CN112881487A - Gold interdigital miniature electrochemical sensor and manufacturing method thereof - Google Patents
Gold interdigital miniature electrochemical sensor and manufacturing method thereof Download PDFInfo
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Images
Classifications
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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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention provides a gold interdigital micro electrochemical sensor and a manufacturing method thereof, wherein the gold interdigital micro electrochemical sensor comprises: the single crystal silicon substrate is of a first set thickness; a silicon dioxide layer with a second set thickness is arranged on the monocrystalline silicon substrate; the surface of the silicon dioxide layer is provided with interdigital electrode pairs, and the interdigital electrode pairs comprise a 10-20 nm nano titanium bonding layer and a 50-150 nm nano gold sensing layer from inside to outside. The manufacturing method adopts a manufacturing mode of integrated circuit micro-nano processing, takes silicon dioxide as an insulating substrate, and titanium/gold as a bonding layer/a sensing layer respectively, and is prepared by electron beam evaporation and metal stripping processes. And under the treatment of various organic reagent cleaning and vacuum low-temperature drying processes, gold interdigital micro electrochemical sensors with complete structural morphology and sensitive electrochemical characteristics are obtained in batches, the physical and chemical properties are more stable, the response is sensitive, and the gold interdigital micro electrochemical sensors can tolerate strong acid, strong alkali and various organic solutions.
Description
Technical Field
The invention relates to the technical field of manufacturing of chemical stability interdigital electrode sensors, in particular to a gold interdigital micro electrochemical sensor and a manufacturing method thereof.
Background
The micro interdigital electrode as a microelectrode has the advantages of simple structure, stable physicochemical property, quick response and output of detection signals, miniaturization, portability, high signal-to-noise ratio and the like, is sensitive, is separated from various planar electrodes, and is widely applied to the detection fields of electrochemical sensing, bioelectrochemical sensing, ion sensing and the like at present.
The traditional manufacturing process of the miniature interdigital electrode mostly uses electroplating, silk-screen printing and other processes for manufacturing and processing, although the methods are simple and easy to implement, a multi-interlayer electrode structure with controllable thickness is difficult to form, the accurate control on target heavy metal and detection precision is difficult to realize, and the microelectrode prepared by the traditional method is limited by the material and the process of the electrode, so that the electrode has the defects of no good environmental stress resistance, easy influence of ultrasonic vibration to damage the structure, poor tolerance on an organic solvent and the like, and the application of the interdigital miniature electrode in the field of sensing detection is greatly limited.
Disclosure of Invention
The embodiment of the invention provides a gold interdigital micro electrochemical sensor and a manufacturing method thereof, and aims to solve the problems that a micro interdigital electrode produced by a traditional manufacturing process is unstable in physical and chemical properties, poor in environmental stress resistance, easy to damage a structure by ultrasonic vibration and difficult to form a multi-interlayer electrode structure with controllable thickness.
The technical scheme of the invention is as follows:
in one aspect, the present invention provides a gold interdigital micro electrochemical sensor, comprising:
the single crystal silicon substrate is of a first set thickness;
a silicon dioxide layer with a second set thickness is arranged on the monocrystalline silicon substrate;
the surface of the silicon dioxide layer is provided with interdigital electrode pairs, and the interdigital electrode pairs comprise a 10-20 nm nano titanium bonding layer and a 50-150 nm nano gold sensing layer from inside to outside.
In some embodiments, the pairs of interdigitated electrodes are in a circular, zigzag, or parallel array.
In some embodiments, the ratio of the thickness of the nanotitanium adhesion layer to the nanogold sensing layer is 1: 8.
In some embodiments, the pairs of interdigitated electrodes are in a parallel array and the length of the interdigitated structure is 2700 μm, the width of the interdigitated structure is 2, 3, 5, 10 or 15 μm, and the duty cycle of the interdigitated structure is 1: 1.
In some embodiments, the second set thickness is 200 to 300 nm.
