CN114107943A - Conductivity sensor based on boron-doped diamond film and preparation method thereof - Google Patents
Conductivity sensor based on boron-doped diamond film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a sensor based on a boron-doped diamond film, which comprises the following steps: s1, oxidizing the upper surface of the cleaned silicon wafer to generate a silicon dioxide layer; s2, soaking the substrate obtained in the step S1 in the nano-diamond powder suspension, taking out and drying the substrate, and depositing a boron-doped diamond film on the surface of the substrate by utilizing hot wire chemical deposition equipment; s3, depositing an aluminum mask layer on the surface by magnetron sputtering with aluminum as a target material; s4, coating photoresist on the aluminum mask layer, prebaking, photoetching, developing and postbaking to prepare a photoresist mask of the interdigital electrode pattern; s5, removing the aluminum mask layer without the protection of the photoresist mask; and S6, removing the boron-doped diamond film without the protection of the aluminum mask layer. The conductivity sensor of the interdigital electrode doped with boron diamond is prepared by taking the boron-doped diamond as an electrode material and combining with an interdigital electrode preparation process, and has ultra-low measuring range and durability.
Description
Technical Field
The invention belongs to the technical field of sensors, and relates to a conductivity sensor based on a boron-doped diamond film and a preparation method thereof.
Background
With the strong encouragement and promotion of new energy vehicles in China, the new energy vehicles have gone into thousands of households nowadays. The working voltage of the new energy vehicle is high, in order to ensure the safety of passengers and vehicles, the normal work of a high-low voltage electrical system needs to be ensured, the requirement of high insulation level is met, the conductivity of the battery cooling liquid is an important index for representing the performance of the cooling liquid, and the high-precision measurement of the ultralow-range conductivity is usually required within the range of 0-10 uS/cm.
The main conductivity measuring methods generally adopt an electrode measuring method, an electromagnetic induction measuring method and an ultrasonic measuring method, wherein the electrode measuring method is mainly based on the principle of solution conductivity to measure the conductivity by measuring the impedance of a solution, and the electrode and the measuring solution can generate complex electrochemical reaction during the measuring process to generate an electric double layer phenomenon. The electromagnetic induction type measuring method is based on the electromagnetic induction principle of an inductive sensor, a transmitting coil is used for generating voltage in a loop, and a receiving coil receives the induced voltage and generates current in the loop. Generally, sensors utilizing the electromagnetic induction principle have annular housings and do not use electrodes, but the sensors have poor interference resistance and narrow measurement range.
By adopting an electrode measurement method, the high-precision conductivity measurement is widely applied to the field of ocean monitoring. The domestic ocean conductivity tester mostly adopts a machining manufacturing process, for example, the high-precision four-electrode measuring range which is successfully developed by the national ocean technology center is 0-65 mS/cm, the precision reaches +/-0.007 mS/cm, the seven-electrode conductivity measuring system measuring range is 2-65mS/cm, and the precision reaches +/-0.005 mS/cm. Both of them are to improve the accuracy of the sensor by skillfully designing and adding a plurality of electrodes to reduce the error of measurement as much as possible. Due to the design, difficulty is brought to the design of a rear-end circuit, and due to the limitation of precision in the traditional machining and manufacturing method, the manufactured conductivity cell can form large random machining errors, so that a series of difficulties are brought to subsequent calibration work, the large-batch preparation cost is high, and the measurement range precision requirement and the low-cost preparation requirement of the conductivity measurement of the new energy automobile battery cooling liquid cannot be met.
An mems (micro Electro Mechanical system), abbreviated as a micro Electro Mechanical system, is a system that integrates a micro circuit and a micro machine on a chip according to functional requirements. The MEMS is based on traditional semiconductor technologies such as photoetching and corrosion, and is integrated with ultra-precise machining, so that the miniaturization and the batch of the sensor are realized, the consistency performance of the sensor is greatly improved, the production cost is reduced, and the space density and the coverage range of data detection are increased. At present, sensors are gradually developed towards miniaturization and integration, and MEMS sensors become the mainstream of sensor manufacturing technology due to the advantages of high sensitivity and easy integration. The conductivity sensor based on the MEMS process has the advantages of smaller detection limit, higher sensitivity, higher precision and better consistency.
