CN113138049A - Integrated micro-nano sensor for water body temperature and salt depth detection and manufacturing method thereof - Google Patents
Integrated micro-nano sensor for water body temperature and salt depth detection and manufacturing method thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/04—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of resistance-strain gauges
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- 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
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/22—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a non-linear resistance, e.g. thermistor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/06—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of piezo-resistive devices
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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
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
Abstract
The temperature and salt depth integrated micro-nano sensor for detecting temperature, conductivity and pressure in a water body and the manufacturing method thereof are provided, the temperature and salt depth integrated micro-nano sensor comprises a silicon substrate (1) and a glass substrate (2) which are bonded together, wherein the silicon substrate (1) is respectively provided with a temperature sensor (3), a pressure sensor and a conductivity sensor (4); 2 transverse conductive areas (15) and 2 longitudinal conductive areas (16) formed by ion implantation doping are symmetrically arranged in a pressure sensing area and are connected through a metal conductive connecting wire, so that the resistance values of the conductive areas are the same, a Wheatstone bridge is formed, the 2 transverse conductive areas (15) and the 2 longitudinal conductive areas (16) are respectively used as four bridge arms of the Wheatstone bridge, a vacuum pressure groove (5) is formed on the back surface of the pressure sensing area on a bonding surface of a silicon chip (1), a pressure sensitive film (17) deformed when being pressed is formed, and the piezoresistive effect is generated when being pressed.
Description
Technical Field
The invention relates to an integrated micro-nano sensor for water body temperature and salt depth detection and a manufacturing method thereof, belonging to the technical field of sensors and environmental protection.
Background
A Temperature-Depth sensor (CTD sensor for short) is an important tool for measuring the physical characteristics of a water body mainly comprising ocean. At present, a temperature sensor in water body temperature and salinity (CTD) is widely used as a thermistor or a platinum resistor, and the temperature sensor is easy to manufacture, stable in performance and good in linearity. The conductivity sensor is mainly in an electrode type, current is induced by an external electric field, the magnitude of the current depends on the number of ions in the solution, and the detected output voltage is in direct proportion to the conductivity of the detected medium. The traditional pressure sensor has various measuring methods such as a piezoresistive method, a piezoelectric method, a capacitance method and the like, the piezoelectric method calculates the pressure by positive and negative charges induced by internal polarization when a dielectric layer senses the external pressure, and the pressure sensor has the advantages of small volume, high temperature resistance and the like, but cannot be used for static measurement. The capacitance method is to measure the change of internal capacitance caused by the deformation of the upper and lower electrode plates in the capacitor, and a specific circuit is required to measure the change of capacitance.
At present, cable type, ship fixed type and towed type thermohaline depth measuring equipment developed at home has a plurality of problems, such as complex equipment, huge volume, low integration level, low innovation, low instrument precision and the like, and the defects are urgently needed to be overcome along with the gradual promotion of the development strategy of the deep open sea.
The applicant of the present application filed an invention patent application entitled "an integrated micro-nano sensor and a manufacturing method thereof" in 2019, 01, 30, published in 2019, 05, 28, and the reference number is CN109813778A, and provides an integrated micro-nano sensor for rapid online detection of three parameters of pH, conductivity and temperature of a water body and a manufacturing method thereof, but the integrated micro-nano sensor lacks a pressure detection function. The invention can be regarded as a further development result on the basis of the technology.
Disclosure of Invention
The technical key point of the invention is to provide a temperature and salt depth integrated micro-nano sensor for detecting temperature, conductivity and pressure in a water body and a manufacturing method thereof.
In order to solve the technical problems, the technical scheme adopted by the temperature-salt depth integrated micro-nano sensor is as follows:
an integrated micro-nano sensor for water body temperature and salt depth detection comprises a Pyrex7740 glass substrate which can be bonded with a silicon substrate, wherein the silicon substrate which is provided with a crystal face with a surface of [100] and is polished and oxidized on two sides is covered on the glass substrate in a bonding mode, and the glass substrate and the silicon substrate are bonded into a whole; a temperature sensor, a pressure sensor and an electric conductivity sensor are respectively arranged in a temperature sensing area, a pressure sensing area and an electric conductivity sensing area on the upper surface of the silicon substrate; characterized in that the pressure sensor is arranged such that: the method comprises the following steps that 2 transverse conductive areas and 2 longitudinal conductive areas formed by ion implantation doping are symmetrically arranged on the two transverse sides and the two longitudinal sides of a pressure sensing area respectively, metal conductive connecting wires prepared by sputtering and Lift-off processes are arranged between the conductive areas on the upper surface of the pressure sensing area and are connected, so that the resistance values of the conductive areas are the same, a Wheatstone bridge is formed, the 2 transverse conductive areas and the 2 longitudinal conductive areas are used as four bridge arms of the Wheatstone bridge respectively, a bonding surface of a silicon substrate is hollowed inwards on the back surface of the pressure sensing area through wet etching to form a vacuum pressure groove, and the pressure sensing area becomes a pressure sensitive film with micron-sized thickness and deformed when encountering pressure; when the pressure sensing area is pressed, the 2 transverse conductive areas and the 2 longitudinal conductive areas are pressed and deformed to generate a piezoresistive effect to become piezoresistive sensing strips of four bridge arms of the Wheatstone bridge, the pressure signal is converted into a resistance value signal, namely an electric signal, the metal conductive connecting line is connected with the piezoresistive sensing strips of the four bridge arms in ohmic contact, and the resistance value signal is transmitted through the metal conductive connecting line.
