier concentration.
CN202211138580.1A 2022-09-19 2022-09-19 Multi-channel heat sensor with micro-suspension structure and preparation method thereof Pending CN115465833A (en)

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