In another aspect, the present invention provides a method for manufacturing a gold interdigital micro electrochemical sensor, comprising:
carrying out thermal oxidation treatment on a monocrystalline silicon wafer with a set size to grow a silicon dioxide layer with a set thickness on the surface of the silicon wafer;
placing the silicon wafer subjected to thermal oxidation treatment in ethanol, soaking for a first set time, washing with deionized water, transferring the silicon wafer into an acetone solvent, soaking, washing with ultrasonic waves for a second set time, washing with deionized water, and drying with nitrogen;
coating photoresist on the surface of the silicon wafer and drying, carrying out photoetching and developing treatment on the silicon wafer by adopting a preset mask, transferring the interdigital array pattern to the silicon dioxide layer, and removing the residual photoresist on the interdigital array part on the surface of the silicon dioxide layer by using an oxygen plasma;
depositing 10-20 nm of nano titanium and 50-150 nm of nano gold on the silicon wafer after removing the glue in sequence by adopting an electron beam evaporation process;
and sequentially carrying out ultrasonic cleaning on the silicon wafer in acetone and ethanol, washing with deionized water, carrying out metal stripping and slicing to obtain the gold interdigital miniature electrochemical sensor.
In some embodiments, the method further comprises:
and (3) carrying out vacuum treatment on the gold interdigital micro electrochemical sensor obtained by slicing at 200 ℃ for 12 hours, and sealing and storing after the temperature is reduced to room temperature by a gradient of 20 ℃ per hour.
In some embodiments, performing a thermal oxidation process on a single crystal silicon wafer with a set size to grow a silicon dioxide layer with a set thickness on the surface of the silicon wafer comprises:
cleaning a monocrystalline silicon wafer by adopting hydrofluoric acid, and carrying out thermal oxidation treatment for 2 hours at the temperature of 900 ℃ so as to grow a silicon dioxide layer with the thickness of 300nm on the surface of the silicon wafer.
In some embodiments, the pattern of the interdigital array corresponding to the predetermined mask is a circular, a zigzag or a parallel array.
In some embodiments, the array of fingers is a parallel array, the fingers have a length of 2700 μm, the width of the finger structure is 2, 3, 5, 10, or 15 μm, and the duty cycle of the finger structure is 1: 1; the deposition thickness ratio of the nano titanium to the nano gold is 1: 8.
The invention has the beneficial effects that:
according to the gold interdigital micro electrochemical sensor and the manufacturing method thereof, the gold interdigital micro electrochemical sensor is based on an integrated circuit micro-nano processing manufacturing process, an interdigital electrode pair of a silicon dioxide layer, a nano titanium layer and nano gold is constructed, the thickness of each layer is finely controlled, and detection of heavy metal of a specified target and specified concentration is realized. The gold interdigital miniature electrochemical sensor manufactured by the manufacturing method has high processing precision and stable manufacturing process, and can realize large-scale batch preparation; meanwhile, gold is adopted as an electrode material, so that the electrode material is more stable in physical and chemical properties, sensitive in response, recyclable, rapid in regeneration and resistant to strong acid, strong alkali and various organic solutions. And is resistant to ultrasonic waves, having a robust physical structure.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic flow chart of the manufacturing process of the gold interdigital micro electrochemical sensor according to one embodiment of the present invention;
FIG. 2 is a schematic flow chart of a manufacturing method of the gold interdigital micro electrochemical sensor according to an embodiment of the present invention;
FIG. 3 is a graph of impedance curves of drinking water with different concentrations of manganese ions tested by 2 μm interdigital electrodes in accordance with an embodiment of the present invention;
FIG. 4 shows that the interdigital electrode test with different pitches in one embodiment of the present invention contains 200nmol/L-1Impedance curve of manganese ion drinking water.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings. The exemplary embodiments and descriptions of the present invention are provided to explain the present invention, but not to limit the present invention.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, elements, steps or components, but does not preclude the presence or addition of one or more other features, elements, steps or components.
It is also noted herein that the term "coupled," if not specifically stated, may refer herein to not only a direct connection, but also an indirect connection in which an intermediate is present.
The problem of environmental water resource safety has become a public health problem concerned all over the world, the problem that in recent years, various heavy metal ions represented by lead, arsenic, mercury, copper, manganese and the like are used as harmful pollutants in water is gradually intensified, the heavy metal ions are used as the environmental pollutants, are widely derived from waste water and waste gas generated in various industrial production, pesticide pesticides and the like used in agricultural production, various domestic garbage (batteries and discarded electrical appliances), enter human bodies through various channels such as drinking water, food intake and the like, and cause secretion functional disorder in the bodies, metabolic diseases and even cancers are caused, and the health of human beings is seriously damaged. Heavy metal particle pollutants are various in types and small in molecular weight, exist in trace and trace forms in water, and are effectively detected and quantified by the existing fresh and specific detection and quantification technology.