The following is a further scheme of the temperature-salt depth integrated micro-nano sensor of the invention:
the piezoresistive sensing strip is formed by implanting and doping boron ions, and comprises a light doping area with low doping density and a heavy doping area with high doping density, wherein the doping depths are all nano-scale, and the doping depth is also called doping junction depth, which is called junction depth for short. The lightly doped regions are repeatedly arranged back and forth in the area of the region in a slender strip-shaped snake-like mode along the [110] direction of the surface of the silicon substrate with the crystal direction being [100], the resistance value of the lightly doped region is far greater than that of the heavily doped region, and the lightly doped region is a main body for sensing external pressure; the heavily doped region is a connecting point of bridge arm resistors of the Wheatstone bridge, is arranged in a square shape, has a width larger than that of the lightly doped region, and is used for compensating errors caused by Poisson effect when the piezoresistive effect of the ion injection lightly doped region occurs and increasing the area of the ion injection lightly doped region; the metal conductive connecting line is a metal aluminum connecting line. The Wheatstone bridges are respectively provided with a junction block used as an external connecting wire at 4 corners of the pressure sensing area.
The 2 transverse conductive regions and the 2 longitudinal conductive regions are longitudinally arranged in the light doped region in the shape of a strip.
The length and width of the light doped region and the heavily doped region are micron-sized, the thickness of the metal aluminum connecting wire is micron-sized, the length and width of the metal aluminum connecting wire is millimeter-sized aluminum thin layer, and the doping density of the heavily doped region is 8-12 times that of the light doped region; the vacuum pressure groove is an open groove with the length, width and height of a millimeter level formed by etching the back surface of the silicon substrate [100] by a wet etching process; the temperature sensor and the conductivity sensor are platinum thin layers which are directly formed by a Lift-off process and have the thickness of a nanometer level and the length and the width of a micrometer level.
The thickness of the pressure sensitive film of the silicon substrate pressure sensing area is 50 um to 100 um.
The temperature sensor is formed by arranging a section of platinum resistance wire serving as a thermistor on one area of the surface of the silicon substrate, and the conductivity sensor is formed by arranging 2 pairs of platinum electrodes on one area of the surface of the silicon substrate.
The platinum resistance wire forming the temperature sensor is a Pt1000 resistance wire, and the platinum resistance wire is repeatedly arranged back and forth in the area of the area where the platinum resistance wire is located in a slender strip-shaped snake-like mode on the upper surface of the silicon substrate, so that the resistance value is a set critical value when the length and the width of the whole section of the metal platinum wire forming the temperature sensor can reach the temperature of 0 ℃; and two ends of the platinum resistance wire are respectively provided with a junction block used as an external connection wire.
The 2 pairs of platinum electrodes serving as the conductivity sensor comprise 1 pair of inner ring platinum electrodes and 1 pair of outer ring platinum electrodes, the inner ring platinum electrodes comprise 1 inner ring annular platinum electrode and a connection platinum electrode thereof, and an inner ring broken ring platinum electrode and a connection platinum electrode thereof which surround the inner ring annular platinum electrode, the outer ring platinum electrodes comprise 1 first outer ring broken ring platinum electrode and a connection platinum electrode thereof, and a second outer ring broken ring platinum electrode and a connection platinum electrode thereof which surround the first outer ring broken ring platinum electrode, each connection platinum electrode leads to the edge of the silicon substrate, and the terminal of each connection platinum electrode is provided with a connection block which is used as an external connection wire.
The temperature sensor, the pressure sensor and the conductivity sensor are distributed on the upper surface of the silicon substrate in an arrayed manner, the pressure sensor is positioned in the center of the upper surface of the silicon substrate, and the temperature sensor and the conductivity sensor are respectively positioned on the left side and the right side of the pressure sensor; openings are formed in the areas where the temperature sensor, the pressure sensor and the conductivity sensor are located on the outer packaging silicon substrate, other parts are all packaged, and lead-out wires of all electrodes are led out.
