CN102520012B - MEMS (Micro Electro Mechanical System) technology-based thermal diffusivity sensor chip and manufacturing method thereof - Google Patents
MEMS (Micro Electro Mechanical System) technology-based thermal diffusivity sensor chip and manufacturing method thereof Download PDFInfo
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- CN102520012B CN102520012B CN201110401838.8A CN201110401838A CN102520012B CN 102520012 B CN102520012 B CN 102520012B CN 201110401838 A CN201110401838 A CN 201110401838A CN 102520012 B CN102520012 B CN 102520012B
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Abstract
The invention provides an MEMS (Micro Electro Mechanical System) technology-based thermal diffusivity sensor chip and a manufacturing method thereof. The sensor chip comprises a silicon dioxide isolation layer deposited on the upper surface of an SOI (Silicon On Insulator) wafer, a heater and temperature sensors deposited on the upper surface of the silicon dioxide isolation layer and formed by etching, as well as silicon nitride protective layers which are deposited on the upper surface of the silicon dioxide isolation layer, the upper surface of the heater and the upper surfaces of the temperature sensors, wherein a heat insulation cavity is etched on the SOI wafer upwards from the lower surface to the lower surface; the heater is positioned in the central position of the upper surface of the silicon dioxide isolation layer; and the temperature sensors are uniformly distributed in the radial direction taking the heater as a center. According to the sensor chip provided by the invention, the thermal conductivity factor of fluids can be measured in dozens of seconds only by means of a few microliters of sample liquid, and the measurement can be realized in a large temperature range.
Description
Technical field
The present invention relates to the thermal diffusivity sensor chip based on MEMS (miniature electronic system) technology, particularly a kind of thermal diffusivity sensor chip based on MEMS technology and preparation method thereof, for measuring fluid thermal diffusivity.
Background technology
The method of measuring fluid thermal diffusivity is a lot, and thermal diffusivity is the important hereditary property of fluid, determine that the thermal diffusivity of fluid generally can be calculated and two kinds of approach of measuring by theory.Because the packed structures of fluid molecule does not also have complete theory, the formula that these estimations are supposed and more satisfactoryization of model, simplification, for complicated actual conditions not in full conformity with, often produce larger error, and these equations are generally only applicable to specific system and scope, many fluids still need test determination.Therefore, experiment measuring is the important channel of determining fluid thermal diffusivity, and typical measuring method has horizontal plate method, concentric drums method, heat-pole method, hot arrowband method, heat wire method etc.Instrument and data handling procedure that conventional thermal transient collimation method, Hot-strip Method are measured fluid thermal diffusivity are complicated, and need a large amount of samples, and Measuring Time is long.From precision, think at present and be preferably heat wire method, not only speed is fast, precision is high for the method, and can effectively reduce the impact of convection current, but the equipment of the method is more complicated, and the scope of application is also narrower, can not be for the mensuration of conducting liquid and the large fluid thermal diffusivity of viscosity, such as not measuring thermal diffusivity of crude oil and oil water mixture etc.
Continuous progress along with science such as sensor technology, electronic technology, MEMS technology, optical technology, fluid mechanics, computer technology, acoustics, advantageously promote the development of fluid thermal diffusivity measuring technique, emerged new thermal diffusivity measuring method and device.As adopt heat probe measurement method, and the method for the two heated filaments of transient state is carried out the measurement of thermal diffusivity etc., although above technology can improve measuring accuracy to a certain extent, but still existence needs, sample is too much, the time long or equipment complicated situation.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of thermal diffusivity sensor chip based on MEMS technology and preparation method thereof, by splashing into fluid sample, cover on well heater and sensor, utilize foreign current to heat well heater, then record the temperature variation curve of sensor and calculate its time constant, obtain thus the relation curve of time constant and flow thermal conductivity coefficient, with this, realize the measurement of thermal diffusivity.
The present invention is based on the thermal diffusivity sensor chip of MEMS technology, comprise the silicon dioxide separation layer that is deposited on SOI upper wafer surface, be deposited on silicon dioxide separation layer upper surface the well heater forming and temperature sensor after etching, and be deposited on silicon dioxide separation layer upper surface, the silicon nitride protective layer of well heater upper surface and temperature sensor upper surface, wherein, the lower surface of described SOI wafer is etched with insulation chambers from lower surface to its inside, described well heater is positioned at the center of silicon dioxide separation layer upper surface, the footpath that described temperature sensor is evenly distributed on centered by well heater makes progress, described silicon dioxide separation layer upper surface is provided with the metal lead wire being formed after etching by trace layer, and this metal lead wire adopts Ti/Cu double-decker, and metal lead wire causes pad by the two ends of the two ends of described well heater and temperature sensor respectively.