The interdigital array sensor is used as a good ion sensor and has good detection and quantification prospects for various heavy metal ions in an environmental water sample. Through the improvement of the manufacturing process of the interdigital and the materials of each bonding layer and each sensing layer, the electrochemical response signals for different heavy metal ions are sensitive, the operation and the recovery and regeneration are easy, the chemical stability of the electrode material can be improved, and the acid/alkali solution and organic solvent tolerance of the interdigital electrode is improved.
The invention provides a gold interdigital micro electrochemical sensor, which is shown in figure 1 and comprises the following components:
the single crystal silicon substrate is of a first set thickness; a silicon dioxide layer with a second set thickness is arranged on the monocrystalline silicon substrate; the surface of the silicon dioxide layer is provided with an interdigital electrode pair, and the interdigital electrode pair comprises a 10-20 nm nano titanium bonding layer and a 50-150 nm nano gold sensing layer from inside to outside. Preferably, in some embodiments, the interdigital electrode pair comprises a 10-15nm nanometer titanium bonding layer and a 70-80nm nanometer gold sensing layer from inside to outside.
In the embodiment, the interdigital electrode sensor substrate layer can adopt silicon, quartz or glass as the substrate. Wherein, the glass and the quartz have good surface adsorption and surface reaction capability, which is beneficial to surface modification. However, quartz is relatively expensive, and it is not easy to fabricate a strong metal electrode on glass, so silicon is used as a substrate in the present application, and particularly, a silicon wafer is used as a substrate in the fabrication process. In other application scenarios, a substrate material such as sapphire or silicon carbide may also be used.
The size of the silicon wafer can be set according to actual processing requirements, and more gold interdigital miniature electrochemical sensors can be processed at one time when the size of the silicon wafer is larger. In some embodiments, a 4 inch silicon wafer may be used as a substrate for making 15mm x 10mm gold interdigitated micro electrochemical sensor slices. Further, the first set thickness of the monocrystalline silicon substrate can be set according to the requirements of specific application scenarios.
Further, a silicon dioxide layer is grown as an insulating layer on the single crystal silicon substrate by thermal oxidation treatment. The silicon dioxide layer grown by thermal oxidation treatment belongs to typical amorphous silicon dioxide, and has high resistivity and high breakdown voltage per unit thickness, so that the silicon dioxide layer can play a good insulating role. In some embodiments, the second set thickness of the silicon dioxide layer may be 200 to 300nm, and preferably, 300nm may be set.
In some embodiments, the ratio of the thickness of the nanotitanium adhesion layer to the thickness of the nanogold sensing layer is 1: 8. In the application, the nano titanium bonding layer and the nano gold sensing layer are obtained by depositing nano titanium and nano gold based on an electron beam evaporation process. In order to enhance the structural stability and ensure that the nanogold used as the electrode material can have a good detection effect, the thickness ratio of the nano titanium bonding layer to the nanogold sensing layer is set to be 1:8 so as to achieve the optimal effect.
The screening principle of the micro-interdigital electrode material is as follows: (1) the selected material and the working medium have good compatibility and do not mutually generate chemical reaction; (2) the substrate material should have good insulation and heat dissipation properties; (3) the electrode material has little interference, preferably no interference, with the detection signal; (4) the surface of the electrode material has strong modifiability; (5) the electrode has simple manufacturing process and low material cost.
In the application, gold is used as an electrode, and the gold has the advantages of stable physical and chemical properties, corrosion resistance, difficult oxidation and less oxidation products. The gold has outstanding electrical properties, so that the conductivity of the microelectrode can be improved. In addition, the gold has the application advantages of no toxicity, high temperature resistance, high biocompatibility, easy biological modification, capability of biological modification and the like. The gold interdigital miniature electrochemical sensor prepared by the scheme not only promotes weaker acid-base solution and organic solvent tolerance of the traditional interdigital electrode, but also overcomes the defect that the structure of the traditional electrode is damaged because the traditional electrode easily receives ultrasonic vibration.