In order to solve the technical problems, the manufacturing method of the temperature-salt-depth integrated micro-nano sensor adopts the following technical scheme:
a manufacturing method of an integrated micro-nano sensor for water body temperature and salt depth detection comprises the following steps of manufacturing a silicon substrate and bonding a glass substrate, wherein the manufacturing of the silicon substrate comprises the following steps:
selecting a silicon wafer with a surface of a [100] crystal face, which is polished and oxidized on a single side, as a silicon substrate material, wherein the surface of the silicon wafer is provided with a silicon oxide layer, the thickness of the silicon oxide layer is 2 microns, and the surface flatness of the silicon wafer is less than 1 micron;
secondly, spraying photoresist on the double surfaces of the substrate, photoetching and developing, and etching the silicon oxide layer by using BOE corrosive liquid to prepare a window for preparing a vacuum pressure tank;
step three, adopting 30% KOH corrosive liquid, carrying out anisotropic wet etching on the silicon layer at 50 ℃, preparing a vacuum pressure groove, and controlling the etching rate and the etching time to enable the bottom surface of the vacuum pressure groove to just cover the ion implantation heavily doped region;
etching the double-sided silicon nitride layer;
fifthly, generating a silicon oxide layer with the thickness of 60nm on the silicon wafer with the prepared cavity structure by using a gas phase deposition method Pecvd;
after photoetching, performing oxygen plasma treatment after lightly doping an ion implantation area, and then implanting boron ions into the area;
seventhly, after photoetching, performing oxygen plasma treatment after heavily doping an ion implantation area, and then implanting boron ions into the area;
step eight, etching the single-side silicon dioxide layer;
step nine, performing tube furnace annealing on the silicon wafer, performing photoetching-ohmic contact holes on the connecting positions of the piezoresistive strips and the Al metal connecting wires, and sputtering Al;
step ten, preparing a Ti adhesion layer required by a Pt electrode conducting layer and a lead wire on a silicon chip with a vacuum pressure groove by adopting sputtering and Lift-off processes;
step eleven, preparing a Pt electrode conducting layer and a lead wire by adopting sputtering and Lift-off processes;
step twelve, aligning the prepared silicon substrate with the glass substrate, and forming a micro-nano sensor plate-shaped aggregate in a silicon-glass anodic bonding mode;
thirteen, cutting a single sensor chip along the designed cutting line by adopting a silicon chip cutting machine;
and step fourteen, connecting each electrode lead by using gold wire ball bonding, conductive adhesive and the like, sealing all electrode lead interfaces by using epoxy adhesive, and only reserving a sensor electrode testing area for sample testing to finish the preparation of each device.
The pressure sensor adopts a piezoresistive method, mainly measures the resistance change caused by the external pressure on a sensitive piezoresistive membrane on a substrate, has a simple rear-end detection circuit, does not need excessive circuit elements, has good linearity, usually selects a silicon substrate as the substrate, adopts an ion implantation technology to dope boron ions on the front surface of the silicon substrate to form a piezoresistive strip, and when the sensor is subjected to the external pressure, the substrate can deform to drive the silicon piezoresistive strip to deform, the resistance value of the deformed piezoresistive strip changes, and the pressure can be obtained by measuring the resistance value of the piezoresistive strip. A cavity with a certain depth is etched on the reverse side of the silicon substrate by adopting a wet etching technology, and then the cavity is bonded with pyrex7740 glass to form an insulating cavity, the lower surface of the chip is fixed, the internal pressure of the cavity is fixed, and when the external pressure is greater than the internal pressure of the cavity, the upper surface of the silicon chip bends towards the cavity to drive the piezoresistive strips to deform.
The CTD sensor manufactured by the invention is used in water body detection, based on the characteristics, a micro-nano manufacturing technology is adopted, a vacuum cavity is etched by utilizing the anisotropic corrosion characteristic of [100] crystal orientation silicon, a P-type silicon piezoresistive membrane is prepared on a substrate, a Wheatstone bridge is formed by interconnection on the substrate, a pressure sensor is formed by bonding silicon glass anodes, a Pt1000 resistance wire is prepared as a temperature sensor, 4 Pt annular electrodes form a conductivity sensor, the volume of the manufactured three-parameter sensor is only centimeter square, the three-parameter sensor is easy to integrate with a back end circuit, and the power consumption is low.
The sensor provided by the invention has the following obvious advantages: 1) the sensitivity is high. The pressure-sensitive resistance film patterned on the surface of the silicon wafer forms a Wheatstone bridge, the output impedance is low, the noise interference resistance is strong, the vacuum environment required by the anodic bonding process is favorable for forming a vacuum cavity, the accuracy of absolute pressure measurement is effectively improved, and the detection sensitivity of the sensor is improved; 2) and (4) multi-parameter integration. The sensor realizes single-chip multi-parameter measurement, improves the utilization rate of the area of the silicon chip, is beneficial to reducing the production cost, and simultaneously detects multiple parameters to ensure the measurement accuracy at the same time; 3) high batch consistency, low cost and easy integration. The sensor is manufactured based on the MEMS technology, three parameters of temperature, conductivity and pressure on a silicon substrate are integrated and prepared in batches, the manufacturing cost is reduced, the chip sensor is easy to integrate and package with a rear-end acquisition circuit to form a miniature sensor module, online detection or online monitoring can be realized after networking, and the sensor is particularly suitable for the requirement of measuring the environmental parameters of the ocean thermocline and the saltus layer.