The interdigital electrode structure is an interdigital structure, and the micro-spaced interdigital electrode is the most common micro-spaced electrode structure and is widely applied to the fields of nondestructive testing, electronic communication, chemical testing and the like. Since the chemical property of Pt is very stable and the Faraday impedance generated by the Pt electrode in the test is negligible, Pt is generally used as the interdigital electrode material. However, the Pt electrode is easy to fall off due to the difference of the thermal expansion coefficients of the Si substrate and the ceramic substrate and the glass substrate during long-term measurement and the generation of bubbles during water electrolysis.
Disclosure of Invention
Aiming at the defects of detection of ultralow range conductivity in liquid in the prior art, the invention provides a batch preparation method of a conductivity sensor which is miniaturized, super-sensitive and long in service life based on an interdigital electrode structure of a boron-doped diamond (BBD) film material combined with an MEMS (micro-electromechanical systems) processing technology, and the method makes up for the vacancy of the market.
One purpose of the invention is realized by the following technical scheme:
a conductivity sensor based on a boron-doped diamond film comprises a silicon substrate, a silicon dioxide insulating layer and a boron-doped diamond interdigital electrode which are sequentially arranged and paved from bottom to top.
The other purpose of the invention is realized by the following technical scheme:
a preparation method of a conductivity sensor based on a boron-doped diamond film comprises the following steps:
s1, cleaning the silicon wafer, and oxidizing the upper surface of the silicon wafer to generate a silicon dioxide insulating layer to obtain a substrate;
s2, soaking the substrate obtained in the step S1 in the nano-diamond powder suspension, taking out and drying the substrate, and then depositing a boron-doped diamond film on the surface of the substrate by utilizing hot wire chemical deposition equipment;
s3, depositing an aluminum mask layer on the surface of the boron-doped diamond film by using aluminum as a target material and adopting magnetron sputtering;
s4, coating photoresist on the aluminum mask layer, prebaking, photoetching, developing and postbaking to prepare a photoresist mask of the interdigital electrode pattern;
s5, removing the aluminum mask layer without the protection of the photoresist mask, and then removing the photoresist mask;
and S6, removing the boron-doped diamond film without the protection of the aluminum mask layer by using plasma dry etching, and then removing the residual aluminum mask layer.
Preferably, in step S1, the thickness of the insulating layer of silicon dioxide formed is 0.5 to 5 μm.
Preferably, in step S2, the nano-diamond powder suspension is formed by dispersing nano-diamond powder in an organic reagent, the nano-diamond powder has an average particle size of 1 to 100nm, and the organic reagent is acetone, absolute ethyl alcohol or the like.
Preferably, in step S2, the substrate is immersed in the nano-diamond powder suspension for 10-60 min.
Preferably, the deposition process parameters of the hot-wire chemical deposition equipment adopted in step S2 include: filament temperature is 2200-2400 ℃, methane is used as carbon source, and B is dissolved2O3C of (A)2H5OH gas is boron source gas, and the volume ratio of introduced methane, hydrogen and boron source gas is (1-5): 100: (3-6) the deposition time is 8-12 h.
Preferably, the thickness of the boron-doped diamond film deposited in the step S2 is 2-6 μm.
Preferably, the thickness of the aluminum mask layer deposited in step S3 is 300-500 nm.
Preferably, the method for removing the aluminum mask layer without the protection of the photoresist mask in step S5 includes: soaking the substrate in 70-85% phosphoric acid solution for 500-700 s at 55-65 ℃; the method for removing the photoresist mask comprises the following steps: soaking in concentrated sulfuric acid at 100-130 ℃ for 10-12 min.
Preferably, in the step S6, oxygen plasma dry etching is adopted for 30-60 min.