Gold is used as an electrode material, and nano titanium is used as a connecting material, so that the electrode material has a stable integral structure and is applied to heavy metals in actual samples; the detection of ions has the characteristics of excellent response capability, simple detection operation flow, high detection survival anti-interference capability and repeated cyclic utilization.
Further, in the interdigitated electrode pair, the width, the spacing and the thickness between the interdigitated electrodes are 3 main factors affecting the structure of the microelectrode. The electrode structure is simulated through simulation software, parameters such as electric fields, capacitance, impedance and the like generated by different structures are analyzed, and the electrode structure with excellent performance and both accuracy and sensitivity is optimized. Therefore, the size width of the electrode pair can be set based on a specific detection object. In some embodiments, the pairs of interdigitated electrodes are in a circular, zigzag, or parallel array.
In some embodiments, the pairs of interdigitated electrodes are in a parallel array and the length of the interdigitated structure is 2700 μm, the width of the interdigitated structure is 2, 3, 5, 10 or 15 μm, and the duty cycle of the interdigitated structure is 1: 1.
As shown in FIG. 3, the impedance curve of drinking water containing manganese ions of different concentrations is tested by using interdigital electrode pairs with width of 2 μm and intervals, and the lower the concentration of the tested metal ion solution, the lower the impedance value, and the larger the impedance difference with ultrapure water, the lower the detection limit. In order to make the signal of the interdigital electrode pair in detection stronger and the signal-to-noise ratio higher, the self-resistance of the sensor needs to be reduced as much as possible, and therefore, the lower the pitch of the interdigital electrodes, the higher the precision. As shown in FIG. 4, the concentration in the test was 200nmol/L-1Impedance curve process of manganese ion drinking waterIn (3), the smaller the width and the spacing of the interdigital electrode pair, the smaller the impedance, and the lower the detection limit. Therefore, the smaller the width and the interval of the interdigital electrode pair are, the smaller the impedance is, the higher the detection sensitivity is, and the ions having a lower concentration can be detected.
On the other hand, the invention provides a method for manufacturing a gold interdigital micro electrochemical sensor, which refers to an integrated circuit micro-nano processing technology for processing so as to construct a finer interdigital electrode structure, improve the detection capability of the sensor on specific heavy metals in a water environment, and enable the physicochemical properties to be more stable, as shown in fig. 2, the method comprises the following steps:
step S101: and carrying out thermal oxidation treatment on the monocrystalline silicon wafer with the set size so as to grow a silicon dioxide layer with the set thickness on the surface of the silicon wafer.
Step S102: and placing the silicon wafer subjected to thermal oxidation treatment in ethanol, soaking for a first set time, washing with deionized water, transferring the silicon wafer into an acetone solvent, soaking, washing with ultrasonic waves for a second set time, washing with deionized water, and drying with nitrogen.
Step S103: coating photoresist on the surface of the silicon wafer and drying, carrying out photoetching and developing treatment on the silicon wafer by adopting a preset mask, transferring the interdigital array pattern to the silicon dioxide layer, and removing the residual photoresist on the interdigital array part on the surface of the silicon dioxide layer by using an oxygen plasma.
Step S104: and sequentially depositing 10-20 nm of nano titanium and 50-150 nm of nano gold on the silicon wafer after the glue is removed by adopting an electron beam evaporation process.
Step S105: and sequentially carrying out ultrasonic cleaning on the silicon wafer in acetone and ethanol, washing with deionized water, carrying out metal stripping and slicing to obtain the gold interdigital miniature electrochemical sensor.
In step S101, the method of manufacturing a silicon dioxide layer may include: thermal decomposition deposition, sputtering or vacuum evaporation, anodic oxidation method, chemical meteorology deposit, thermal oxidation method etc. this application can adopt thermal oxidation treatment, and silicon takes place chemical reaction with oxidants such as oxygen or steam and generates silicon dioxide under high temperature, and the thermal oxidation method can be divided into according to the oxidizing atmosphere: dry oxygen oxidation, water vapor oxidation, wet oxygen oxidation, chlorine doping oxidation, hydrogen and oxygen synthesis and the like.