Drawings
FIG. 1 is a front perspective view of the overall structure of a micro-nano sensor according to the invention;
FIG. 2 is a back perspective view of the overall structure of the micro-nano sensor according to the invention;
FIG. 3 is a schematic front perspective view of a silicon substrate;
FIG. 4 is a schematic perspective view of the backside of a silicon substrate;
FIG. 5 is a schematic cross-sectional perspective view of a micro-nano sensor according to the invention;
FIG. 6 is a schematic front view of a silicon substrate;
FIG. 7 is a schematic diagram of a process flow for preparing a micro-nano sensor;
FIG. 8 is a schematic diagram of a Wheatstone bridge;
fig. 9 is a schematic diagram of the operating principle of the piezoresistive pressure sensor.
And (4) prompting: the thickness of each sensor electrode, the metal aluminum connecting wire and the connecting block serving as an external connecting wire formed on the silicon substrate are all in the nanometer level, and the thicknesses of the sensor electrodes, the metal aluminum connecting wire and the connecting block serving as the external connecting wire are exaggerated and displayed to be visible to naked eyes in the figure. The lightly doped regions and the heavily doped regions of the piezoresistance sensing strips of the four bridge arms of the Wheatstone bridge on the silicon substrate are actually doped inwards from the upper surface of the silicon substrate, the doping depth is nanoscale, and the lightly doped regions and the heavily doped regions are displayed as upward bulges which can be seen by naked eyes for making the lightly doped regions and the heavily doped regions obvious.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
The integrated micro-nano sensor for water body temperature and salt depth detection comprises a Pyrex7740 glass substrate 2 which can be bonded with a silicon substrate 1, wherein the silicon substrate 1 with a surface of a [100] crystal face, double-side polishing and oxidation is covered on the glass substrate 2 in a bonding mode, and the glass substrate and the silicon substrate are bonded into a whole, as shown in figures 1 and 2. A temperature sensor 3, a pressure sensor and a conductivity sensor 4 are respectively disposed in a temperature sensing area, a pressure sensing area and a conductivity sensing area on the upper surface of the silicon substrate 1.
The pressure sensor is arranged as follows: as shown in fig. 1 and 3, 2 transverse conductive regions 15 and 2 longitudinal conductive regions 16 formed by ion implantation doping are symmetrically disposed on both sides of the upper surface of the silicon substrate 1, respectively, and metal conductive connection lines prepared by sputtering and Lift-off process are disposed between the conductive regions on the upper surface of the pressure sensing region for detection, so that the resistance values of the conductive regions are the same, and a wheatstone bridge as shown in fig. 7 is formed in principle. As shown in fig. 6, 2 transverse conductive regions 15 and 2 longitudinal conductive regions 16 respectively serve as four arms of the wheatstone bridge.
As shown in fig. 4 and 5, the bonding surface of the detection silicon substrate 1 is hollowed out by wet etching on the back surface of the pressure sensing area to form a vacuum pressure groove 5, so that the remaining part of the pressure sensing area becomes a pressure sensitive film 17 with micron-sized thickness and deformed when being pressed. The thickness of the pressure sensitive film 17 of the pressure sensing area of the silicon substrate 1 is 50 um to 100 um. When the pressure sensing area is pressurized, the 2 transverse conductive areas 15 and the 2 longitudinal conductive areas 16 are pressurized and deformed to generate a piezoresistive effect, so that the piezoresistive sensing strips of the four bridge arms of the wheatstone bridge are formed, pressure signals are converted into resistance value signals, namely electric signals, the detection metal conductive connecting lines are connected with the piezoresistive sensing strips of the four bridge arms in ohmic contact, and the resistance value signals are transmitted through the metal conductive connecting lines.
The integrated micro-nano sensor is used for detecting or monitoring the same point of a water body environment and simultaneously measuring three parameters, namely three parameters of temperature, pressure and conductivity.
The detection principle of the pressure sensor is shown in fig. 7 and 8, because the piezoresistive effect of the Si crystal is anisotropic, pulling force or pressure is applied along different directions of the crystal, and current is passed along different directions, the resistivity of the Si crystal is different, so that a wheatstone bridge can be formed by utilizing the anisotropic characteristic of the Si crystal. The formula is simplified by the silicon crystal piezoresistive effect:
the subscript l represents the machine direction, t represents the cross-machine direction,
representsThe piezoresistive coefficient of the pressure resistance coefficient,
representing strain.
As shown in FIG. 7, the piezoresistance coefficients of the resistors R1, R2, R3 and R4 along the [110] direction on the [100] crystal-oriented silicon wafer can be expressed as:
substituting the typical coefficients can result in:
n-type silicon:
=-31.2， 
=-17.6
p-type silicon:
=71.8， 
=-66.3
it can be known that the longitudinal coefficient and the transverse coefficient of the P-type silicon are just opposite and the values of the longitudinal coefficient and the transverse coefficient are close to each other, if the power-on direction of the P-type silicon resistor is the [110] direction, the resistance value of the P-type silicon resistor is increased when the strain direction is the longitudinal direction, and the resistance value of the P-type silicon resistor is decreased when the strain direction is the transverse direction, so that the P-type silicon resistor is very suitable for forming a Wheatstone bridge.
