CN108802140A - A kind of interdigital electrode and its preparation method and application of porous gold modification - Google Patents
A kind of interdigital electrode and its preparation method and application of porous gold modification Download PDFInfo
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- CN108802140A CN108802140A CN201810917996.0A CN201810917996A CN108802140A CN 108802140 A CN108802140 A CN 108802140A CN 201810917996 A CN201810917996 A CN 201810917996A CN 108802140 A CN108802140 A CN 108802140A
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Abstract
A kind of interdigital electrode and its preparation method and application of porous gold modification.For the interdigital electrode of the porous gold modification in one layer of porous layer gold of common interdigital electrode face finish, the interdigital electrode is alumina ceramic-base or polymer-based or silicon substrate or Metal Substrate interdigital electrode.Preparation method is the deposited Au tin alloy layers after interdigital electrode surface treatment；With the tin in chemical corrosion method or electrochemical erosion method removal alloy, pure water cleaning is drying to obtain the interdigital electrode of porous gold modification.The interdigital electrode of the present invention has high sensitivity and stability to the biological detection of low concentration, pollutant monitoring, can be used for biological detection, electrochemical analysis or sensitive gas detection, is with a wide range of applications.
Description
Technical field
The present invention relates to chemistry or the detection fields of biological substance, and in particular to a kind of preparation and application of interdigital electrode,
Especially a kind of interdigital electrode and its preparation method and application of porous gold modification, belongs to compound test technical field.
Background technology
Biosensor technology is a very active engineering and technological research field, it with bioinformatics, biological core
The subjects such as piece, bio-cybernetics, bionics, biocomputer are in the intersection region of life science and information science together, are
Develop a kind of essential advanced detection of biotechnology and monitoring device.Electrochemical sensor is a kind of very important life
Object sensor, electrochemical sensor by reacting with measured target analyte, and generate with target analyte concentration at than
The electric signal of example carrys out work.Typical electrochemical sensor is made of sensing electrode and counterelectrode, and there are one thin electrolyte layers every
It opens.It in environmental monitoring, can be grown between the electrode of electrochemical sensor, can react and occur with target analytes
The catches of change in resistance realizes most of poisonous and harmful biology in detection environment by detecting the resistance change of catches
The purpose of chemical substance.Electrochemical sensor usually has the characteristics that easy to operate, instrument cost is low.In addition to this, electrochemistry
Sensor can be combined with various advanced MEMS manufacturing technologies, to realize large-scale batch production, and can
To realize miniaturization to reduce cost.During acquiring biological electric signals are with utilizing, biomedical electrode is as a kind of energy
Enough sensors that the ionic potential that organism electrochemical activity generates effectively is converted into measuring system electronic potential, are answered extensively
For modern clinic detection and biomedical measurement.
Biological detection electrode can play swashing for bioelectrical signals as one of the most key core component of measuring system
The effects that encouraging, acquire, conducting, but since bioelectrical signals are weaker, usually require to come using multiple electrodes in most cases
It is carried out at the same time the acquisition and analysis of bioelectrical signals, the flexible electrode of currently used electrode, microneedle electrodes, interdigital electrode etc.,
Wherein interdigital electrode is a kind of common electrochemical detection electrode, and interdigital electrode is a kind of micro- spaced electrodes structure, it is extensive
Applied to multiple fields such as nondestructive testing, telecommunications, test chemicals.In general, different application fields is for fork
Refer to shape, geometry size, processing technology, the selection of material, modeling analysis, the system integration and the analysis of data of electrode all
There is a different requirements, therefore we should distinguish and treat for different fields.
But it is often used Signa Gel often due to detecting, and the electrical impedance unstability of Signa Gel, in high accuracy experiment
In be readily incorporated larger noise and error, so as to cause the inaccurate of measurement result, largely reduce interdigital electricity
The electric conductivity of pole.In addition, before using Ag/AgCl electrodes, it is necessary to be effectively treated to skin, wipe skin as far as possible
The cuticula on skin surface needs certain time, and otherwise Signa Gel may cause cutaneous anaphylaxis, generates red and swollen
Phenomena such as, so that certain measurement process are difficult to carry out.
Invention content
The object of the present invention is to provide a kind of interdigital electrodes and its preparation method and application of porous gold modification.