The silicon dioxide layer is prepared by thermal oxidation, so that the silicon dioxide layer has high repeatability and chemical stability, and the physical property and the chemical property of the silicon dioxide layer are not influenced by humidity and medium-temperature heat treatment.
Further, the thickness of the grown silicon dioxide layer can be controlled by controlling the thermal oxidation treatment time and the like, and the silicon dioxide layer with the set thickness can ensure effective insulation and prevent voltage breakdown, and in some embodiments, the thickness can be set to be 200-300 nm.
In some embodiments, in step S101, performing thermal oxidation treatment on a single crystal silicon wafer with a set size to grow a silicon dioxide layer with a set thickness on the surface of the silicon wafer, includes: cleaning a monocrystalline silicon wafer by adopting hydrofluoric acid, and carrying out thermal oxidation treatment for 2 hours at the temperature of 900 ℃ so as to grow a silicon dioxide layer with the thickness of 300nm on the surface of the silicon wafer.
In step S102, the silicon wafer is placed in a hydrofluoric acid solution to be polished. The first set period of time for soaking in analytically pure ethanol may be 20 min. And finally, washing with deionized water to remove residual hydrofluoric acid, metal impurities and hydrophilic residues. Further, the silicon wafer was soaked in acetone and cleaned with ultrasonic waves to remove organic impurities. The second set period of immersion in acetone may be 20 min. And then deionized water is adopted for washing to remove residual acetone and other organic matters. Blow-dried with nitrogen for further processing.
In step S103, the photoresist may be a positive photoresist or a negative photoresist, and a corresponding mask is set according to the type of the photoresist. The shape of the mask plate corresponds to the interdigital array. For example, the United states of America may be used
The chip surface was spin coated with a NR-1500 type photoresist (negative resist) from company. Mask plates with different sizes are used for carrying out photoetching and developing treatment on the dried chip, so that the interdigital array pattern is transferred to the silicon dioxide layerAnd removing the residual photoresist by oxygen plasma sputtering. Specifically, oxygen plasma sputtering can remove residual photoresist on the silicon dioxide layer exposed after photolithography, and can also remove a small amount of photoresist at unexposed positions.
In some embodiments, the pattern of the interdigital array corresponding to the predetermined mask is a circular, a zigzag or a parallel array. The specific shape is configured according to actual preparation requirements. In other embodiments, the array of fingers is a parallel array, the fingers have a length of 2700 μm, the finger width is 2, 3, 5, 10, or 15 μm, and the duty cycle of the finger is 1: 1;
in step S104, a vacuum evaporation coating method may be used to fabricate the nano-titanium bonding layer and the nano-gold sensing layer, in this application, an electron beam evaporation process may be used to sequentially deposit 10-20 nm of nano-titanium on the silicon wafer as the nano-titanium bonding layer for connecting the silicon dioxide layer and the nano-gold sensing layer, and deposit 50-150 nm of nano-gold as the electrode. Preferably, the nano titanium can deposit 10-15nm, and the nano gold can deposit 70-80 nm.
In some embodiments, the ratio of the deposition thickness of the nano titanium to the deposition thickness of the nano gold is 1:8, and the total thickness of the interdigital part is 80-100 nm.
In step S105, ultrasonic cleaning is performed in acetone and 2-propanol in sequence, and then deionized water is used for cleaning to remove hydrophilic impurities and hydrophobic impurities. And removing the photoresist and the metal on the surface of the photoresist through a metal stripping process to form the final gold interdigital micro electrochemical sensor.
In some embodiments, after step S105, the method further comprises:
the gold interdigital micro electrochemical sensor obtained by slicing is also subjected to vacuum treatment for 12 hours at the temperature of 200 ℃, and is sealed and stored after being cooled to room temperature by the gradient of 20 ℃ per hour. Gradually cooling is carried out to ensure the structural stability and prevent the interlayer peeling caused by the unbalanced shrinkage. And treated in vacuum to prevent adsorption of microparticles and dust. The cleanliness of the electrode surface is ensured, so that the electrode can be stored for a long time.