As shown in FIG. 6, the silicon wafer has a bottom-up orientation of [100]]Crystal orientation, up-down direction is [110]]In the direction, four P-type silicon resistors are formed after the ion implantation process, the ion implantation light doped regions of the four P-type silicon resistors are the same in area, and the heavy doped regions are the same in area, so that the resistance values of the four Wheatstone bridge arms formed by the four P-type silicon resistors are the same, and the four P-type silicon resistors are equally dividedThe silicon chip is distributed in a main stress area of a silicon chip sensitive film, the electrifying directions are consistent, when pressure is uniformly applied downwards from the upper surface of the chip, the upper and lower P-type silicon resistors are subjected to transverse strain, the resistance value is reduced, the left and right P-type silicon resistors are subjected to longitudinal strain, the resistance value is increased, the variation quantity is equal, if the P-type silicon resistors are connected through metal Al, a Wheatstone bridge is formed, and a constant voltage is applied to the input end of the bridge
As shown in fig. 7, the output voltage can be represented as:
wherein
Which is representative of the pressure applied to,
representing strain parameters, keeping the input voltage fixed, changing the magnitude of applied pressure, and carrying out a series of calibrations to obtain a linear equation of the output voltage value and the pressure, thereby completing the conversion from the pressure signal to the electric signal.
As shown in fig. 1 and 3, the detection piezoresistive sensing strip is formed by doping through boron ion implantation, and includes a lightly doped region 6 with low doping density and a heavily doped region 7 with high doping density, the doping junction depths are all nano-scale, the lightly doped region 6 is repeatedly arranged back and forth in the area of the region where the lightly doped region 6 is located in a slender strip-shaped zigzag manner along the [110] direction of the surface of the silicon substrate 1 with the crystal direction of [100], the resistance value of the lightly doped region 6 is far greater than that of the heavily doped region 7, and the detection piezoresistive sensing strip is a main body for sensing external pressure; the heavily doped region 7 is a connecting point of bridge arm resistors of the Wheatstone bridge, is arranged in a square shape, has a width larger than that of the lightly doped region 6, and is used for compensating errors caused by a Poisson effect when the piezoresistive effect of the ion injection lightly doped region 6 occurs and increasing the area of the ion injection lightly doped region 6; the metal conductive connecting line is a metal aluminum connecting line 8; the wheatstone bridge is provided with terminal blocks 9 serving as external connection lines at 4 corners of the pressure sensing area, respectively. The lightly doped regions 6 in the form of strips for detecting 2 transverse conductive regions 15 and 2 longitudinal conductive regions 16 are longitudinally arranged as shown in the figure.
As shown in fig. 6, the length and width of the detection lightly doped region 6 and the heavily doped region 7 are in the micrometer scale, the junction depth is in the nanometer scale, and the junction depth is preferably 100 nm. The doping density of the heavily doped region 7 is 8 to 12 times that of the lightly doped region 6; preferably, the matching is as follows: the ion implantation lightly doped region has a doping concentration of
The ion implantation heavily doped region has a doping concentration of
. The metal aluminum connecting wire 8 is an aluminum thin layer with the thickness of micron level and the length and the width of millimeter level. As shown in FIGS. 4, 5 and 6, the vacuum pressure groove 5 is detected as 100 for etching the silicon substrate 1 by a wet etching process]The back is formed with an opening slot with a length, width and height of millimeter level. The thickness of the pressure sensitive film 17 of the pressure sensing area of the test silicon substrate 1 is 50 um to 100 um.
The detection temperature sensor 3 and the conductivity sensor 4 are platinum thin layers which are directly formed by a Lift-off process and have the thickness of a nanometer level, the length of a millimeter level and the width of a micrometer level. As shown in fig. 1 and 3, the temperature detection sensor 3 is formed by arranging a platinum resistance wire as a thermistor on one region of the surface of the silicon substrate 1, and the conductivity sensor 4 is formed by arranging 2 pairs of platinum electrodes on one region of the surface of the silicon substrate 1. The platinum resistance wire forming the detection temperature sensor 3 is a Pt1000 resistance wire, and the detection platinum resistance wire is repeatedly arranged back and forth in the area of the region where the platinum resistance wire is located in a slender strip-shaped snake-like mode on the upper surface of the silicon substrate 1, so that the resistance value is a set critical value when the length and the width of the whole section of the metal platinum wire forming the temperature sensor 3 can reach the temperature of 0 ℃; the threshold value may be set to an integer value, such as 1000 Ω, 5000 Ω, or 10000 Ω. The two ends of the platinum resistance wire are respectively provided with a junction block 9 used as an external connection wire.
As shown in fig. 1 and 3, the 2 pairs of platinum electrodes as the conductivity sensor 4 include 1 pair of inner ring platinum electrodes and 1 pair of outer ring platinum electrodes, the inner ring platinum electrodes include 1 inner ring circular platinum electrode 10 and its connection platinum electrode 11, and an inner ring broken ring platinum electrode 12 and its connection platinum electrode 11 surrounding the inner ring circular platinum electrode 10, the outer ring platinum electrodes include 1 first outer ring broken ring platinum electrode and its connection platinum electrode 11, and a second outer ring broken ring platinum electrode 14 and its connection platinum electrode 11 surrounding the first outer ring broken ring platinum electrode 13, each connection platinum electrode 11 leads to the edge of the silicon substrate 1, and the terminal of each connection platinum electrode 11 is provided with a terminal block 9 for an external connection wire.
