CN115465833B - A multi-channel thermal sensor with micro-suspension structure and its preparation method - Google Patents
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- 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
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- 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
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- B81C1/00301—Connecting electric signal lines from the MEMS device with external electrical signal lines, e.g. through vias
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
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Abstract
本发明公开了一种微悬浮结构的多流道热传感器及其制备方法，包括微流道入口、微流道和微流道出口，微流道入口与微流道出口之间接通有多个微流道，微流道包括微流体通道顶盖、微流体通道壁和微流体通道底板，微流体通道底板的底部设置有悬浮桥式结构衬底，微流体通道顶盖与微流体通道底板的边沿处连接有微流体通道壁，微流体通道空腔的内部设置有参考热电偶和主热电偶，微流体通道底板的顶端两侧分别设有加热器和接地处。本发明传感器含有悬浮桥式结构的微流体通道，实现了灵敏度的提高和热损失的减小；通过微流控测量室对小体积液体样品进行敏感测量，以最大限度地减少生物流控样品加载剂量，将助力便携式医疗保健应用。
The present invention discloses a multi-channel thermal sensor with a micro-suspension structure and a preparation method thereof, comprising a microchannel inlet, a microchannel and a microchannel outlet, wherein a plurality of microchannels are connected between the microchannel inlet and the microchannel outlet, the microchannel comprises a microfluidic channel top cover, a microfluidic channel wall and a microfluidic channel bottom plate, a suspended bridge structure substrate is arranged at the bottom of the microfluidic channel bottom plate, the microfluidic channel top cover and the edge of the microfluidic channel bottom plate are connected with the microfluidic channel wall, a reference thermocouple and a main thermocouple are arranged inside the microfluidic channel cavity, and a heater and a grounding point are arranged on both sides of the top of the microfluidic channel bottom plate. The sensor of the present invention contains a microfluidic channel with a suspended bridge structure, which realizes the improvement of sensitivity and the reduction of heat loss; the sensitive measurement of small volume liquid samples is performed through the microfluidic measurement chamber to minimize the loading dose of biofluidic samples, which will help portable medical care applications.
Description
Technical Field
The invention relates to the field of thermal sensors, in particular to a multi-runner thermal sensor with a micro-suspension structure and a preparation method thereof.
Background
A thermal sensor is a device that can collect information analyzing the temperature difference of a sample to be detected from a detection element. With the development of subjects such as material science and electronic science, thermal sensors become research hot spots, and in recent years, various novel thermal detection sensors with excellent performance are appeared, and requirements on the precision, detection speed and volume of the thermal sensors are also higher and higher. With the development of integration technology, it is becoming a trend to provide a sensor with small size, light weight, and high detection accuracy.
With the development of Micro-Electro-MECHANICAL SYSTEM, MEMS, higher requirements are put on the performance and processing technology of various microstructures due to the requirements of the Micro-system performance or structure. The micro-suspension structure has wide requirements because of being capable of effectively avoiding intermolecular and surface effects and heat transfer between the micro-suspension structure and the substrate and increasing the contact area with the surrounding environment. The suspension structure is relatively isolated from the substrate, so that heat flow caused by other external factors can be reduced to the greatest extent, and the detection precision of the sensor is improved. The suspension structure is combined with the thermal sensor, so that the heat dissipated in heat transfer can be effectively detected, and the detection precision and sensitivity of the sensor are improved.
Existing processes for manufacturing suspended structures between microstructures include bulk silicon process etching, electrospinning, chemical vapor deposition, etc., often have high process costs due to the high equipment or experimental conditions required, or it is difficult to establish an accurate and strong mechanical bond and efficient electrical contact between the suspended structures and the microstructures.
With the continuous promotion of MEMS technical level, compare in heavy traditional thermal sensor, micro-suspension structure thermal sensor with micro-channel structure and micro-suspension structure by virtue of MEMS technique combine together, have high performance, small, with low costs, a great deal of advantages such as stability height.