A specific example of the preparation and characterization of an identified gold interdigitated electrochemical sensor is given below:
the gold interdigital micro electrochemical sensor comprises the following preparation steps:
1) after a 4-inch silicon wafer is cleaned by 5mL of hydrofluoric acid, the silicon wafer is subjected to thermal oxidation treatment at 900 ℃ for 2 hours to obtain a silicon dioxide insulating layer with the thickness of 300 nm.
2) And (3) soaking the silicon dioxide sheet in a hydrofluoric acid solution for 20min, washing with deionized water, transferring to an acetone solvent for soaking and performing ultrasonic treatment for 20min, washing the chip for three times, and drying by using nitrogen.
3) 5mL of photoresist (negative photoresist) is dripped on the surface of the silicon chip to spin-coat the surface of the chip and then dry the chip. And photoetching and developing the dried chip by using the interdigital mask plate to transfer the interdigital array pattern to the silicon dioxide layer, and removing the residual photoresist by using oxygen plasma.
4) And (3) respectively carrying out nano titanium (10-15nm in thickness) deposition and nano gold deposition (70-80nm) on the chip surface after the glue removal through an electronic book evaporation process.
5) And ultrasonically cleaning the substrate by using acetone and 2-propanol solvent, washing the substrate by using deionized water, stripping the metal from the chip, and slicing the chip to obtain the gold interdigital micro electrochemical sensor.
6) The gold interdigital micro electrochemical sensor is characterized by a series of means such as a scanning electron microscope, a transmission electron microscope, an atomic force microscope and the like, and the result shows that the gold interdigital micro electrochemical sensor is successfully prepared.
Furthermore, the gold interdigital micro electrochemical sensor is used as a metal ion sensor and can be used for detecting copper (II) ions and manganese (II) ions in a water phase sample:
(1) the application of the method in detecting copper (II) ions and manganese (II) ions in environmental water.
(2) The application of the method in detection of copper (II) ions and manganese (II) ions in domestic water.
(3) The application of the method in detecting copper (II) ions and manganese (II) ions in water for agricultural irrigation and animal husbandry.
(4) The application of the copper (II) ion and the manganese (II) ion detection in bottled water, wine, beverage and other liquid beverages.
Specifically, the gold interdigital miniature electrochemical sensor can be provided with electrodes with the thickness of 50-100 nm, the interdigital size of the electrodes can be 2 micrometers in width and interval, 3 micrometers in width and interval or 5 micrometers in width and interval, and the gold interdigital miniature electrochemical sensor is applied to the ultra-sensitive detection of the manganese Mn (II) heavy metal ion pollutants in the environmental water.
Tap water is used as a sample matrix, and a manganese sulfate aqueous solution with the concentration of 0.01 nM-100 nM is prepared, and each concentration system is 1.0 mL. And taking 10 mu L of sample to be detected as working solution by using a micropipettor, accurately dripping the working solution on the surface of the interdigital microsensor, standing for 1.0min, and then carrying out impedance test on the manganese ion solution to be detected by using an electrochemical workstation. And (3) drawing a frequency-impedance curve by using a Nyquist-Bode diagram in an electrochemical impedance method to the sampling frequency of the measured solution and the corresponding impedance value, wherein the sampling frequency is 10 KHz. The recovery rate of the manganese ion solution in the test is shown in table 1, and the recovery rate of the manganese ion solution to be tested with three different concentrations of 0.01nM, 1.0nM and 100nM is 90.9% -99.8%, the total average recovery rate is 96.5% and the standard deviation (RSD) is 4.9%. The established content determination method has high accuracy and meets the requirement of the recovery rate at the concentration of 0.01 nM-100 nM.
TABLE 1 results of the manganese ion solution recovery test
Furthermore, the gold interdigital miniature electrochemical sensor can be provided with electrodes with the thickness of 100-150 nm, the interdigital size of the electrodes can be 10 micrometers in width and interval or 15 micrometers in width and interval, and the gold interdigital miniature electrochemical sensor is applied to the ultra-sensitive detection of copper Cu (II) heavy metal ion pollutants in environmental water.