The other purpose of the invention is realized by the following technical scheme:
a method for detecting the conductivity of a solution, comprising the steps of:
preparing a standard solution for measuring the conductivity, immersing a packaged conductivity sensor based on the boron-doped diamond film into the standard solution for measuring the conductivity, connecting an external lead into an electrochemical workstation to apply current, collecting data, and calculating to obtain a conductivity cell constant;
and then immersing the packaged conductivity sensor based on the boron-doped diamond film into the solution to be measured, measuring the impedance of the solution to be measured at the same temperature, and calculating according to the constant of the conductivity cell to obtain the conductivity.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, the boron-doped diamond film is deposited on the substrate by adopting a hot wire chemical vapor deposition technology, and is combined with the substrate in a covalent bond form, so that the combination effect is tighter, the boron-doped diamond film is not easy to fall off, the sensor is beneficial to long-term durability, and the boron-doped diamond is taken as an electrode material to effectively prolong the service life of the sensor;
(2) the preparation of the boron-doped diamond interdigital electrode is successfully realized by adopting the technologies of a metal sputtering process, a Lift-Off process, phosphoric acid solution wet etching, oxygen plasma etching and the like;
(3) the conductivity sensor comprises a silicon substrate, a silicon dioxide insulating layer and a boron-doped diamond interdigital electrode which are sequentially arranged and paved from bottom to top, wherein the boron-doped diamond electrode is made into the interdigital electrode, and the sensitivity of the sensor for measuring the conductivity can be greatly increased by adopting the structure of the boron-doped diamond interdigital electrode;
(4) according to the invention, the conductivity sensor based on the boron-doped diamond interdigital electrode is prepared by taking the boron-doped diamond as an electrode material and combining a special interdigital electrode preparation process, has the advantages of ultra-low range, high sensitivity, durability and long service life, can be prepared in batch, obviously reduces the cost, and provides support for large-scale application of the conductivity sensor.
Drawings
FIG. 1 is a schematic structural view of a conductivity sensor based on a boron-doped diamond film according to the present invention;
FIG. 2 is a diagram of a process for preparing a conductivity sensor based on a boron-doped diamond film according to the present invention;
FIG. 3 is a graph of conductance data collected by an electrochemical workstation connected to a sensor of example 1 of the present invention as a function of the conductivity of a standard solution;
FIG. 4 is a plot of a straight line fit of the data from calibration experiments at low range for the sensor of example 1 of the present invention.
In fig. 1, a boron-doped diamond interdigital electrode; 2. a silicon dioxide insulating layer; 3. a silicon substrate.
Detailed Description
Hereinafter, embodiments will be described in detail with respect to the method for manufacturing a boron-doped diamond film-based conductivity sensor of the present invention, however, these embodiments are exemplary and the present disclosure is not limited thereto. And the drawings used herein are for the purpose of illustrating the disclosure better and are not intended to limit the scope of the invention.
The preparation method of the conductivity sensor based on the boron-doped diamond film is characterized by comprising the following steps of:
s1, cleaning the silicon wafer, and oxidizing the upper surface of the silicon wafer to generate a silicon dioxide insulating layer to obtain a substrate;
s2, soaking the substrate obtained in the step S1 in the nano-diamond powder suspension, taking out and drying the substrate, and then depositing a boron-doped diamond film on the surface of the substrate by utilizing hot wire chemical deposition equipment;
s3, depositing an aluminum mask layer on the surface of the boron-doped diamond film by using aluminum as a target material and adopting magnetron sputtering;
s4, coating photoresist on the aluminum mask layer, prebaking, photoetching, developing and postbaking to prepare a photoresist mask of the interdigital electrode pattern;
s5, removing the aluminum mask layer without the protection of the photoresist mask, and then removing the photoresist mask;
and S6, removing the boron-doped diamond film without the protection of the aluminum mask layer by using plasma dry etching, and then removing the residual aluminum mask layer.
Steps S1-S6 will be described in more detail below.