Described well heater and temperature sensor are formed by polysilicon; Described temperature sensor surrounds concentric structure centered by well heater; Described Ti layer thickness is 50～100nm.
The preparation method who the present invention is based on the thermal diffusivity sensor chip of MEMS technology comprises the following steps:
(1) dry method thermal oxide is carried out in the front of SOI wafer in tubular furnace at 850～1150 ℃ of temperature, at the upper surface of SOI wafer, form the silicon dioxide separation layer of thickness 0.1 μ m～0.3 μ m;
(2) the thick polysilicon of the positive deposit 0.2 μ m～0.3 μ m of device that adopts low-pressure chemical vapor phase deposition technology to obtain in step 1), by forming well heater and temperature sensor after photoetching and etching;
(3) in step 2) the positive etching fairlead of the device that obtains adopt sputtering technology in the thick Ti/Cu double-decker trace layer of front side of silicon wafer deposit 0.1 μ m～0.3 μ m, after photoetching and etching, form internal lead;
(4) the thick silicon nitride protective layer of the positive deposit 0.2 μ m～0.5 μ m of device obtaining in step 3) by low-pressure vapor phase deposition technology;
(5) chamber corrosion is carried on the back at the device back side that adopts wet etching technique to obtain in step 4), forms hot separate cavities;
(6) adopt photoetching and etching technics, the silicon nitride of chip-pad area is removed, reserve pad, so that follow-up signal connects;
(7) adopt gold ball bonding or aluminium wire wedge bonding Wire Bonding Technology that the pad of spun gold or aluminium wire and silicon pad and PCB card extender is coupled together.
Thermal diffusivity sensor chip that the present invention is based on MEMS technology and preparation method thereof at least has the following advantages: invention sensor chip layout adopts the positive square well heater of central authorities, and temperature sensor is for annular and be distributed in different radial positions.Measure and adopt instantaneous measurement method, this invention sensor chip is placed in the controlled constant temperature oven of temperature, detected fluid is got microlitre magnitude by transfer pipet and is dripped on chip.During measurement, set an initial temperature, make temperature constant in constant temperature oven in initial temperature value.When well heater is during with the heating of constant heating power, the time dependent relation of temperature that temperature sensor is surveyed is not identical, thereby yet corresponding different time constant.In permanent power heating process, with datalogger, set regular hour step-length, by continuous record, each measures the measured temperature of temperature sensor constantly, thereby obtain one group of data value of temperature and time, by Correlation method for data processing method, obtained again the matched curve of data and time, determine its time constant.Finally by the funtcional relationship between coefficient of diffusion and time constant, try to achieve the thermal diffusivity α of sample.This sensor chip only needs the sample liquids of several microlitres can in tens seconds, complete the measurement of measuring flow thermal conductivity coefficient, and can very in large-temperature range, realize measurement.
Accompanying drawing explanation
Fig. 1 is the cut-open view that the present invention is based on the thermal diffusivity sensor chip of MEMS technology;
Fig. 2 is the planimetric map that the present invention is based on the thermal diffusivity sensor chip of MEMS technology;
Fig. 3 is the encapsulating structure figure that the present invention is based on the thermal diffusivity sensor chip of MEMS technology.
Label in figure represents as follows:
| 1 | Sample liquid | 2 | Silicon nitride |
| 3 | Silicon |
4 | |
| 8 | Well |
9 | Silicon dioxide buried |
| 10 | |
11 | |
| 12 | |
13 | Pad |
Embodiment
Below in conjunction with accompanying drawing, thermal diffusivity sensor chip that the present invention is based on MEMS technology and preparation method thereof is described in detail:
With reference to Fig. 1, the primary structure of sensor chip of the present invention comprises that (SOI wafer comprises body silicon 11 to SOI wafer, be deposited on the silicon dioxide buried regions 9 of body silicon 11 upper surfaces, and the top layer silicon 10 that is deposited on silicon dioxide buried regions 9 upper surfaces), be deposited on the silicon dioxide separation layer 3 of SOI wafer top layer silicon upper surface, be deposited on well heater 8 and the temperature sensor 4 of silicon dioxide separation layer 3 upper surfaces, and be deposited on silicon dioxide separation layer 3 upper surfaces, the silicon nitride protective layer 2 of well heater upper surface and temperature sensor upper surface, wherein, the body silicon 11 of described SOI wafer upwards caves in and is provided with insulation chambers 12 from lower surface.During test, sample liquid 1 drops on sensor chip of the present invention.