In micro-suspended thermal sensors, the sensor is typically fabricated on a suspended thin film structure to improve the thermal insulation of the device to improve the high sensitivity of the sensor, while the micro-fluidic channels are typically directly bonded over the sensor as a reservoir and reaction chamber for the reactant sample, facilitating manipulation of the reactant sample. The suspended structure can effectively improve the thermal insulation property of the device and reduce the heat capacity of the device, thereby increasing the thermal sensitivity of the device. At present, different substrate materials such as silicon, glass, polymer and the like are more mature to be applied to the processing and manufacturing of microfluidic structures. Silicon is a relatively common material with outstanding thermal stability, chemical inertness and good thermal conductivity, and a complete set of mature processing technology is currently available. The glass has 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. PDMS material is resistant to high and low temperature, does not harden at low temperature, does not deform and soften at high temperature, always keeps flexible characteristics, and has good dielectric property and certain ventilation effect. SU-8 materials have high transparency at certain wavelengths, large refractive index, low loss, and are considered good materials for optical waveguide applications.
In the current adopted microfluidic substrate materials, the preparation process of the silicon-based materials is mature, but the etching process is relatively complicated, the requirements on the environment are severe, the processing period is long, and the large-scale application of the processing technology is limited. Furthermore, suspended films based on silicon materials are very fragile and complex in manufacturing process. Glass, while transparent, is difficult to etch relative to the vertical cross-section of a silicon wafer due to its amorphous nature. Although both silicon and glass can be mass processed, the sealing process of 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 materials have better tensile strength and lower thermal conductivity, and are easier to prepare into film structures. However, polymer materials have the disadvantage that surface modification is generally required and most are not resistant to high temperatures. While PDMS is a good 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 demoulded. The prepared PDMS fluid structure requires an adhesion process integrated with the sensor chip, which needs to ensure sealability and is difficult to adhere to the suspended microstructure. And the load force of the PDMS fluid system chip can damage the suspension structure of the thermal sensor, and the method is applied to the suspension structure of the micro-sensor device.
SU-8 based cantilevers exhibit higher resistance to temperature changes than other cantilevers, which can reduce noise and increase sensitivity. The micro fluidic system of the microsensor device was fabricated using SU-8 polymers due to their high chemical resistance. Preparation of a microchannel with a 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 increase sensitivity compared to conventional bulk PDMS chambers.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a multi-runner 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-runner thermal sensor with a micro-suspension structure, which comprises a micro-runner inlet, a micro-runner and a micro-runner outlet, wherein a plurality of micro-runners are communicated between the micro-runner inlet and the micro-runner outlet, the micro-runner comprises a micro-runner top cover, a micro-runner wall and a micro-runner bottom plate, a suspension bridge structure substrate is arranged at the bottom of the micro-runner bottom plate, the micro-runner wall is connected with the edge of the micro-runner top cover and the micro-runner bottom plate, a micro-runner cavity is formed inside the micro-runner top cover, a reference thermocouple and a main thermocouple are arranged inside the micro-runner cavity, and a heater and a grounding part are respectively arranged at the two sides of the top end of the micro-runner bottom plate.
As a preferable technical scheme of the invention, the micro flow channels are uniformly distributed at intervals, and the interval is 200um.
As a preferable 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 micro-fluid channel is made of SU-8 photoresist.
The invention also provides a preparation method of the multi-channel thermal sensor with the micro-suspension structure, which comprises the following steps of;
s1, preparing a processing substrate, taking an insulating silicon wafer as a substrate, doping silicon dioxide into the silicon substrate by using an ion implantation process, and reducing the resistance of a sensor;
S2, preparing a separation layer, depositing a silicon dioxide film on a substrate to serve as the separation layer through a chemical vapor deposition technology, etching the silicon dioxide layer through a buffer 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 electrode of the heater;
s4, preparing a port of a thermocouple electrode, depositing a chromium/gold layer on the top through 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 micro-channels with the same structure, wherein the micro-channel wall and the separation layer are made of SU-8 photoresist, and preparing a top cantilever structure into a bridging structure through BHF etching and silicon etching;
s6, realizing a micro-channel coverage pattern, covering the SU-8 dry film on the substrate by using force and temperature control, and preparing a coverage film pattern on the channel by using a photoetching method;
and S7, preparing a cavity structure at the bottom of the silicon dioxide layer, and etching the bottom of the silicon dioxide layer to form a cavity at the bottom.