Step S1, preferably selecting a silicon wafer with a surface of (100) crystal plane and double-sided polishing, and preferably performing three cleaning steps: first step of cleaning, using H2SO4:H2O2Taking (6-8): 1 (mass ratio) as a cleaning solution, cleaning in the second step, and adopting NH4OH:H2O2:H2O is 1, (0.8-1.2) and (6-8) (mass ratio) as a cleaning solution, and the third step of cleaning is carried out by adopting HF and H2And O is 1 (40-60) (mass ratio) as a cleaning liquid. Thoroughly removing oxides on the surface of the silicon wafer by using three cleaning stepsOrganic matter, and the surface flatness of the silicon wafer is less than 0.1 μm after cleaning. After the silicon wafer is cleaned, preferably in an environment of 1000-1200 ℃, pure O is dried2Medium dry oxidation for 40-60 min in water vapor-containing O2And (3) medium-humidity oxidation for 400-500 min, and preferably preparing a silicon dioxide insulating layer with the thickness of 0.5-5 mu m on the surface of the silicon wafer.
And step S2, placing the substrate obtained in the step S1 in 70-90% alcohol for ultrasonic cleaning for 5-20 min, then soaking the substrate in a nano diamond powder suspension for 10-60 min, and self-assembling compact diamond grains on the substrate, wherein the nano diamond powder suspension is formed by dispersing nano diamond powder in an organic reagent, and the organic reagent is acetone, absolute ethyl alcohol and the like. Preferably, the average particle size of the nano-diamond powder is 1-100 nm, and the content of the nano-diamond powder in the nano-diamond powder suspension is 1-10 mg/ml. Taking out the substrate after soaking and drying, then placing the substrate in hot wire chemical deposition equipment, and depositing the boron-doped diamond film on the surface of the substrate, wherein the deposition process parameters of the hot wire chemical deposition equipment comprise: the filament temperature is 2200-2400 deg.C, the filament material can be tungsten, rhenium, tantalum, molybdenum, etc., the distance between the filament and the substrate is about 4-10 mm, methane is used as carbon source, and B is dissolved in the filament2O3C of (A)2H5OH gas is boron source gas, wherein, B2O3At C2H5The content of OH is 100-1000 ppm, and the volume ratio of introduced methane, hydrogen and boron source gas is (1-5): 100: (3-6), hydrogen flow rate is 150-250 sccm, vacuum degree of the reaction chamber is 1X 10-3～1×10-5mbar, deposition time is 8-12h, and the thickness of the deposited boron-doped diamond film is preferably 2-6 μm.
And step S3, using pure aluminum as a sputtering target material, using high-purity argon as sputtering gas, and depositing an aluminum mask layer on the surface of the boron-doped diamond film by using magnetron sputtering equipment, wherein the thickness of the deposited aluminum mask layer is preferably 300-500 nm.
And step S4, coating photoresist on the aluminum mask layer, wherein the coating thickness is preferably 1-3 μm, and performing pre-baking (at the temperature of 100-120 ℃ for 80-100S), photo-etching (with the exposure time of 10-20S), developing (with the developing time of 30-50S) and post-baking (at the temperature of 120-140 ℃ for 20-40 min) to prepare the photoresist mask with the interdigital electrode pattern.
And step S5, placing the substrate obtained in the step S4 in 70-85% phosphoric acid solution, soaking for 500-700S at 55-65 ℃, removing the aluminum mask layer without the protection of the photoresist mask, and exposing the boron-doped diamond film. And then soaking the photoresist mask in concentrated sulfuric acid at the temperature of 100-130 ℃ for 10-12 min to remove the residual photoresist mask, wherein the mass fraction of the concentrated sulfuric acid is preferably 92-98%.
And S6, preferably, performing dry etching for 30-60 min by adopting oxygen plasma, and fully removing the boron-doped diamond film without the protection of the aluminum mask layer. And then, placing the process piece into 70-85% phosphoric acid solution, and soaking for 500-700 s at 55-65 ℃ to remove the residual aluminum mask layer.
The process of preparing the conductivity sensor based on the boron-doped diamond film according to the steps S1-S6 of the present invention is shown in fig. 2. The schematic structural diagram of the conductivity sensor obtained by the preparation method of steps S1-S6 of the present invention is shown in fig. 1, and the silicon substrate 3, the silicon dioxide insulating layer 2 and the boron-doped diamond interdigital electrode 1 are sequentially laid from bottom to top. After scribing, routing and packaging, the conductivity sensor can be put into practical use.