With reference to Fig. 2, plane structure chart for sensor chip of the present invention, as we know from the figure, well heater 8 is positioned at center, 8 temperature sensors 4 surround two concentric circless centered by well heater 8, metal lead wire causes pad 13 by the two ends of the two ends of described well heater and temperature sensor respectively, like this, and by making radially equally distributed temperature sensor produce temperature-responsive rapidly and accurately to the heating of the foursquare well heater 8 in center.Well heater and temperature sensor are made by polysilicon, because the high value of polysilicon and resistance produce great variety with temperature.Therefore, thereby make well heater heating that heat is transmitted in testing liquid by foreign current, by the change in resistance of temperature sensor, can record the change curve of temperature and time, calculate the time constant of this curve, by test findings, can be set up the corresponding curve of thermal diffusivity and time constant, thereby realize the measurement of thermal diffusivity.
With reference to Fig. 3, the technological process of sensor chip of the present invention comprises the following steps:
1), dry method thermal oxide is carried out in the front of SOI wafer in tubular furnace at 850～1150 ℃ of temperature, by controlling oxidization time and temperature at the silicon dioxide separation layer 3 of the upper surface formation thickness 0.1 μ m～0.3 μ m of SOI wafer;
2), the thick polysilicon of the positive deposit 0.2 μ m～0.3 μ m of device that adopts low-pressure chemical vapor phase deposition (LPCVD) technology to obtain in step 1), by forming well heater 8 and temperature sensor 4 after photoetching and etching;
3), in step 2) the positive etching fairlead of the device that obtains adopt sputtering technology in the thick Ti/Cu double-decker trace layer of front side of silicon wafer deposit 0.1 μ m～0.3 μ m, after photoetching and etching, form internal lead;
4) the thick silicon nitride protective layer 2 of the positive deposit 0.2 μ m～0.5 μ m of device, obtaining in step 3) by low-pressure vapor phase deposition technology;
5), adopt the device back side (being the body silicon lower surface of SOI wafer) that wet etching technique obtains in step 4) to carry on the back chamber corrosion, form hot separate cavities 12;
6), adopt photoetching and etching technics, the silicon nitride of chip-pad area is removed, reserve pad, so that follow-up signal connects;
7), adopt the Wire Bonding Technology such as gold ball bonding or aluminium wire wedge bonding that the pad of spun gold or aluminium wire and silicon pad and PCB card extender is coupled together.
The groundwork principle of sensor chip is exactly to confirm the resistance of polysilicon temp sensor and the relation curve of temperature, obtains thus the relation between its time constant and thermal diffusivity, realizes the measurement of convection cell thermal diffusivity.In calibration process, sensor is inserted in a thermostatic container that can regulate temperature, and use a thermopair to confirm the real time temperature in constant temperature oven, the resistance of measuring temperature sensor with datalogger, the linear relationship that obtains resistance and temperature is roughly: R=a-bT, wherein a, b is constant, R is resistance, and T is temperature, by the curved line relation of resistance and temperature, can obtain its exact value.
Measuring method is instantaneous measurement method, and its fundamental measurement principle is: this chip is placed in the controlled constant temperature oven of temperature, and detected fluid is got microlitre magnitude by transfer pipet and dripped on chip.During measurement, set an initial temperature, and remain unchanged in whole measuring process chips environment temperature, even if the temperature constant in constant temperature oven is in initial temperature value.For the lower detected fluid of some boiling point, environment temperature setting value should be lowlyer advisable, in order to avoid fluid volatilizees in a large number, affects measurement result.When passing into electric current and make well heater with the heating of constant heating power, laterally and vertically spread simultaneously on hot-fluid edge in detected fluid, different fluid correspondences different thermal diffusivities, thermal diffusivity is larger, more along vertical heat transmission, fewer along lateral transport heat flux, the time dependent relation of temperature that temperature sensor is surveyed is not identical, thereby yet corresponding different time constant.In permanent power heating process, with datalogger, set regular hour step-length, by continuous record, each measures the measured value of temperature sensor constantly, thereby obtain one group of data value of temperature and time, by computing machine, by Correlation method for data processing method, obtained again the matched curve of data and time, determine its time constant.Finally by the funtcional relationship between thermal diffusivity and time constant, try to achieve the thermal diffusivity of sample.
