CN112285182A - High-precision interdigital electrode and preparation method and application thereof - Google Patents
High-precision interdigital electrode and preparation method and application thereof Download PDFInfo
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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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3271—Amperometric enzyme electrodes for analytes in body fluids, e.g. glucose in blood
- G01N27/3272—Test elements therefor, i.e. disposable laminated substrates with electrodes, reagent and channels
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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
- G01N27/327—Biochemical electrodes, e.g. electrical or mechanical details for in vitro measurements
- G01N27/3275—Sensing specific biomolecules, e.g. nucleic acid strands, based on an electrode surface reaction
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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
- G01N27/36—Glass electrodes
Abstract
The invention provides a high-precision interdigital electrode, and a preparation method and application thereof. The invention adopts a semiconductor film process, processes a metal film on an insulating substrate by adopting a magnetron sputtering mode, photoetches an interdigital electrode circuit pattern, forms a graphic circuit by developing and exposing, and etches a bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode. The line width and line distance of the high-precision interdigital electrode is 1-40 mu m, and the high-precision interdigital electrode is provided with a conductive inner layer and a reaction layer, can be used for biomolecule detection, and can be particularly used for preparing an electrochemical immunosensor.
Description
Technical Field
The invention belongs to the field of electrochemical sensors, and relates to a high-precision interdigital electrode, and a preparation method and application thereof.
Background
The interdigital electrode is an electrode with a periodic pattern in a finger-shaped or comb-shaped surface, and is a hyperfine circuit obtained by electrochemical processing. As an electrical signal transmission core component, the material is widely applied to important fields of biomedical detection, environment on-line monitoring, food safety detection, safety monitoring and the like.
In recent years, with the rapid development of industry 4.0 and the internet of things, the requirements of emerging industry and other industries on sensors are more and more, and the interdigital electrode as one of the core components of the sensor is more and more concerned by society, so how to improve the reliability of the interdigital electrode is directly related to the technical level of various sensors, which also becomes an industry common problem in the electronic information industry.
Aluminum nitride or aluminum oxide is generally adopted at home and abroad as a base body to design and develop the interdigital electrode, selection and design are carried out according to different applications of the interdigital electrode, and the interdigital electrode is applied to the fields of gas detection, microorganism detection and the like at present, but different enterprises adopt different processing technologies in the aspects of reliability and precision of the interdigital electrode, so that the performance indexes are greatly different, the product processing reject ratio is high, and the interdigital electrode is also a main problem faced by the current interdigital electrode industry.
Disclosure of Invention
In view of the above, the invention provides a high-precision interdigital electrode, and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
a high-precision interdigital electrode comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer.
The insulating substrate of the high-precision interdigital electrode provided by the invention is any one of non-metallic materials such as silicon substrate, ceramics, glass and the like.
Preferably, the insulating substrate is silicon-based, and the surface of the insulating substrate is modified with a silicon dioxide protective layer.
The thickness of the conductive inner layer of the high-precision interdigital electrode is 20-50 nm, and the conductive inner layer is made of metal formed by one of Cr, Ti and Ni or alloy formed by at least two of Cr, Ti and Ni.
The thickness of the reaction layer of the high-precision interdigital electrode provided by the invention is 100nm, and the reaction layer is one of Au, Ag and Pt.
The line width and line distance of the high-precision interdigital electrode provided by the invention is 1-40 μm.
The invention also provides a preparation method of the high-precision interdigital electrode, which comprises the following steps:
magnetron sputtering the conductive inner layer and the reaction layer on the insulating substrate in sequence, and mechanically spin-coating photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
The method for magnetron sputtering the conductive inner layer specifically comprises the following steps: the sputtering target is metal, the diameter of the target is 15-25 mm, and the thickness of the target is 2-5 mm; the distance between the target and the insulating substrate is 10-15 cm; the magnetron sputtering power is 180-200W, the sputtering air pressure is 1-3 Pa, and the sputtering time is 5-15 min;
the method for magnetron sputtering the reaction layer specifically comprises the following steps: the sputtering target is metal, the diameter of the target is 20-30 mm, and the thickness of the target is 2-5 mm; the distance between the target and the insulating substrate is 10-15 cm; the magnetron sputtering power is 200-250W, the sputtering pressure is 3-5 Pa, and the sputtering time is 15-25 min.