According to the invention, the conductivity sensor comprising the silicon substrate, the silicon dioxide insulating layer and the boron-doped diamond interdigital electrode which are sequentially arranged and paved from bottom to top is successfully prepared by taking the boron-doped diamond as the electrode material and combining a special interdigital electrode preparation process, and the conductivity sensor has the advantages of ultra-low range, high sensitivity, durability and long service life.
The working principle and the testing method for measuring the conductivity by the conductivity sensor of the invention are as follows:
the boron-doped diamond interdigital electrode is designed in an interdigital mode, wherein one electrode is an excitation electrode and provides excitation voltage, and the other electrode is a reference electrode. When a voltage excitation signal with a certain amplitude is applied to the excitation electrode, ions in the solution move in the solution under the excitation action of an electric field, and a current is generated between the electrodes, so that the whole electrode-solution-electrode system has certain impedance and conductance in the process, and the conductance between the two electrodes and the conductivity of the solution are in a proportional relation, namely a proportionality coefficient, namely a conductivity cell constant. During measurement, the conductivity cell constant of the sensor is calibrated by measuring the resistance of a known solution, and the conductivity of the solution is determined by measuring the impedance conductance between the two electrodes after the conductivity cell constant is calibrated.
According to the preparation method of the calibration solution for measuring the conductivity of GB/T27502-2011, KCl and deionized water are used for preparing a standard solution for measuring the conductivity, the packaged conductivity sensor is slowly immersed in the standard solution (an experiment for preventing bubbles from being generated on the surface of the sensor to influence the experiment), an external lead is connected to an electrochemical workstation for collecting data, the test experiment is carried out at the room temperature of 25 ℃, and the conductivity cell constant of the sensor is obtained through calculation. And then slowly immersing the conductivity sensor into a solution to be measured, measuring the impedance of the solution to be measured at the room temperature of 25 ℃, and calculating according to the constant of the conductivity cell to obtain the conductivity.
The technical solutions of the present invention are further described and illustrated below by specific examples, it should be understood that the specific examples described herein are only for the purpose of facilitating understanding of the present invention, and are not intended to be specific limitations of the present invention. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1
The conductivity sensor of the present example was prepared by the following preparation method:
s1, selecting a four-inch silicon wafer with a (100) crystal face surface and double-sided polishing, and completely removing oxides and organic matters on the surface of the silicon wafer by using three cleaning steps: first step of cleaning, using H2SO4:H2O2Taking the mass ratio of 7:1 as a cleaning solution, cleaning in a second step, and adopting NH4OH:H2O2:H2Taking O-1: 1:7 (mass ratio) as a cleaning solution, and cleaning in the third step by adopting HF: H2And O is 1:50 (mass ratio) and is used as a cleaning solution to clean the silicon wafer. After cleaning, the surface flatness of the silicon wafer is less than 0.1 μm. Then in an environment of 1100 deg.CIn the presence of dry pure O2Medium dry oxidation for 50min in water vapor-containing O2And (4) carrying out medium-humidity oxidation for 450min to prepare a silicon dioxide insulating layer with the thickness of 2 mu m, thus obtaining the substrate.
S2, placing the substrate obtained in the step S1 in 75% alcohol for ultrasonic cleaning for 10min, then soaking the substrate in 5mg/ml nano diamond powder (average particle size is 20nm) acetone suspension for 30min, taking out the substrate after soaking, drying the substrate, and then placing the substrate in hot wire chemical deposition equipment, wherein the deposition technological parameters of the hot wire chemical deposition equipment comprise: filament temperature is 2300 ℃, methane is used as carbon source, and B is dissolved in the filament2O3C of (A)2H5OH gas is boron source gas, wherein, B2O3At C2H5The content of OH is 400ppm, and the volume ratio of introduced methane, hydrogen and boron source gas is 10: 200: 10, hydrogen flow of 200sccm, vacuum degree of the reaction chamber of 1X 10- 5mbar, deposition time of 10h, and deposition thickness of 4 μm boron-doped diamond film on the substrate.