Tap water is used as a sample matrix, and copper acetate aqueous solution with the concentration of 0.001 nM-10 nM (1.0 pM-10000 pM) is prepared, and each concentration system is 1.0 mL. And taking 10 mu L of sample to be tested as working solution by using a micropipettor, accurately dripping the working solution on the surface of the interdigital microsensor, standing for 1.0min, and then carrying out impedance test on the copper ion solution to be tested by using an electrochemical workstation. And (3) drawing a frequency-impedance curve by using a Nyquist-Bode diagram in an electrochemical impedance method to the sampling frequency of the measured solution and the corresponding impedance value, wherein the sampling frequency is 10 KHz. The test recovery rates of the copper ion solutions are shown in Table 1, and the recovery rates of the copper ion solutions to be tested with different concentrations of 0.001nM, 0.1nM and 10nM are 93.86% -99.77%, the total average recovery rate is 97.25% and the standard deviation (RSD) is 2.32%. The established content determination method has high accuracy and meets the requirement that the recovery rate is between 0.001nM and 10.0 nM.
TABLE 2 copper ion solution impedance test recovery test results
In other embodiments, the gold interdigital micro electrochemical sensor can also be used for detecting other heavy metal ions, such as lead ions, arsenic ions, mercury ions and the like, in a water phase sample, such as environmental water, industrial water, domestic water and the like.
Furthermore, the gold interdigital micro electrochemical sensor developed by the invention has recycling capability, and can be reused for at least 100 times after regeneration treatment of a small amount of methanol and deionized water. Powerful guarantee is provided for developing novel high-efficient, green and low-cost environmental water detection quantitative technology.
The gold interdigital micro electrochemical sensor prepared by the invention has high detectability and signal response aiming at heavy metal ions in various environmental water, has the advantages of simple and convenient operation, quick regeneration and the like, can greatly simplify the operation process of quantitative detection of samples, shorten the detection and regeneration time, reduce the usage amount of various chemical reagents in the detection process, improve the detection quantitative efficiency and realize the ultra-sensitive detection of trace or ultra-trace harmful heavy metal ions in water sample matrixes when being used in the field of detection of heavy metal ions in drinking water and food safety.
The gold interdigital micro electrochemical sensor prepared by the invention has the advantages of sensitive response to target heavy metal ions, cyclic utilization, rapid regeneration, strong acid, strong alkaline solution and various organic solvents resistance, and has a stable physical structure capable of resisting 600w power and continuous 3-hour treatment of a 40KHz ultrasonic cleaner. The method is used for detecting heavy metal ions in water, can simplify the operation process, improve the detection quantitative sensitivity, save the use of reagents and improve the detection limit of a target object.
In summary, in the gold interdigital micro electrochemical sensor and the manufacturing method thereof, the gold interdigital micro electrochemical sensor constructs the interdigital electrode pair of the silicon dioxide layer, the nanometer titanium layer and the nanometer gold based on the integrated circuit micro-nano processing manufacturing process, the thickness of each layer is finely controlled, and the detection of the heavy metal of the specified target and the specified concentration is realized. The gold interdigital miniature electrochemical sensor manufactured by the manufacturing method has high processing precision and stable manufacturing process, and can realize large-scale batch preparation; meanwhile, gold is adopted as an electrode material, so that the electrode material is more stable in physical and chemical properties, sensitive in response, recyclable, rapid in regeneration and resistant to strong acid, strong alkali and various organic solutions. And is resistant to ultrasonic waves, having a robust physical structure.
It should also be noted that the exemplary embodiments mentioned in this patent describe some methods or systems based on a series of steps or devices. However, the present invention is not limited to the order of the above-described steps, that is, the steps may be performed in the order mentioned in the embodiments, may be performed in an order different from the order in the embodiments, or may be performed simultaneously.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments in the present invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes may be made to the embodiment of the present invention by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A gold interdigitated micro-electrochemical sensor, comprising:
the single crystal silicon substrate is of a first set thickness;
a silicon dioxide layer with a second set thickness is arranged on the monocrystalline silicon substrate;
the surface of the silicon dioxide layer is provided with interdigital electrode pairs, and the interdigital electrode pairs comprise a 10-20 nm nano titanium bonding layer and a 50-150 nm nano gold sensing layer from inside to outside.
2. The gold interdigitated micro electrochemical sensor of claim 1 wherein the pair of interdigitated electrodes is in a circular, zig-zag or parallel array.
3. The gold interdigitated micro-electrochemical sensor of claim 2, wherein the thickness ratio of the nano-titanium adhesion layer to the nano-gold sensing layer is 1: 8.