S8, stripping photoresist at the bottom of the silicon dioxide layer to finish the preparation of the MEMS thermal sensor with the cavity with the suspended structure
As a preferred embodiment of the present invention, in the step S1, the ion implantation condition of the silicon substrate is 100kev voltage and 1020cm -3 carrier concentration
Compared with the prior art, the invention has the following beneficial effects:
the sensor of the invention comprises a micro-fluid channel with a suspension bridge type structure, thereby realizing the improvement of sensitivity and the reduction of heat loss.
The invention carries out sensitive measurement on the small-volume liquid sample through the microfluidic measuring chamber so as to furthest reduce the loading dose of the biological fluid sample and apply the power-assisted portable medical care.
The sensor of the invention comprises a plurality of micro-fluid channels, can realize quick response and small-volume sample detection, can process a plurality of solutions at the same time for component detection, and solves the problems of less detection information and long processing time of the traditional MEMS thermal sensor.
And 4, the sensor can be produced in a one-time mass production mode by adopting a standard MEMS process, meanwhile, the manufacturing cost is low, the sensor can be produced without complex equipment, and the sensor has the potential of wide use.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic structural view of a MEMS thermal sensor of the present invention;
FIG. 2 is a schematic elevational view of a multi-channel thermal sensor of the micro-suspension structure of the present invention;
FIG. 3 is a structural exploded view 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 of the fabrication of a multi-channel thermal sensor of the micro-suspension structure of the present invention;
FIG. 5 is a response time of a microfluidic channel of a multi-channel thermal sensor of the micro-suspension structure of the present invention;
FIG. 6 is a sensitivity test result of a microfluidic channel of a multi-channel thermal sensor of the micro-suspension structure of the present invention;
In the figure, 1, a micro-channel inlet, 3, a micro-channel, 4, a micro-channel outlet, 6, a heater, 7, a micro-fluid channel upper top cover, 8, a micro-fluid channel wall, 9, a grounding part, 10, a micro-fluid channel bottom plate, 11, a reference thermocouple, 12, a main thermocouple, 13 and a micro-fluid channel cavity.
Detailed Description
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Example 1
As shown in fig. 1-3, the 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, the micro-channel 3 comprises a micro-channel top cover 7, a micro-channel wall 8 and a micro-channel bottom plate 10, a suspension bridge structure substrate is arranged at the bottom of the micro-channel bottom plate 10, the micro-channel wall 8 is connected at the edges of the micro-channel top cover 7 and the micro-channel bottom plate 10, a micro-channel cavity 13 is formed inside the micro-channel top cover, a reference thermocouple 11 and a main thermocouple 12 are arranged inside the micro-channel cavity 13, and a heater 6 and a grounding 9 are respectively arranged at the two sides of the top end of the micro-channel bottom plate 10.
Further, the micro flow channels 3 are uniformly distributed at intervals, and the interval is 200um.
Further, the micro-fluid channel cavity 13 is strip-shaped, the volume in the middle is larger than that of the two sides, the square containing cavity is arranged in the middle, the side length is 500um, the height is 50um, and the micro-channel 3 is made of SU-8 photoresist.
Specifically, the heater 6 is matched with the ground 9 for evaluating after the sensor is produced and simulating the generated reaction heat, when the thermal sensor starts to work, firstly, eye fluid of a patient to be tested is injected into the micro-channel inlet 1 by a titration method, each micro-channel 3 is respectively injected by a shunt so that the solution fills the whole micro-fluid channel cavity 13 and the micro-channel, at the moment, 5 cavities are filled with various enzymes, the enzymes are placed in the middle area of the micro-fluid channel cavity 13, 1 is an experimental group, the rest 4 are control groups, different enzymes react with the solution to generate reaction heat, then the thermocouple 11 and the main thermocouple 12 are referred to sense heat, the released heat is detected, and finally, an electric signal is transmitted to a computer for processing.