And S3, depositing an aluminum mask layer with the thickness of 450nm on the surface of the boron-doped diamond film by using a magnetron sputtering device (the sputtering power is 200W, the pressure of the sputtering Ar gas is 0.2Pa, and the rotating speed of the substrate is 2r/min) with pure aluminum as a sputtering target material and high-purity argon gas as a sputtering gas.
S4, coating positive photoresist LC100A with the thickness of 2.4 microns on the aluminum mask layer, and performing pre-baking (the temperature is 110 ℃, the time is 90S), photoetching (the exposure time is 15S), developing (FHD-320 developing solution, the developing time is 40S) and post-baking (the temperature is 135 ℃, the time is 30min) to prepare the photoresist mask with the interdigital electrode pattern.
And S5, placing the substrate obtained in the step S4 in 80% phosphoric acid solution, soaking for 600S at 60 ℃, removing the aluminum mask layer without the protection of the photoresist mask, and exposing the boron-doped diamond film. Then soaking the substrate in 95% concentrated sulfuric acid at 120 ℃ for 10min to remove the residual photoresist mask.
And S6, performing dry etching for 45min by using oxygen plasma, and fully removing the boron-doped diamond film without the protection of the aluminum mask layer. The obtained substrate was placed in an 80% phosphoric acid solution and immersed for 600 seconds at 60 ℃ to remove the residual aluminum mask layer. And (4) scribing, routing and packaging to obtain the conductivity sensor.
Example 2
The conductivity sensor of the present example was prepared by the following preparation method:
s1, selecting a four-inch silicon wafer with a (100) crystal face surface and double-sided polishing, and completely removing oxides and organic matters on the surface of the silicon wafer by using three cleaning steps: first step of cleaning, using H2SO4:H2O2Taking 6:1 (mass ratio) as a cleaning solution, cleaning in a second step, and adopting NH4OH:H2O2:H2Taking O-1: 0.9:6 (mass ratio) as a cleaning solution, and cleaning in the third step by adopting HF: H2And O is 1:55 (mass ratio) and is used as a cleaning liquid to clean the silicon wafer. After cleaning, the surface flatness of the silicon wafer is less than 0.1 μm. Then drying the pure O in the environment of 1200 DEG C2Medium dry oxidation for 60min in water vapor-containing O2And (5) carrying out medium-humidity oxidation for 500min to prepare a silicon dioxide insulating layer with the thickness of 2.8 mu m, thus obtaining the substrate.
S2, placing the substrate obtained in the step S1 in 80% alcohol for ultrasonic cleaning for 15min, then soaking the substrate in 2mg/ml nano diamond powder (average particle size is 20nm) absolute ethyl alcohol suspension for 40min, taking out the substrate after soaking, drying the substrate, and then placing the substrate in hot wire chemical deposition equipment, wherein the deposition process parameters of the hot wire chemical deposition equipment comprise: filament temperature is 2200 ℃, methane is used as carbon source, and B is dissolved in the filament2O3C of (A)2H5OH gas is boron source gas, wherein, B2O3At C2H5The content of OH is 500ppm, and the volume ratio of introduced methane, hydrogen and boron source gas is 3: 100: 5 the hydrogen flow is 180sccm, the vacuum degree of the reaction chamber is 1X 10-4mbar, deposition time 12h, and deposition thickness of 4.3 μm boron-doped diamond film on the substrate.
And S3, depositing an aluminum mask layer with the thickness of 460nm on the surface of the boron-doped diamond film by using a magnetron sputtering device (the sputtering power is 250W, the sputtering Ar gas pressure is 0.2Pa, and the substrate rotating speed is 3r/min) with pure aluminum as a sputtering target material and high-purity argon gas as a sputtering gas.