As shown in fig. 1 and 3, the detection temperature sensor 3, the pressure sensor and the conductivity sensor 4 are distributed on the upper surface of the detection silicon substrate 1 in an arrangement manner, the pressure sensor is located at the center of the upper surface of the detection silicon substrate 1, and the detection temperature sensor 3 and the conductivity sensor 4 are respectively located at the left side and the right side of the pressure sensor; openings are arranged in the areas where the temperature sensor 3, the pressure sensor and the conductivity sensor 4 are located on the detection outer packaging silicon substrate 1, other parts are all packaged, and lead-out wires of electrodes are led out through the wiring blocks 9.
The invention discloses a method for manufacturing an integrated micro-nano sensor for detecting the temperature and the salt depth of a water body, which respectively comprises the steps of manufacturing a detection silicon substrate 1 and detecting the bonding of a glass substrate 2, wherein the manufacturing of the detection silicon substrate 1 comprises the following steps:
selecting a silicon wafer with a surface of a [100] crystal face and a polished and oxidized single side as a silicon substrate 1 material, wherein the surface of the silicon wafer is provided with a silicon oxide layer, the thickness of the silicon oxide layer is 2 microns, and the surface flatness of the silicon wafer is less than 1 micron; as shown in fig. 9 a.
Secondly, spraying photoresist on the double surfaces of the substrate, photoetching and developing, and etching the silicon oxide layer by using BOE corrosive liquid to prepare a window for preparing the vacuum pressure tank 5; as shown in fig. 9 b.
Step three, adopting 30% KOH corrosive liquid, carrying out anisotropic wet etching on the silicon layer at 50 ℃, preparing a vacuum pressure tank 5, and controlling the etching rate and the etching time to enable the bottom surface of the vacuum pressure tank 5 to just cover the ion implantation heavy doping area 7; as shown in fig. 9 c.
Etching the double-sided silicon nitride layer; as shown in fig. 9 d.
Fifthly, generating a silicon oxide layer with the thickness of 60nm on the silicon wafer with the prepared cavity structure by using a gas phase deposition method Pecvd; as shown in fig. 9 e.
After photoetching, performing oxygen plasma treatment after lightly doping an ion implantation area, and then implanting boron ions into the area; as shown in fig. 9 f.
Seventhly, after photoetching, performing oxygen plasma treatment after heavily doping an ion implantation area, and then implanting boron ions into the area; as shown in fig. 9 g.
Step eight, etching the single-side silicon dioxide layer; as shown in fig. 9 h.
Step nine, performing tube furnace annealing on the silicon wafer, performing photoetching-ohmic contact holes on the connecting positions of the piezoresistive strips and the Al metal connecting wires, and sputtering Al; as shown in fig. 9 i.
Step ten, preparing a Ti adhesion layer required by the Pt electrode conducting layer and the lead wire on the silicon chip with the vacuum pressure groove 5 by adopting sputtering and Lift-off processes; as shown in fig. 9 j.
Step eleven, preparing a Pt electrode conducting layer and a lead wire by adopting sputtering and Lift-off processes; as shown in fig. 9 k.
Step twelve, aligning the prepared silicon substrate 1 and the glass substrate 2, and forming a micro-nano sensor plate-shaped aggregate in a silicon-glass anodic bonding mode; as shown in fig. 9 l.
And thirteen, cutting out a single sensor chip by a silicon chip cutting machine along the designed cutting line.
And step fourteen, connecting each electrode lead by using gold wire ball bonding, conductive adhesive and the like, sealing all electrode lead interfaces by using epoxy adhesive, and only reserving a sensor electrode testing area for sample testing to finish the preparation of each device.
When the integrated micro-nano sensor is used for detecting the temperature and the salt depth of the water body, a detection value is obtained through the reading circuit, and then the integrated micro-nano sensor is matched with the back end circuit for actual detection.
The invention discloses a sensor signal reading method and a parameter calibration method, which comprises the following steps:
(1) the temperature sensor measures resistance change of the Pt wire along with temperature change by adopting a Wheatstone bridge method, the temperature and the resistance have a linear relation, and a temperature value is obtained through the measured resistance value;
(2) the conductivity sensor is tested by loading 1kHz alternating signals, and is calibrated with temperature parameters to obtain a conductivity value;
(3) the pressure sensor measures the pressure, the pressure and the potential difference are in a linear relation, and the pressure and the temperature parameter are calibrated to obtain a final pressure value.
The structural design and layout of the three sensors involved in the invention have the following significant advantages:
(1) the three sensors are integrated on the same microchip, can measure and measure the environmental parameters of the same locus at the same time, is beneficial to back-end data analysis and parameter calibration, and improves the accuracy of measurement.