As shown in fig. 4-6, the invention also provides a preparation method of the multi-channel thermal sensor with the micro-suspension structure, which comprises the following steps:
S1, referring to FIG. 4 (a), preparing a processing substrate, wherein a silicon-on-insulator (SOI) is used as a substrate, the thickness of the SOI is 10 μm, 1 μm and 400 μm respectively, and the device layer of the SOI substrate is N-type silicon;
s2, referring to FIG. 4 (b), preparing a separation layer, depositing a 500nm SiO 2 film on a substrate by chemical vapor deposition, etching the separation layer on a 500nm silicon dioxide (SiO 2) layer by using a buffer hydrofluoric acid (BHF) etching solution, and opening an ion implantation window to prepare a PN junction;
s3, referring to FIG. 4 (c), realizing electrode patterns of the heater and the 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 electrode of the heater;
S4, referring to FIG. 4 (d), preparing a port of a thermocouple electrode, depositing a 200nm chromium/gold (Cr-Au) layer on the top through a sputtering deposition method after a photoetching process, specifically, sputtering a 40nm thick chromium (Cr) layer on the front surface of 500 mu m thick silicon dioxide by using a sputtering device, sputtering a 160nm thick gold (Au) layer on the chromium (Cr) layer, finally completing depositing 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 keeping for 1 minute so as to realize ohmic contact of the thermocouple sensor;
S5 referring to FIG. 4 (e), a microchannel supporting wall is prepared, the microchannel has the same structure according to design, the microchannel wall and the separation layer are made of SU-8 photoresist, the etching is 50 μm, the SU-8 wall is manufactured on the substrate by the etching process after the cleaning process of the substrate, and the microchannel has a width of 50 μm and a height of 50 μm. Forming a top cantilever structure into a bridge structure by buffered hydrofluoric acid (BHF) etching and silicon etching;
S6, referring to FIG. 4 (f), a micro flow channel coverage pattern is realized, the thickness of a channel cover is prepared by a dried SU-8 film (50 μm), firstly, the dried SU-8 film with a support film is covered on a channel at 55 ℃ for 3 minutes, after 80 seconds of exposure, a substrate is pre-baked at 85 ℃ for 30 seconds, after that, the support film is moved, and the substrate is heated at 95 ℃ for 5 minutes to harden the pattern on the substrate;
s7, referring to FIG. 4 (g), preparing a cavity structure at the bottom of the silicon dioxide layer, etching the bottom of the silicon dioxide layer to form a cavity at the bottom, developing the SU-8 film by using SU-8 developing solution, washing the developing solution after 10min, and completing the preparation of the hollow structure on the substrate;
S8, referring to FIG. 4 (h), stripping photoresist at the bottom of the silicon dioxide layer, and preparing the MEMS thermal sensor with a bridge structure through a back silicon etching and buffer hydrofluoric acid (BHF) etching process.
After step S8, simulation software is used to perform simulation test on the MEMS thermal sensor, as shown in FIG. 5, and response time test is performed on the multi-target detection MEMS thermal sensor according to the embodiment, it can be seen that when step temperature is input, the sensor can react to temperature change quickly, the thermocouple detects the temperature change and outputs a response signal in less than 200ms, and then the response signal is converted into an electrical signal to be output, and the result shows that the thermal sensor has quick response and good thermal characteristics.
As shown in FIG. 6, the sensitivity test is performed on the multi-target detection MEMS thermal sensor in the embodiment, and the test result shows that the sensor has extremely high thermal characterization precision, so that the prepared microsensor can measure the catalytic reaction heat of enzyme, and the suspension bridge structure provided by the invention can improve the sensitivity of thermal detection.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007212390A (en) * | 2006-02-13 | 2007-08-23 | Kyushu Univ | Nanoscale thermal sensor and heating probe |
| CN217103071U (en) * | 2022-04-22 | 2022-08-02 | 四川大学 | A MEMS thermal sensor based on a single thermocouple and suspended microfluidics |
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| KR101152791B1 (en) * | 2010-05-10 | 2012-06-12 | 광주과학기술원 | Sensor for detecting heat generation of cells utilizing zweifach-fung effect and method of making the same |
| WO2016065361A2 (en) * | 2014-10-24 | 2016-04-28 | The Trustees Of Columbia University In The City Of New York | Mems-based calorimeter, fabrication, and use thereof |
| US10876903B2 (en) * | 2019-03-20 | 2020-12-29 | Xiang Zheng Tu | Multi-purpose MEMS thermopile sensors |
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