S4, coating positive photoresist LC100A with the thickness of 2.5 microns on the aluminum mask layer, and performing pre-baking (the temperature is 120 ℃, the time is 80S), photoetching (the exposure time is 13S), developing (FHD-320 developing solution, the developing time is 45S) and post-baking (the temperature is 130 ℃, the time is 25min) to prepare the photoresist mask with the interdigital electrode pattern.
And S5, placing the substrate obtained in the step S4 in 75% phosphoric acid solution, soaking for 650S at 55 ℃, removing the aluminum mask layer without the protection of the photoresist mask, and exposing the boron-doped diamond film. And soaking the photoresist layer in 95% concentrated sulfuric acid at 120 ℃ for 12min to remove the residual photoresist mask.
And S6, performing dry etching for 50min by using oxygen plasma, and fully removing the boron-doped diamond film without the protection of the aluminum mask layer. The obtained substrate was immersed in a 75% phosphoric acid solution at 55 ℃ for 650 seconds to remove the residual aluminum mask layer. And (4) scribing, routing and packaging to obtain the conductivity sensor.
Minimum detection limit measurement
According to the preparation method of the calibration solution for measuring the GB/T27502-2011 conductivity, a series of standard solutions with the conductivities of 0.1 muS/cm within the range of 3.0 muS/cm-4.0 muS/cm are prepared by using KCl and deionized water, the packaged interdigital electrode sensor in the example 1 is slowly immersed in the standard solutions (the surface of the sensor is prevented from generating bubbles to influence the experiment), an external lead is connected to an electrochemical workstation to apply an excitation current with the frequency of 0.5 muA and 1kHz, the impedance of the solution is measured by the interdigital electrode at the room temperature of 25 ℃, and data are acquired and converted into conductance mapping analysis.
FIG. 3 is a graph of conductance data collected by an electrochemical workstation connected to a sensor of example 1 of the present invention as a function of the conductivity of a standard solution; the sensor can be intuitively seen in the figure, the sensor can very sensitively sense the conductivity change of the standard solution of 0.1 mu S/cm, the change of the measured conductivity value and the conductivity change form a linear relation, and the sensor can easily detect the conductivity of the standard solution of about 3.0 mu S/cm.
Sensor accuracy measurement
Several sets of standard solutions with conductivities ranging from 0 to 20 μ S/cm were prepared using KCl and deionized water according to the preparation method of the calibration solutions for conductivity measurement in GB/T27502-2011. The interdigital electrode sensor packaged in example 1 is slowly immersed in a standard solution (experiment for preventing bubbles from being generated on the surface of the sensor), an external lead is connected to an electrochemical workstation, excitation current with the frequency of 0.5 muA and the frequency of 1kHz is applied to acquire data, a test experiment is carried out at the room temperature and the environment of 25 ℃, and a fitting straight line is calibrated. And then slowly immersing the conductivity sensor into a solution to be measured, measuring the impedance of the solution to be measured at the room temperature of 25 ℃, and obtaining the measured conductivity value through calibrated fitting linear transformation.
FIG. 4 is a plot of a straight line fit of calibration experiments data at low range for the sensor of example 1 of the present invention; table 1 shows the parameters associated with fitting a straight line.
TABLE 1 parameters associated with fitting straight lines
| Fang Cheng | y＝a+bx |
| Drawing | Conductance of electricity |
| Weight of | Not weighted |
| Intercept of a beam | 2.93298±0.2000 |
| Slope of | 3.06312±0.014 |
| Sum of squares of residuals | 0.44299 |
| pearson's | 0.99992 |
It can be seen from fig. 4 and table 1 that the linear degree of calibration of the sensor is very good, which can reach more than 0.999.
Three groups of standard solutions to be measured with the conductivities of 5.08 muS/cm, 8.47 muS/cm and 9.98 muS/cm are respectively prepared, the conductivity sensor in the embodiment 1 is slowly immersed into the solution to be measured, the impedance of the solution to be measured is measured at the room temperature of 25 ℃, the conductivity is obtained by taking the reciprocal, and then the measured conductivity value is obtained by the conversion of a calibrated fitting straight line.