4. The gold interdigitated micro electrochemical sensor of claim 3 wherein the pair of interdigitated electrodes are in a parallel array and the length of the interdigitated structure is 2700 μm, the width of the interdigitated structure is 2, 3, 5, 10 or 15 μm, and the duty cycle of the interdigitated structure is 1: 1.
5. The gold interdigitated micro-electrochemical sensor according to claim 1, wherein the second set thickness is 200 to 300 nm.
6. A method for manufacturing a gold interdigital micro electrochemical sensor is characterized by comprising the following steps:
carrying out thermal oxidation treatment on a monocrystalline silicon wafer with a set size to grow a silicon dioxide layer with a set thickness on the surface of the silicon wafer;
placing the silicon wafer subjected to thermal oxidation treatment in ethanol, soaking for a first set time, washing with deionized water, transferring the silicon wafer into an acetone solvent, soaking, washing with ultrasonic waves for a second set time, washing with deionized water, and drying with nitrogen;
coating photoresist on the surface of the silicon wafer and drying, carrying out photoetching and developing treatment on the silicon wafer by adopting a preset mask, transferring the interdigital array pattern to the silicon dioxide layer, and removing the residual photoresist on the interdigital array part on the surface of the silicon dioxide layer by using an oxygen plasma;
depositing 10-20 nm of nano titanium and 50-150 nm of nano gold on the silicon wafer after removing the glue in sequence by adopting an electron beam evaporation process;
and sequentially carrying out ultrasonic cleaning on the silicon wafer in acetone and ethanol, washing with deionized water, carrying out metal stripping and slicing to obtain the gold interdigital miniature electrochemical sensor.
7. The method of manufacturing a gold interdigitated micro-electrochemical sensor according to claim 6, further comprising:
and (3) carrying out vacuum treatment on the gold interdigital micro electrochemical sensor obtained by slicing at 200 ℃ for 12 hours, and sealing and storing after the temperature is reduced to room temperature by a gradient of 20 ℃ per hour.
8. The method for manufacturing a gold interdigital micro electrochemical sensor according to claim 6, wherein the thermal oxidation treatment is performed on a monocrystalline silicon wafer with set size to grow a silicon dioxide layer with set thickness on the surface of the silicon wafer, comprising:
cleaning a monocrystalline silicon wafer by adopting hydrofluoric acid, and carrying out thermal oxidation treatment for 2 hours at the temperature of 900 ℃ so as to grow a silicon dioxide layer with the thickness of 300nm on the surface of the silicon wafer.
9. The manufacturing method of the gold interdigital micro electrochemical sensor according to claim 6, wherein the interdigital array pattern corresponding to the preset mask is a ring-shaped, a zigzag-shaped or a parallel array.
10. The method of manufacturing a gold interdigitated micro electrochemical sensor according to claim 9, wherein said interdigitated array is a parallel array, the length of the interdigitated fingers is 2700 μm, the width of the interdigitated structure is 2, 3, 5, 10 or 15 μm, and the duty cycle of the interdigitated structure is 1: 1; the deposition thickness ratio of the nano titanium to the nano gold is 1: 8.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012081965A1 (en) * | 2010-12-15 | 2012-06-21 | Mimos Berhad | Interdigitated capacitor and dielectric membrane sensing device |
| CN109809359A (en) * | 2019-01-10 | 2019-05-28 | 北方工业大学 | 2.5D interdigital electrode manufacturing method and interdigital electrode |
-
2021
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012081965A1 (en) * | 2010-12-15 | 2012-06-21 | Mimos Berhad | Interdigitated capacitor and dielectric membrane sensing device |
| CN109809359A (en) * | 2019-01-10 | 2019-05-28 | 北方工业大学 | 2.5D interdigital electrode manufacturing method and interdigital electrode |
Non-Patent Citations (2)
| Title |
|---|
| HAOCHEN QI ET.AL: "Rapid detection of trace Cu<sup>2+</sup> using an L-cysteine based interdigitated electrode sensor integrated with AC electrokinetic enrichment", 《ELECTROPHORESIS》 * |
| 孟庆一 等: "微电极法测定饮用水中锰离子含量", 《食品安全质量检测学报》 * |
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