The key technical indexes that the present invention can reach is as follows:
1, measuring media: fluid;
2, precision: be better than ± 0.5%FS;
3, working temperature: 0 ℃～200 ℃.
The present invention adopts the separation layer silicon dioxide of the uniformity forming through energetic oxygen ions implantttion technique, the well heater on upper strata and temperature sensor and silicon base are kept apart, avoided causing the unstable of sensor even to be lost efficacy because of the environment temperature leakage current causing that raises.Metal lead wire adopts the Ti/Cu double-decker of physical vapour deposition (PVD).The Ti of deposition 50nm～100nm thickness both can be used as adhesion layer, also can be used as restraining barrier, and while preventing hot operation, Cu-Si dissolves the component failure causing, can form good Ohmic contact with polysilicon contact district simultaneously.In order to coordinate the variation of above-mentioned metal lead wire geometric configuration and thickness, the graphical ICP high-density plasma dry etching technology that adopted of metal lead wire, thereby in the time of can effectively suppressing common wet etching, live width loss is larger, the problem that the undercutting of step place is serious, further strengthens the reliability of metal lead wire.
In addition, silicon dioxide separation layer of the present invention is arranged between well heater and SOI wafer isolates the two, like this, when well heater heats, has avoided affecting due to the transmission of hot temperature degree the performance of SOI wafer; In addition, because SOI wafer lower surface is provided with insulation chambers, therefore, the heat that SOI wafer absorbs is relatively little, has further improved the impact of temperature on SOI wafer.
Sensor chip layout of the present invention adopts the positive square well heater of central authorities, and temperature sensor is for annular and be distributed in different radial positions.Measure and adopt instantaneous measurement method, this invention sensor chip is placed in the controlled constant temperature oven of temperature, detected fluid is got microlitre magnitude by transfer pipet and is dripped on chip.During measurement, set an initial temperature, make temperature constant in constant temperature oven in initial temperature value.When well heater is during with the heating of constant heating power, the time dependent relation of temperature that temperature sensor is surveyed is not identical, thereby yet corresponding different time constant.In permanent power heating process, with datalogger, set regular hour step-length, by continuous record, each measures the measured temperature of temperature sensor constantly, thereby obtain one group of data value of temperature and time, by Correlation method for data processing method, obtained again the matched curve of data and time, determine its time constant.Finally by the funtcional relationship between coefficient of diffusion and time constant, try to achieve the thermal diffusivity α of sample.This sensor chip only needs the sample liquids of several microlitres can in tens seconds, complete the measurement of measuring flow thermal conductivity coefficient, and can very in large-temperature range, realize measurement.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading instructions of the present invention, is claim of the present invention and contains.
Claims (5)
1. the thermal diffusivity sensor chip based on MEMS technology, it is characterized in that: comprise the silicon dioxide separation layer (3) that is deposited on SOI upper wafer surface, the well heater that is deposited on silicon dioxide separation layer upper surface and forms after etching (8) and temperature sensor (4), and be deposited on silicon dioxide separation layer upper surface, the silicon nitride protective layer of well heater upper surface and temperature sensor upper surface (2), wherein, the lower surface of described SOI wafer is etched with insulation chambers (12) to its inside from lower surface, described well heater (8) is positioned at the center of silicon dioxide separation layer upper surface, the footpath that described temperature sensor is evenly distributed on centered by well heater makes progress, described silicon dioxide separation layer upper surface is provided with the metal lead wire being formed after etching by trace layer, and this metal lead wire adopts Ti/Cu double-decker, and metal lead wire causes pad by the two ends of the two ends of described well heater and temperature sensor respectively.
2. the thermal diffusivity sensor chip based on MEMS technology as claimed in claim 1, is characterized in that: described well heater and temperature sensor are formed by polysilicon.
3. the thermal diffusivity sensor chip based on MEMS technology as claimed in claim 1, is characterized in that: described temperature sensor surrounds concentric structure centered by well heater.
4. the thermal diffusivity sensor chip based on MEMS technology according to claim 1, is characterized in that: described Ti layer thickness is 50～100nm.