An object of the present invention is to provide a kind of interdigital electrode of porous gold modification, and this interdigital electrode is in regular fork
Refer to made of one layer of porous layer gold of electrode face finish.
Further, the interdigital electrode is alumina ceramic-base or polymer-based or silicon substrate or the interdigital electricity of Metal Substrate
Pole.
Further, the thickness of the porous gold is 1-5 μm.
Further, secondary modification noble metal, metal oxide or protease activity can also be carried out after porous gold modification
Property substance.
The second object of the present invention is to provide a kind of preparation method of the interdigital electrode of above-mentioned porous gold modification, step is prepared
It is rapid as follows：
1) common interdigital electrode is surface-treated, obtains surface-treated interdigital electrode；
2) in interdigital electrode surface deposited Au tin alloy layers；
3) tin in chemical corrosion method or electrochemical erosion method removal alloy, pure water cleaning is used to be drying to obtain porous gold and repair
The interdigital electrode of decorations.
Further, the surface treatment of the step 1) can be chemical treatment or electrochemical treatments, be chemically treated and be
Interdigital electrode is impregnated 10-30 minutes in citric acid solution；Electrochemical treatments are that interdigital electrode is placed in electrochemistry in lye
Processing, specially：It is cathode by anode, platinized platinum of interdigital electrode, interdigital electrode is immersed in lye, energization processing；
Preferably, the citric acid concentration is 1-3%wt, and electrical current is 0.5-0.7A in the electrochemical treatments.
Further, the gold-tin alloy solution composition in the step 2) used in middle electrochemical deposition be soluble gold salt,
Soluble pink salt, ascorbic acid, potassium sulfate and dipotassium hydrogen phosphate；
It is preferred that the soluble gold salt is at least one of citric acid gold, aurous chloride potassium, sulfurous acid gold potassium, it is solvable
Property pink salt be sulfurous acid tin, tin methane sulfonate, nitric acid tin at least one；
It is preferred that the group of the gold-tin alloy solution becomes：It is citric acid gold 10-50g/L, stannous sulfate 10-50g/L, anti-bad
Hematic acid 10-40g/L, potassium sulfate 10-40g/L, dipotassium hydrogen phosphate 10-40g/L；
The group of preferred gold-tin alloy solution becomes：Citric acid gold 20-40g/L, stannous sulfate 20-40g/L, Vitamin C
Sour 20-30g/L, potassium sulfate 20-30g/L, dipotassium hydrogen phosphate 20-30g/L.
Further, in the step 2) electrochemical deposition temperature be 40-60 DEG C, current density 1.0-2.0ASF, when
Between be 5-20min, pH value 4-7；
It is furthermore preferred that the electrodeposition temperature is 45-55 DEG C, current density 1.0-1.5ASF, time 5-
10min, pH value 5-6.
Further, in the step 3), tin is removed using chemical corrosion method, it is specific using potassium hydroxide and hydrogen peroxide
Aqueous solution is corroded；
It is preferred that concentration of potassium hydroxide is 5-10mol/L, hydrogen peroxide 5-10mol/L.
The third object of the present invention is the application of the interdigital electrode of the present invention, it is characterised in that by the porous gold modification
Interdigital electrode is applied to biological detection, Electrochemical Detection, gas detection or the sensing chip in above-mentioned detection or sensor group
Part.
Concrete application is illustrated such as：(1) in biological detection class sensor chip：Interdigital electrode modified on silicon substrate surface is more
Kong Jin, then protease is modified, it can be used as disease detection sensing chip.(2) Electrochemical Detection：The interdigital electrode of the porous gold of modified
Area load electrode active material is detected for Electroanalytical Chemistry.(3) air-sensitive detection：The interdigital electrode load of porous gold modification
Vapor sensitivity substance can be applied to gas sensor device.
The beneficial effects of the invention are as follows：
(1) increased by the active surface area in the porous gold of interdigital electrode surface modification contacting, it, increase sensor
Sensitivity, active material load can be significantly increased by porous gold modification, improve bio-sensing, electrochemical sensing and air-sensitive pass
The sensitivity of inductor component.