Electroplating processing cannot be directly carried out on the insulating base body, magnetron sputtering is needed, and in addition, the problem of thermal stress mismatch between the insulating base body and the conductive metal layer can be relieved.
By magnetron sputtering, a transition metal layer can be formed on any insulating base layer (including but not limited to ceramics, glass and high molecular polymer), and further metal is attached and an electrode layer is etched. The invention optimizes the parameters of magnetron sputtering, improves the stability of the electrode layer and the insulating base layer, and avoids the problem that the two sides of the electrode layer are easy to separate from the insulating base body due to uneven stress caused by the existence of the porous metal layer.
As shown in the attached figure 1, the high-precision interdigital electrode prepared by the invention is provided. The electrode insulation substrate adopts a silicon substrate, metal titanium as a conductive inner layer and a pure gold layer as a reaction layer are sequentially modified on the silicon substrate, the number of pairs of interdigital electrodes of the electrode is 25, the line width and the line distance of the electrode are 5 mu m, the size of the whole electrode is 6.0mm x 4.0mm, the thickness of the silicon substrate is 500 mu m, the thickness of the conductive inner layer is 20nm, and the thickness of the reaction layer is 100 nm.
As shown in fig. 2, the high-precision interdigital electrode prepared by the invention is provided. The electrode insulation substrate adopts a silicon substrate, metal titanium as a conductive inner layer and a pure gold layer as a reaction layer are sequentially modified on the silicon substrate, the number of pairs of interdigital electrodes of the electrode is 25, the line width and the line distance of the electrode are 10 mu m, the size of the whole electrode is 6.0mm x 4.0mm, the thickness of the silicon substrate is 500 mu m, the thickness of the conductive inner layer is 20nm, and the thickness of the reaction layer is 100 nm.
As shown in fig. 3, the high-precision interdigital electrode prepared by the invention is provided. The electrode insulation substrate adopts a silicon substrate, metal titanium as a conductive inner layer and a pure gold layer as a reaction layer are sequentially modified on the silicon substrate, the number of pairs of interdigital electrodes of the electrode is 25, the line width and the line distance of the electrode are 15 mu m, the size of the whole electrode is 6.0mm x 4.0mm, the thickness of the silicon substrate is 500 mu m, the thickness of the conductive inner layer is 30nm, and the thickness of the reaction layer is 100 nm.
As shown in fig. 4, the high-precision interdigital electrode prepared by the invention is provided. The electrode insulation substrate adopts a silicon substrate, metal titanium as a conductive inner layer and a pure gold layer as a reaction layer are sequentially modified on the silicon substrate, the number of pairs of interdigital electrodes of the electrode is 25, the line width and the line distance of the electrode are 20 mu m, the size of the whole electrode is 6.0mm x 4.0mm, the thickness of the silicon substrate is 500 mu m, the thickness of the conductive inner layer is 40nm, and the thickness of the reaction layer is 100 nm.
As shown in fig. 5, the high-precision interdigital electrode prepared by the invention is provided. The electrode insulation substrate adopts a silicon substrate, metal titanium as a conductive inner layer and a pure gold layer as a reaction layer are sequentially modified on the silicon substrate, the number of pairs of interdigital electrodes of the electrode is 25, the line width and the line distance of the electrode are 30 micrometers, the size of the whole electrode is 6.0mm x 4.0mm, the thickness of the silicon substrate is 500 micrometers, the thickness of the conductive inner layer is 50nm, and the thickness of the reaction layer is 100 nm.
As shown in fig. 6, is a schematic cross-sectional view of a high-precision interdigital electrode prepared by the present invention. As can be seen from the figure, the high-precision interdigital electrode is provided with a conductive inner layer which is made of metal Ti and is formed by magnetron sputtering on an insulating base material, and the thickness of the conductive inner layer is 20-50 nm; the metal reaction layer plated outside the conductive inner layer is metal Au, and the thickness of the metal reaction layer is 100 nm.
The invention also provides application of the high-precision interdigital electrode.
The high-precision interdigital electrode provided by the invention can be used for biomolecule detection, and particularly can be used for preparing an electrochemical immunosensor.
As shown in fig. 7, the stability test chart (a) and the anti-interference test chart (b) for detecting uric acid by the high-precision interdigital electrode prepared by the invention are shown. As can be seen from the figure, the high-precision interdigital electrode has excellent stability and good anti-interference property, and can detect trace uric acid under the condition that substances such as glucose, citric acid, glycine, urea and the like exist at the same time.