5. a preparation method for the thermal diffusivity sensor chip based on MEMS technology, is characterized in that: comprise the following steps:
(1) dry method thermal oxide is carried out in the front of SOI wafer in tubular furnace at 850～1150 ℃ of temperature, at the upper surface of SOI wafer, form the silicon dioxide separation layer of thickness 0.1 μ m～0.3 μ m;
(2) the thick polysilicon of the positive deposit 0.2 μ m～0.3 μ m of device that adopts low-pressure chemical vapor phase deposition technology to obtain in step (1), by forming well heater and temperature sensor after photoetching and etching;
(3) the positive etching fairlead of device obtaining in step (2) also adopts sputtering technology in the thick Ti/Cu double-decker trace layer of front side of silicon wafer deposit 0.1 μ m～0.3 μ m, after photoetching and etching, forms internal lead;
(4) the thick silicon nitride protective layer of the positive deposit 0.2 μ m～0.5 μ m of device obtaining in step (3) by low-pressure vapor phase deposition technology;
(5) chamber corrosion is carried on the back at the device back side that adopts wet etching technique to obtain in step 4), forms hot separate cavities;
(6) adopt photoetching and etching technics, the silicon nitride of chip-pad area is removed, reserve pad, so that follow-up signal connects;
(7) adopt gold ball bonding or aluminium wire wedge bonding Wire Bonding Technology that the pad of spun gold or aluminium wire and silicon pad and PCB card extender is coupled together.
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| CN103063877B (en) * | 2012-12-25 | 2014-08-20 | 西安交通大学 | Silicon substrate quartz acceleration sensor with temperature isolation structure |
| JP2016524713A (en) * | 2013-06-05 | 2016-08-18 | ザ トラスティーズ オブ コロンビア ユニバーシティ イン ザ シティ オブ ニューヨーク | MEMS calorimeter, its manufacture and use |
| CN103698357B (en) * | 2013-11-16 | 2016-10-19 | 西安交通大学 | A kind of thermal conductivity based on MEMS double-heater and thermal diffusion coefficient sensor |
| TWI521200B (en) * | 2014-01-29 | 2016-02-11 | 先技股份有限公司 | Calibration chemical sensing device |
| CN104155472A (en) * | 2014-07-18 | 2014-11-19 | 苏州能斯达电子科技有限公司 | Hot-film wind speed and wind direction sensor and preparation method thereof |
| DE102015225284A1 (en) * | 2015-12-15 | 2017-06-22 | Linseis Meßgeräte GmbH | Messchip and method for determining the thermal conductivity of a thin layer |
| CN106017713B (en) * | 2016-06-28 | 2020-04-24 | 中航电测仪器股份有限公司 | Temperature measuring resistor |
| CN107089638A (en) * | 2017-04-24 | 2017-08-25 | 广东美的制冷设备有限公司 | Microheater and its processing method |
| CN108158039B (en) * | 2018-01-03 | 2023-07-11 | 云南中烟工业有限责任公司 | MEMS heating chip integrated with multiple Pt temperature sensors and manufacturing method thereof |
| DE102018006868B4 (en) * | 2018-08-30 | 2020-03-19 | Diehl Metering Gmbh | Measuring device for determining the thermal conductivity of a fluid |
| CN111620300B (en) * | 2020-06-04 | 2023-07-28 | 绍兴中芯集成电路制造股份有限公司 | Device with back cavity structure and forming method thereof |
| DE102021213046B3 (en) | 2021-06-18 | 2022-10-27 | Linseis Messgeräte Gesellschaft mit beschränkter Haftung | Sensor, sensor system and method for detecting thermodynamic parameters of a sample and the use of the sensor or sensor system |
| CN115445032A (en) * | 2022-09-30 | 2022-12-09 | 杭州电子科技大学 | MEMS chip capable of atomizing nutrient solution |
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| CN1040577C (en) * | 1990-08-01 | 1998-11-04 | 涂相征 | Heat-flow sensor of integrated Si-membrane and making method thereof |
| US7878056B2 (en) * | 2007-12-19 | 2011-02-01 | Siargo Ltd. | Micromachined thermal mass flow sensor with self-cleaning capability and methods of making the same |
| CN101929968B (en) * | 2009-10-30 | 2012-07-18 | 中国计量科学研究院 | Device for measuring thermal diffusivity |
| US8827550B2 (en) * | 2009-12-23 | 2014-09-09 | Intel Corporation | Thermal sensor using a vibrating MEMS resonator of a chip interconnect layer |
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