(2) porous gold utensil has higher stability, is easy to load various sensitive active materials on the surface thereof, can adapt to
Various different detection environment.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure for the porous gold modification interdigital electrode that embodiment 1 is prepared；
Fig. 2 is scanning electron microscope (SEM) figure for the porous gold modification interdigital electrode that embodiment 2 is prepared；
Figure (a) in Fig. 3 be the interdigital electrode working electrode (Au) that embodiment 3 is prepared and to electrode (Pt) in ceramics
The scanning electron microscope sem image on surface；Figure (b) is microcosmic scanning electron microscope (SEM) figure for the interdigital electrode that embodiment 3 is prepared；
Fig. 4 is the cyclic voltammetric of the porous gold modification interdigital electrode detection glucose oxidability of supporting Pt in application examples
Figure；
Fig. 5 is the pictorial diagram of double modification interdigital electrodes prepared by the present invention；
Fig. 6 is the scanning electron microscope of nickel foam surface modification porous golden interdigital electrode part and amplification prepared by the present invention
(SEM) figure.
Fig. 7 is the XRD spectrum of the porous golden interdigital electrode of nickel foam surface modification prepared by the present invention.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1,
The interdigital electrode of nano-porous gold modification：
(1) interdigital electrode surface will be commercialized to impregnate after ten minutes using the citric acid solution of 1%wt, deionized water cleaning
It is clean for use；
(2) surface-treated interdigital electrode is immersed into citric acid gold 10g/L, stannous sulfate 20g/L, ascorbic acid 10g/
L, potassium sulfate 20g/L, dipotassium hydrogen phosphate 20g/L, pH value is between 4-6, and temperature is between 45-55 DEG C, current density 1.0-
1.5ASF, electrodeposition time 5min obtain gold-tin alloy coating later.
(3) the interdigital electrode sample containing golden tin will be obtained and is immersed in potassium hydroxide 10mol/L, hydrogen peroxide 5mol/L is held
Continuous 3h, obtains the interdigital electrode of nano-porous gold modification.
Attached drawing 1 is scanning electron microscope (SEM) photograph of the interdigital electrode in 1 μm of grade of 1 nano-porous gold of embodiment modification, can be with from Fig. 1
It will become apparent from that there is uniform nano-porous structure.
Embodiment 2,
The interdigital electrode of nano-porous gold modification：
(1) interdigital electrode surface will be commercialized to impregnate after ten minutes using the citric acid solution of 1.5%wt, deionized water is clear
Wash clean is for use；
(2) surface-treated interdigital electrode is immersed into citric acid gold 20g/L, stannous sulfate 20g/L, ascorbic acid 10g/
L, potassium sulfate 20g/L, dipotassium hydrogen phosphate 20g/L, pH value are 5 or so, and temperature is between 45-55 DEG C, current density 2.0-
2.5ASF, electrodeposition time 5min obtain gold-tin alloy coating later.
(3) the interdigital electrode sample containing golden tin will be obtained and is immersed in potassium hydroxide 5mol/L, hydrogen peroxide 10mol/L is held
Continuous 3h, obtains the interdigital electrode of nano-porous gold modification.
Attached drawing 2 is scanning electron microscope (SEM) photograph of the interdigital electrode in 1 μm of grade of 2 nano-porous gold of embodiment modification, can be with from Fig. 2
It will become apparent from that there is uniform nano-porous structure.
Embodiment 3,
The batch production of the interdigital electrode of nano-porous gold modification：
(1) by magnetron sputtering Ti/Pt/Au on alumina ceramic plate, the ceramic substrate that outer surface is gold is formed, often
Layer sputters layer thickness
(2) using photoresist is coated with, photoresist thickness is 2 μm.
(3) develop under litho machine and expose, form interdigital electrode pattern.
(4) in solution of potassium carbonate, photoresist developing.
(5) band glue plating or citric acid solution immersion treatment after carry out plating form gold-tin alloy, solution composition is lemon
Lemon acid gold 8g/L, tin methane sulfonate 10g/L, ascorbic acid 10g/L, potassium sulfate 20g/L, dipotassium hydrogen phosphate 20g/L, pH value is in 4-
Between 6, temperature is between 45-55 DEG C, current density 1.0-1.5ASF, electrodeposition time 5min.
(6) photoresist is removed in potassium hydroxide solution, while being etched and being carried in the hydrofluoric acid solution of 5mol/L
The interdigital electrode of gold-tin alloy.