As shown in fig. 8, the stability test chart (a) and the anti-interference test chart (b) for detecting dopamine by the high-precision interdigital electrode prepared by the invention are shown. As can be seen from the figure, the high-precision interdigital electrode has excellent stability and good anti-interference property, and can detect trace dopamine under the condition that substances such as glucose, citric acid, glycine, urea and the like exist at the same time.
The invention adopts a semiconductor film process, processes a metal film on an insulating substrate by adopting a magnetron sputtering mode, photoetches an interdigital electrode circuit pattern, forms a graphic circuit by developing and exposing, and etches a bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode. The line width and line distance of the high-precision interdigital electrode is 1-40 mu m, and the high-precision interdigital electrode is provided with a conductive inner layer and a reaction layer, can be used for biomolecule detection, and can be particularly used for preparing an electrochemical immunosensor.
The invention has the beneficial effects that: according to the invention, a semiconductor film process is adopted, a metal film is directly modified on an insulating substrate to obtain the high-precision interdigital electrode, the line width and the line distance of the electrode are as fine as 1 mu m, so that the electrode has high process precision; the electrode reaction gold layer is fine to 100nm, has excellent biocompatibility, is suitable for modifying antigen and antibody, can be applied to the fields of biological medicine and electrochemical immunosensors, and can be used for electrochemical precise molecular detection.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is a high-precision interdigital electrode prepared by example 2 of the present invention;
FIG. 2 is a high-precision interdigital electrode prepared by example 3 of the present invention;
fig. 3 shows a high-precision interdigital electrode prepared in example 4 of the present invention:
FIG. 4 is a high-precision interdigital electrode prepared by example 5 of the present invention;
FIG. 5 shows a high-precision interdigital electrode prepared in example 6 of the present invention;
FIG. 6 is a schematic cross-sectional level diagram of a high-precision interdigital electrode prepared by the present invention;
FIG. 7 is (a) a stability test chart and (b) an anti-interference test chart of the high-precision interdigital electrode prepared by the invention for detecting uric acid;
fig. 8 is (a) a stability test chart and (b) an anti-interference test chart of the high-precision interdigital electrode prepared by the invention for detecting dopamine.
Detailed Description
In order that the objects, aspects and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the following detailed description and the accompanying drawings.
Example 1
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 20 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 1 μm, and the interdigital number of the electrode is 25 pairs.
The preparation method comprises the following steps:
carrying out magnetron sputtering on a conductive inner Ti layer on an insulating substrate silicon substrate, wherein a sputtering target material is metal Ti, the diameter of the target material is 25mm, and the thickness of the target material is 2 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 180W, the sputtering air pressure is 1.5Pa, and the sputtering time is 5 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 30mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 250W, the sputtering air pressure is 5Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 2
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 1 and 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 20 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 5 μm, and the interdigital number of the electrode is 25 pairs.
The preparation method comprises the following steps:
performing magnetron sputtering on an insulating substrate silicon substrate to form a conductive inner Ti layer, wherein a sputtering target material is metal Ti, the diameter of the target material is 15mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 1Pa, and the sputtering time is 5 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 20mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 10 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 20 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 3
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 2 and 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Further, the conductive inner layer is Ti with the thickness of 30 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 10 μm, and the interdigital number of the electrode is 25 pairs.
The preparation method comprises the following steps:
performing magnetron sputtering on an insulating substrate silicon substrate to form a conductive inner Ti layer, wherein a sputtering target material is metal Ti, the diameter of the target material is 20mm, and the thickness of the target material is 3 mm; the distance between the target and the insulating substrate is 12 cm; the magnetron sputtering power is 190W, the sputtering air pressure is 2Pa, and the sputtering time is 5 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 25mm, and the thickness of the target material is 3 mm; the distance between the target and the insulating substrate is 12 cm; the magnetron sputtering power is 22W, the sputtering air pressure is 4Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 4
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 3 and 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 40 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 15 μm, and the electrode interdigital number is 25 pairs.
The preparation method comprises the following steps:
performing magnetron sputtering on an insulating substrate silicon substrate to form a conductive inner Ti layer, wherein a sputtering target material is metal Ti, the diameter of the target material is 20mm, and the thickness of the target material is 5 mm; the distance between the target and the insulating substrate is 12 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 5 min.