The readings of the impedance conversion into the conductance of the three collected by the electrochemical workstation are 19.0548780487805 mu S, 28.9100896212778 mu S and 33.2778702163062 mu S respectively, and the measured values are 5.26 mu S/cm, 8.48 mu S/cm and 9.91 mu S/cm obtained by calibrated linear conversion, so that the sensor has high accuracy.
Finally, it should be noted that the specific examples described herein are merely illustrative of the spirit of the invention and do not limit the embodiments of the invention. Various modifications, additions and substitutions for the embodiments described herein will occur to those skilled in the art, and all such embodiments are neither required nor possible. While the invention has been described with respect to specific embodiments, it will be appreciated that various changes and modifications may be made without departing from the spirit and scope of the invention, as defined by the appended claims.
Claims (10)
1. The conductivity sensor based on the boron-doped diamond film is characterized by comprising a silicon substrate, a silicon dioxide insulating layer and a boron-doped diamond interdigital electrode which are sequentially arranged and paved from bottom to top.
2. The method for preparing the conductivity sensor based on the boron-doped diamond film according to claim 1, comprising the following steps:
s1, cleaning the silicon wafer, and oxidizing the upper surface of the silicon wafer to generate a silicon dioxide insulating layer to obtain a substrate;
s2, soaking the substrate obtained in the step S1 in the nano-diamond powder suspension, taking out and drying the substrate, and then depositing a boron-doped diamond film on the surface of the substrate by utilizing hot wire chemical deposition equipment;
s3, depositing an aluminum mask layer on the surface of the boron-doped diamond film by using aluminum as a target material and adopting magnetron sputtering;
s4, coating photoresist on the aluminum mask layer, prebaking, photoetching, developing and postbaking to prepare a photoresist mask of the interdigital electrode pattern;
s5, removing the aluminum mask layer without the protection of the photoresist mask, and then removing the photoresist mask;
and S6, removing the boron-doped diamond film without the protection of the aluminum mask layer by using plasma dry etching, and then removing the residual aluminum mask layer.
3. The method according to claim 2, wherein in step S1, the thickness of the insulating layer of silicon dioxide is 0.5-5 μm.
4. The method according to claim 2, wherein in step S2, the nano-diamond powder suspension is formed by dispersing nano-diamond powder in an organic reagent, and the average particle size of the nano-diamond powder is 1 to 100 nm.
5. The method according to claim 2 or 4, wherein the substrate is immersed in the nano-diamond powder suspension for 10-60 min in step S2.
6. The method according to claim 2, wherein the deposition process parameters of the hot wire chemical deposition equipment adopted in the step S2 include: filament temperature is 2200-2400 ℃, methane is used as carbon source, and B is dissolved2O3C of (A)2H5OH gas is boron source gas, and the volume ratio of introduced methane, hydrogen and boron source gas is (1-5): 100: (3E >6) The deposition time is 8-12 h.
7. The preparation method according to claim 2, wherein the thickness of the boron-doped diamond film deposited in step S2 is 2 to 6 μm; the thickness of the aluminum mask layer deposited in step S3 is 300-500 nm.
8. The method of claim 2, wherein the step S5 of removing the aluminum mask layer without the protection of the photoresist mask comprises: soaking the substrate in 70-85% phosphoric acid solution for 500-700 s at 55-65 ℃; the method for removing the photoresist mask comprises the following steps: soaking in concentrated sulfuric acid at 100-130 ℃ for 10-12 min.
9. The preparation method of claim 2, wherein the step S6 is performed by oxygen plasma dry etching for 30-60 min.
10. A method for detecting the conductivity of a solution is characterized by comprising the following steps:
preparing a standard solution for conductivity measurement, immersing the packaged conductivity sensor based on the boron-doped diamond film according to claim 1 into the standard solution for conductivity measurement, connecting an external lead to an electrochemical workstation to apply current, collecting data, and calculating to obtain a conductivity cell constant;
then, the well-packaged conductivity sensor based on the boron-doped diamond film according to claim 1 is immersed in a solution to be measured, the impedance of the solution to be measured is measured at the same temperature, and the conductivity is obtained by calculation according to the conductivity cell constant.
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