(7) sample is immersed to 5h in the potassium hydroxide of 10mol/L and the hydrogen peroxide of 5mol/L, obtains and is modified containing porous gold
Interdigital electrode sample.
Attached drawing 3 is scanning electron microscope (SEM) photograph of the interdigital electrode of 3 nano-porous gold of embodiment modification under different sizes.Fig. 3 (a)
In good order, Fig. 3 (b) shows the micro- of the nano gold layer on each interdigital electrode surface to the interdigitated electrode structure that display etching obtains
Pore structure and highly uniform.
Application examples,
Using the porous gold modification interdigital electrode of embodiment 1, hydro-thermal method is used again on the interdigital electrode surface of porous gold modification
One layer of Pt is modified, double modification interdigital electrodes are obtained, by double modification interdigital electrodes for following in 10mM glucose+1M KOH solutions
Ring voltammogram, blank solution are the potassium hydroxide solution of 1M, and reference electrode is Ag/AgCl electrodes, sweep speed 50mV/s.
Grape is detected afterwards from can be seen that the modified metal element (Pt) in porous gold modification interdigital electrode in attached drawing 4 (a)
Glycoxidative ability is remarkably reinforced relative to the testing result of the interdigital electrode of not supporting Pt, illustrates that the interdigital electrode of the present invention can
For blood sugar test.From in attached drawing 4 (b) it can be seen that testing result under the different current densities of 1.0-5.0ASF, porous
The interdigital electrode of golden supporting Pt has different degrees of enhancing to the detection of glucose oxidability, illustrates the interdigital of supported porous gold
Electrode has preferable stability under different test environments.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to before
Stating embodiment, invention is explained in detail, it will be understood by those of ordinary skill in the art that：It still can be to preceding
The technical solution recorded in each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
Modification or replacement, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution,
The essence of corresponding technical solution will not be made to be detached from the research and development spirit of the present invention.
Claims (10)
1. a kind of interdigital electrode of porous gold modification, it is characterised in that：In one layer of porous layer gold of common interdigital electrode face finish.
2. interdigital electrode according to claim 1, it is characterised in that：The interdigital electrode is alumina ceramic-base or height
Molecule base or silicon substrate or Metal Substrate interdigital electrode.
3. interdigital electrode according to claim 1, it is characterised in that：The thickness of the porous gold is 1-5 μm.
4. according to the interdigital electrode described in claim 1-3 any one, it is characterised in that：It can also be into after porous gold modification
Row secondary modification noble metal, metal oxide or proteinase activity substance.
5. the preparation method of the interdigital electrode according to claim 1-5 any one, it is characterised in that including steps are as follows：
1) common interdigital electrode is surface-treated, obtains surface-treated interdigital electrode；
2) in interdigital electrode surface deposited Au tin alloy layers；
3) tin in chemical corrosion method or electrochemical erosion method removal alloy, pure water cleaning is used to be drying to obtain porous gold modification
Interdigital electrode.
6. a kind of preparation method as claimed in claim 5, it is characterised in that the surface treatment of step 1) can be chemical treatment
Or electrochemical treatments, it is chemically treated to impregnate interdigital electrode in citric acid solution 10-30 minutes；Electrochemical treatments be by
Interdigital electrode is placed in electrochemical treatments in lye, specially：It is cathode by anode, platinized platinum of interdigital electrode, interdigital electrode is soaked
Enter in lye, energization processing；
Preferably, the citric acid concentration is 1-3%wt, and electrical current is 0.5-0.7A in the electrochemical treatments.
7. preparation method according to claim 5, it is characterised in that the gold-tin alloy in step 2) used in electrochemical deposition
Solution composition is soluble gold salt, soluble pink salt, ascorbic acid, potassium sulfate and dipotassium hydrogen phosphate；
It is preferred that the soluble gold salt is at least one of citric acid gold, aurous chloride potassium, sulfurous acid gold potassium, soluble tin
Salt is at least one of sulfurous acid tin, tin methane sulfonate, nitric acid tin；
It is preferred that the group of the gold-tin alloy solution becomes：Citric acid gold 10-50g/L, stannous sulfate 10-50g/L, ascorbic acid
10-40g/L, potassium sulfate 10-40g/L, dipotassium hydrogen phosphate 10-40g/L；
The group of preferred gold-tin alloy solution becomes：Citric acid gold 20-40g/L, stannous sulfate 20-40g/L, ascorbic acid
20-30g/L, potassium sulfate 20-30g/L, dipotassium hydrogen phosphate 20-30g/L.