Then carrying out magnetron sputtering on the Au layer of the reaction layer, wherein the sputtering target material is metal Au, the diameter of the target material is 25mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 5
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 4 and 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 50 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 20 μm, and the electrode interdigital number is 25 pairs.
The preparation method comprises the following steps:
performing magnetron sputtering on an insulating substrate silicon substrate to form a conductive inner Ti layer, wherein a sputtering target material is metal Ti, the diameter of the target material is 15mm, and the thickness of the target material is 4 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 15 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 20mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 10 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 20 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 6
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 5 and 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 500 μm, and the overall electrode size is 6.0mm x 4.0 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 50 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 30 μm, and the number of pairs of interdigital electrodes is 25.
The preparation method comprises the following steps:
carrying out magnetron sputtering on a conductive inner Ti layer on an insulating substrate silicon substrate, wherein a sputtering target material is metal Ti, the diameter of the target material is 25mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 1.5Pa, and the sputtering time is 5-15 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 30mm, and the thickness of the target material is 2 mm; the distance between the target and the insulating substrate is 12 cm; the magnetron sputtering power is 250W, the sputtering air pressure is 3Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 7
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 6.
In this embodiment, the insulating substrate is silicon-based.
Further, the thickness of the silicon-based substrate is 0.6mm, and the size of the whole electrode is 13.0mm x 7.0 mm.
Furthermore, the conductive inner layer is Ni, and the thickness is 50 nm; the reaction layer is Ag and has a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 20 μm, and the number of pairs of interdigital electrodes is 10.
The preparation method comprises the following steps:
carrying out magnetron sputtering on a conductive inner Ni layer on an insulating substrate silicon substrate, wherein a sputtering target material is metal Ni, the diameter of the target material is 15mm, and the thickness of the target material is 2 mm; the distance between the target material and the insulating substrate is 10 cm; the magnetron sputtering power is 180W, the sputtering air pressure is 1Pa, and the sputtering time is 15 min.
Then carrying out magnetron sputtering on the reaction layer Ag layer, wherein the sputtering target material is metal Ag, the diameter of the target material is 20mm, and the thickness of the target material is 3 mm; the distance between the target and the insulating substrate is 12 cm; the magnetron sputtering power is 220W, the sputtering air pressure is 3Pa, and the sputtering time is 20 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 8
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 6.
In this embodiment, the insulating substrate is made of ceramic.
Further, the ceramic substrate thickness is 0.38mm, and the overall electrode size is 10mm x 10 mm.
Furthermore, the conductive inner layer is Ti with the thickness of 50 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 20 μm, and the number of pairs of interdigital electrodes is 30.
The preparation method comprises the following steps:
carrying out magnetron sputtering on a conductive inner Ti layer on an insulating substrate ceramic base, wherein a sputtering target material is metal Ti, the diameter of the target material is 25mm, and the thickness of the target material is 2 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 2Pa, and the sputtering time is 10 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 25mm, and the thickness of the target material is 2 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 9
The embodiment provides a high-precision interdigital electrode, which specifically comprises an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer, as shown in fig. 6.
In this embodiment, the insulating substrate is made of quartz glass.
Further, the thickness of the quartz glass substrate was 0.70mm and the overall electrode size was 5mm x 8 mm.
Furthermore, the conductive inner layer is Cr and has the thickness of 30 nm; the reaction layer was Au and had a thickness of 100 nm.
Furthermore, the line width and the line distance of the interdigital electrode are 10 μm, and the number of pairs of interdigital electrodes is 30.
The preparation method comprises the following steps:
performing magnetron sputtering on a conductive inner Cr layer on quartz glass of an insulating substrate, wherein a sputtering target material is metal Cr, the diameter of the target material is 20mm, and the thickness of the target material is 5 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 180W, the sputtering air pressure is 1Pa, and the sputtering time is 10 min.
Then, a reaction layer Au layer is sputtered by magnetron sputtering, the sputtering target material is metal Au, the diameter of the target material is 25mm, and the thickness of the target material is 2 mm; the distance between the target material and the insulating substrate is 15 cm; the magnetron sputtering power is 200W, the sputtering air pressure is 3Pa, and the sputtering time is 15 min.
Mechanically spin-coating a photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; and removing the adhesive film to obtain the high-precision interdigital electrode.
Example 10
Enzyme substances are modified on the surfaces of the high-precision interdigital electrodes prepared in the embodiments 1-6 to prepare the electrochemical immunosensor. The sensor was used for uric acid assay under the same conditions, and the results are shown in table 1 below.