(2) The preparation process of the three sensors is compatible with a Micro Electro Mechanical System (MEMS) process, so that large-scale batch preparation can be realized, and the manufacturing cost of a single device is reduced. The Pt resistance wire of the temperature sensor, 4 Pt electrodes of the conductivity sensor and electrode leads of all the electrodes are finished on the [100] silicon substrate by one step through a metal sputtering and stripping process (Lift-off), and the vacuum pressure cavity is finished by a potassium hydroxide anisotropic wet etching process. The whole process flow is compatible with a Micro Electro Mechanical System (MEMS) process, and batch manufacturing of dozens to hundreds of devices at a time can be carried out on a 4-inch or 8-inch MEMS manufacturing platform.
The micro-nano sensor can be used for quickly detecting or monitoring three parameters of pressure, conductivity and temperature in water such as ocean, rivers, lakes, reservoirs and the like on line. The using method is the same as the existing on-line detection method of the similar micro-nano sensor.
Claims (10)
1. An integrated micro-nano sensor for water body temperature and salt depth detection comprises a Pyrex7740 glass substrate (2) which can be bonded with a silicon substrate (1), wherein the silicon substrate (1) with a crystal face (100) on the surface and polished and oxidized on two sides is covered on the glass substrate (2) in a bonding mode, and the glass substrate and the silicon substrate are bonded into a whole; a temperature sensor (3), a pressure sensor and an electric conductivity sensor (4) are respectively arranged in a temperature sensing area, a pressure sensing area and an electric conductivity sensing area on the upper surface of a silicon substrate (1); characterized in that the pressure sensor is arranged such that: 2 transverse conductive areas (15) and 2 longitudinal conductive areas (16) formed by ion implantation doping are symmetrically arranged on the two transverse sides and the two longitudinal sides of the pressure sensing area respectively, metal conductive connecting wires prepared by sputtering and Lift-off processes are arranged between the conductive areas on the upper surface of the pressure sensing area and are connected, so that the resistance values of the conductive areas are the same, a Wheatstone bridge is formed, the 2 transverse conductive areas (15) and the 2 longitudinal conductive areas (16) are respectively used as four bridge arms of the Wheatstone bridge, the bonding surface of the silicon substrate (1) is hollowed inwards on the back surface of the pressure sensing area by wet etching to form a vacuum pressure groove (5), and the pressure sensing area becomes a pressure sensitive film (17) with micron-sized thickness and deforming when encountering pressure; when the pressure sensing area is pressed, the 2 transverse conductive areas (15) and the 2 longitudinal conductive areas (16) are pressed and deformed to generate a piezoresistive effect to become piezoresistive sensing strips of four bridge arms of the Wheatstone bridge, pressure signals are converted into resistance signals, namely electric signals, the metal conductive connecting lines are connected with the piezoresistive sensing strips of the four bridge arms in ohmic contact and transmitted through the metal conductive connecting lines.
2. The integrated micro-nano sensor according to claim 1, wherein the piezoresistive sensing strips are formed by boron ion implantation doping, and comprise a lightly doped region (6) with low doping density and a heavily doped region (7) with high doping density, the doping junction depths are all nano-scale, the lightly doped regions (6) are repeatedly arranged back and forth in the area of the region in a slender strip-shaped zigzag manner along the [110] direction of the surface of the [100] silicon substrate (1) along the crystal direction, the resistance value of the lightly doped region (6) is far greater than that of the heavily doped region (7), and the piezoresistive sensing strips are main bodies for sensing external pressure; the heavily doped region (7) is a connecting point of bridge arm resistors of a Wheatstone bridge, is arranged in a square shape, has a width larger than that of the lightly doped region (6), and is used for compensating errors caused by a Poisson effect when the piezoresistive effect of the ion injection lightly doped region (6) occurs and increasing the area of the ion injection lightly doped region (6); the metal conductive connecting wire is a metal aluminum connecting wire (8); the Wheatstone bridge is respectively provided with a junction block (9) used as an external connecting wire at 4 corners of the pressure sensing area.
3. An integrated micro-nano sensor according to claim 2, characterized in that the 2 transverse conductive regions (15) and the 2 longitudinal conductive regions (16) are longitudinally arranged in the form of the elongated strip-shaped lightly doped region (6).
4. The integrated micro-nano sensor according to claim 2, wherein the length and width of the lightly doped region (6) and the heavily doped region (7) are micron-sized, the thickness of the metal aluminum connecting line (8) is a micron-sized aluminum thin layer with a length and width of millimeter-sized, and the doping density of the heavily doped region (7) is 8 to 12 times that of the lightly doped region (6); the vacuum pressure groove (5) is an open groove with the length, width and height of millimeter level formed by etching the back surfaces of the silicon substrates (1) (100) by a wet etching process; the temperature sensor (3) and the conductivity sensor (4) are platinum thin layers which are directly formed by a Lift-off process and have the thickness of a nanometer grade and the length and the width of a micrometer grade.
5. An integrated micro-nano sensor according to claim 1, characterized in that the thickness of the pressure sensitive membrane (17) of the pressure sensing area of the silicon substrate (1) is 50 um to 100 um.