8. preparation method according to claim 5, it is characterised in that in step 2) electrochemical deposition temperature be 40-60 DEG C,
Current density is 1.0-2.0ASF, time 5-20min, pH value 4-7；
Preferably, the electrodeposition temperature be 45-55 DEG C, current density 1.0-1.5ASF, time 5-10min, pH value
For 5-6.
9. preparation method according to claim 5, it is characterised in that in step 3), tin, tool are removed using chemical corrosion method
Body is corroded using the aqueous solution of potassium hydroxide and hydrogen peroxide,
It is preferred that concentration of potassium hydroxide is 5-10mol/L, hydrogen peroxide 5-10mol/L.
10. a kind of modify according to porous gold prepared by claim 1-4 any one or claim 5-9 any one methods
Interdigital electrode application, it is characterised in that by it is described it is porous gold modification interdigital electrode be applied to biological detection, electrochemistry examine
Survey, gas detection or the sensing chip in above-mentioned detection or sensor module.
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| CN109632909A (en) * | 2018-12-14 | 2019-04-16 | 惠州市金百泽电路科技有限公司 | A kind of production method of ceramic base sensing electrode surface fine-line |
| CN109828012A (en) * | 2019-03-01 | 2019-05-31 | 广州钰芯传感科技有限公司 | A kind of preparation method and application of the coplanar integrated interdigital electrode of three electrode |
| CN110148758A (en) * | 2018-12-28 | 2019-08-20 | 广州钰芯传感科技有限公司 | It is a kind of using carbohydrate as the porous gold electrode of fuel cell electro-catalysis and preparation method of raw material and its application in artificial intelligence sensor |
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| CN110148758A (en) * | 2018-12-28 | 2019-08-20 | 广州钰芯传感科技有限公司 | It is a kind of using carbohydrate as the porous gold electrode of fuel cell electro-catalysis and preparation method of raw material and its application in artificial intelligence sensor |
| CN109828012A (en) * | 2019-03-01 | 2019-05-31 | 广州钰芯传感科技有限公司 | A kind of preparation method and application of the coplanar integrated interdigital electrode of three electrode |
| CN110243901A (en) * | 2019-03-29 | 2019-09-17 | 惠州市钰芯电子材料有限公司 | A kind of no enzyme cortisol nanoporous platinum sensing electrode and its preparation method and application |
| CN110243901B (en) * | 2019-03-29 | 2021-11-16 | 惠州市钰芯电子材料有限公司 | Enzyme-free cortisol nano-porous platinum sensing electrode and preparation method and application thereof |
| CN110243894A (en) * | 2019-06-27 | 2019-09-17 | 惠州市钰芯电子材料有限公司 | Platinum/nano-porous gold tin/carbon fiber paper combination electrode preparation method that is a kind of while detecting ascorbic acid, dopamine, uric acid |
| CN110320255A (en) * | 2019-06-27 | 2019-10-11 | 广州钰芯传感科技有限公司 | A kind of nano-porous gold/carbon fiber paper multiple sensing electrodes preparation method and application can be used for detecting uric acid and dopamine simultaneously |
| CN110455894A (en) * | 2019-07-29 | 2019-11-15 | 惠州市钰芯电子材料有限公司 | A kind of nano-porous gold of sweat detection glucose is without enzyme flexible sensing electrode and the preparation method and application thereof |
| CN112630274A (en) * | 2020-07-31 | 2021-04-09 | 华南理工大学 | Nano-porous silver electrode for simultaneously detecting acetaminophen and dopamine, and preparation method and application thereof |
| CN112362707A (en) * | 2020-09-29 | 2021-02-12 | 广州钰芯传感科技有限公司 | Cobaltosic oxide modified nano-porous gold composite electrode and application thereof in chemical sensing |
| CN112362707B (en) * | 2020-09-29 | 2023-02-28 | 广州钰芯传感科技有限公司 | Cobaltosic oxide modified nano-porous gold composite electrode and application thereof in chemical sensing |
| CN112285182A (en) * | 2020-12-25 | 2021-01-29 | 广州钰芯智能科技研究院有限公司 | High-precision interdigital electrode and preparation method and application thereof |
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