The stability of the electrode for detecting uric acid is shown in fig. 7(a), under the condition that interfering substances such as glucose, citric acid, glycine, urea and the like exist at the same time, a trace amount of uric acid (10 μ M) is continuously added, and the detection result is not interfered, as shown in fig. 7(b), so that the high-precision interdigital electrode prepared by the invention can detect uric acid and has the characteristics of high sensitivity, high stability and excellent anti-interference.
Example 11
Enzyme substances are modified on the surfaces of the high-precision interdigital electrodes prepared in the embodiments 1-6 to prepare the electrochemical immunosensor. The sensor was used for dopamine measurement under the same conditions, and the results are shown in table 1 below.
The stability of the electrode for detecting dopamine is shown in fig. 8(a), under the condition that interfering substances such as glucose, citric acid, glycine, urea and the like exist at the same time, a trace amount of dopamine (10 μ M) is continuously added, and the detection result is not interfered, as shown in fig. 8(b), so that the high-precision interdigital electrode prepared by the invention can detect dopamine and has high sensitivity, high stability and excellent anti-interference characteristics.
According to the embodiments 10 to 12, the high-precision interdigital electrode prepared by the invention can be used for detecting small biological molecules such as uric acid, dopamine and the like, the electrode detection limit for detecting uric acid molecules is less than or equal to 15ppm, and the electrode detection limit for detecting dopamine molecules is less than or equal to 20 ppm.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single technical solution, and such description is for clarity only, and those skilled in the art should take the description as a whole, and the technical solutions in the embodiments may be combined appropriately to form other embodiments that those skilled in the art can understand. The technical details not described in detail in the present invention can be implemented by any of the prior arts in the field. In particular, all technical features of the invention which are not described in detail can be achieved by any prior art.
Claims (10)
1. The high-precision interdigital electrode is characterized by comprising an insulating base body, a conductive inner layer and a reaction layer, wherein the conductive inner layer is arranged on the surface of the insulating base body, and the reaction layer is arranged on the outer surface of the conductive inner layer.
2. The high-precision interdigital electrode according to claim 1, wherein the insulating substrate is any one of non-metallic materials such as silicon-based, ceramic, glass, etc.
3. The high-precision interdigital electrode according to claim 2, wherein the insulating substrate is preferably silicon-based, and the surface thereof is modified with a silicon dioxide protective layer.
4. The high-precision interdigital electrode according to claim 1, wherein the thickness of the conductive inner layer is 20-50 nm.
5. The high-precision interdigital electrode according to claim 4, wherein the conductive inner layer is made of a metal formed of one of Cr, Ti, Ni or an alloy formed of at least two of them.
6. The high-precision interdigital electrode according to claim 1, wherein the thickness of the reaction layer is 100 nm.
7. The high-precision interdigital electrode according to claim 6, wherein the reaction layer is one of Au, Ag and Pt.
8. The high-precision interdigital electrode according to claim 1, wherein the line width and the line distance of the interdigital electrode are 1-40 μm.
9. A method for preparing the high-precision interdigital electrode of claim 1, which comprises the following steps: magnetron sputtering the conductive inner layer and the reaction layer on the insulating substrate in sequence, and mechanically spin-coating photoresist; developing and exposing to form a pattern circuit, and etching the bottom layer to form an electrode circuit; removing the adhesive film to obtain the high-precision interdigital electrode;
the method for magnetron sputtering the conductive inner layer specifically comprises the following steps: the sputtering target is metal, the diameter of the target is 15-25 mm, and the thickness of the target is 2-5 mm; the distance between the target and the insulating substrate is 10-15 cm; the magnetron sputtering power is 180-200W, the sputtering air pressure is 1-3 Pa, and the sputtering time is 5-15 min;
the method for magnetron sputtering the reaction layer specifically comprises the following steps: the sputtering target is metal, the diameter of the target is 20-30 mm, and the thickness of the target is 2-5 mm; the distance between the target and the insulating substrate is 10-15 cm; the magnetron sputtering power is 200-250W, the sputtering pressure is 3-5 Pa, and the sputtering time is 15-25 min.
10. Use of a high-precision interdigital electrode according to claim 1, characterized in that it is used for biomolecule detection, in particular for the preparation of electrochemical immunosensors.
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