6. The integrated micro-nano sensor according to claim 1, wherein the temperature sensor (3) is formed by arranging a section of platinum resistance wire as a thermistor on one area of the surface of the silicon substrate (1), and the conductivity sensor (4) is formed by arranging 2 pairs of platinum electrodes on one area of the surface of the silicon substrate (1).
7. The integrated micro-nano sensor according to claim 6, wherein the platinum resistance wire forming the temperature sensor (3) is a Pt1000 resistance wire, and the platinum resistance wire is repeatedly arranged back and forth in the area of the silicon substrate (1) in a slender strip-shaped snake-like manner on the upper surface of the silicon substrate, so that the resistance value is a set critical value when the length and the width of the whole section of the platinum wire forming the temperature sensor (3) can reach the temperature of 0 ℃; and two ends of the platinum resistance wire are respectively provided with a junction block (9) used as an external connection wire.
8. An integrated micro-nano sensor according to claim 6, characterized in that the 2 pairs of platinum electrodes as the conductivity sensor (4) comprise 1 pair of inner circle platinum electrodes and 1 pair of outer circle platinum electrodes, the inner circle platinum electrodes comprise 1 inner circle ring-shaped platinum electrode (10) and the platinum electrode (11) connected with the inner circle ring-shaped platinum electrode, an inner ring broken ring platinum electrode (12) surrounding the outer part of the inner ring circular ring platinum electrode (10) and a platinum electrode (11) connected with the inner ring broken ring platinum electrode, the outer ring platinum electrode comprises 1 first outer ring broken ring platinum electrode (13) and a platinum electrode (11) connected with the first outer ring broken ring platinum electrode, and a second outer ring broken ring platinum electrode (14) and a connecting platinum electrode (11) thereof which surround the first outer ring broken ring platinum electrode (13), wherein each connecting platinum electrode (11) leads to the edge of the silicon substrate (1), and a terminal of each connecting platinum electrode (11) is provided with a junction block (9) used as an external connecting wire.
9. The integrated micro-nano sensor according to claim 1, wherein the temperature sensor (3), the pressure sensor and the conductivity sensor (4) are distributed on the upper surface of the silicon substrate (1) in a arrayed manner, the pressure sensor is positioned at the center of the upper surface of the silicon substrate (1), and the temperature sensor (3) and the conductivity sensor (4) are respectively positioned at the left side and the right side of the pressure sensor; openings are formed in the areas where the temperature sensor (3), the pressure sensor and the conductivity sensor (4) are located on the outer packaging silicon substrate (1), other parts are all packaged, and lead-out wires of all electrodes are led out.
10. The manufacturing method of the integrated micro-nano sensor for water body temperature and salt depth detection comprises the steps of manufacturing the silicon substrate (1) and bonding the glass substrate (2), wherein the manufacturing of the silicon substrate (1) comprises the following steps:
selecting a silicon wafer with a polished and oxidized single surface with a (100) crystal face as a silicon substrate (1) material, wherein the surface is provided with a silicon oxide layer, the thickness of the silicon oxide layer is 2 microns, and the surface flatness of the silicon wafer is less than 1 micron;
secondly, spraying photoresist on the double surfaces of the substrate, photoetching and developing, and etching the silicon oxide layer by using BOE corrosive liquid to prepare a window for preparing a vacuum pressure tank (5);
step three, adopting 30% KOH corrosive liquid, carrying out anisotropic wet etching on the silicon layer at 50 ℃, preparing a vacuum pressure groove (5), and controlling the etching rate and the etching time to ensure that the bottom surface of the vacuum pressure groove (5) just covers the ion implantation heavy doping area (7);
etching the double-sided silicon nitride layer;
fifthly, generating a silicon oxide layer with the thickness of 60nm on the silicon wafer with the prepared cavity structure by using a gas phase deposition method Pecvd;
after photoetching, performing oxygen plasma treatment after lightly doping an ion implantation area, and then implanting boron ions into the area;
seventhly, after photoetching, performing oxygen plasma treatment after heavily doping an ion implantation area, and then implanting boron ions into the area;
step eight, etching the single-side silicon dioxide layer;
step nine, performing tube furnace annealing on the silicon wafer, performing photoetching-ohmic contact holes on the connecting positions of the piezoresistive strips and the Al metal connecting wires, and sputtering Al;
step ten, preparing a Ti adhesion layer required by the Pt electrode conducting layer and the lead wire on the silicon chip with the vacuum pressure groove (5) by adopting sputtering and Lift-off processes;
step eleven, preparing a Pt electrode conducting layer and a lead wire by adopting sputtering and Lift-off processes;
step twelve, aligning the prepared silicon substrate (1) with the glass substrate (2), and forming a micro-nano sensor plate-shaped aggregate in a silicon-glass anodic bonding mode;
thirteen, cutting a single sensor chip along the designed cutting line by adopting a silicon chip cutting machine;
and step fourteen, connecting each electrode lead by using gold wire ball bonding, conductive adhesive and the like, sealing all electrode lead interfaces by using epoxy adhesive, and only reserving a sensor electrode testing area for sample testing to finish the preparation of each device.
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