CN108982613A - Based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode system - Google Patents
Based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode system Download PDFInfo
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- 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
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- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The invention discloses a kind of based on nanochannel arrays surface spraying plating carbon/platinum integration type electrochemical electrode system.Using anode oxidation aluminium nanochannel arrays as carrier, pass through vacuum vapour deposition spraying plating carbon-coating in its one side, another side passes through ion sputtering process spraying plating platinum layer, then electrochemical workstation system is connected to by conducting wire, the carbon-coating of AAO one side is as working electrode, the platinum layer of another side is as reference electrode and to electrode, to construct electrode system.Electrode system of the invention is integrated with nanochannel and electrode, has Conventional electrochemical system function, and its is simple for production, small in size and easy to carry, easy to operate, has innovative and application prospect in micro-nano analysis and context of detection.
Description
Technical field
The invention belongs to a kind of electrochemical fields based on nanochannel, and in particular to one kind is based on nanochannel arrays table
Face spraying plating carbon/platinum integrative electrochemical electrode system.
Background technique
Nanochannel is structurally ordered, has moderately good physics and chemical property and has been commercialized, these features make it
There are huge potentiality in overdelicate single molecule analysis detection field, the detection technique based on nanochannel is also increasing.
Currently, can be divided mainly into electrochemical detection method and optical detecting method using the method that nanochannel is detected.Wherein, electric
Chemical detection method is easy to operate, high sensitivity, the favor by numerous researchers.And it is received with electrochemical test method detection
The cross-film electric signal in rice grain pattern road is a kind of common analysis means.
Electrode is essential a part in electro-chemical test.Using electrochemical workstation carry out nanochannel across
When film electric signal is tested, usually there are three types of test macros: bipolar electrode test macro, three electrode test systems and four electrode test systems
System.Conventional three electrodes and four electrode test systems often contain traditional reference electrode and to electrodes, in order to make these electrodes
It can not sufficiently can be omitted with electrolyte contacts, electrolytic cell；And conventional bipolar electrode test macro needs respectively to put two electrodes
The electrolytic cell for entering nanochannel both ends carries out electrical signal detection.In brief, conventional bipolar electrode, three electrodes and four electrode tests
In system, electrode is separated with nanochannel, and contains electrolytic cell；The two features cause the whole of conventional electrodes test macro to be surveyed
It is big to try environment volume, is unfavorable for the detection of analytes in low concentration.Therefore, the electrode system for seeking to integrate with nanochannel has
Significant innovative and application prospect.
Summary of the invention
The purpose of the present invention is the shortcoming for existing electrode system, by nanochannel and electrode fully-integratedization,
Reduce the volume of entire electrode system, development can be used for the model electrochemical system of micro-nano analysis, improve electrochemical analysis and inspection
The simplicity and sensitivity of survey.
To achieve the above object, The technical solution adopted by the invention is as follows:
The integrative electrochemical electrode system is working electrode, reference electrode and the three electrode test systems to electrode
Or bipolar electrode test macro, at least described working electrode are C-AAO-Pt electrode slice, C-AAO-Pt electrode slice is by anodic oxygen
Change aluminium nanochannel arrays (AAO) (sheet material) and spraying plating in the carbon-coating and platinum of anodised aluminium nanochannel arrays both side surface
Layer is constituted.
The C-AAO-Pt electrode slice is encapsulated by insulating layer and connects electrochemical workstation through conducting wire.
The C-AAO-Pt electrode slice that the present invention makes can be in conjunction with electrochemical workstation for electrochemical analysis and detection.
It is sprayed with carbon-coating and platinum layer, carbon-coating and platinum layer point respectively on two surface of lamella of anodised aluminium nanochannel arrays
Do not cover respective surface completely.Form the sandwich of sandwiched anodised aluminium nanochannel arrays lamella between carbon-coating and platinum layer
Structure.
The C-AAO-Pt electrode slice uses ion sputtering process anodised aluminium nanochannel arrays (AAO) with certain angle
It is intracavitary that degree is placed in ion sputtering, by adjusting sputtering current and time, in the side anodised aluminium nanochannel arrays (AAO) table
Face spraying plating platinum layer；Anodised aluminium nanochannel arrays (AAO) are placed in using vacuum vapour deposition by vacuum coating at a certain angle
Instrument is intracavitary, by adjusting electric current and time, in anodised aluminium nanochannel arrays (AAO) side surface spraying plating carbon-coating；To
Obtain C-AAO-Pt electrode slice.
It can be first in AAO one side spraying plating platinum layer；Again in another side spraying plating carbon-coating；It is final to obtain one side spraying plating platinum layer,
The C-AAO-Pt electrode slice of spraying plating carbon-coating on one side.
Thus C-AAO-Pt electrode slice that the present invention is prepared is found to have in the experiment of integrative electrochemical electrode
Nanometer enhancement effect, improves the sensitivity of electrochemical analysis and test.
When ion sputtering, the pedestal of plane and ion sputtering instrument cavity where anodised aluminium nanochannel arrays (AAO)
Angular range between plane is 5 °~80 °, and charging and discharging currents are not less than 3 μ A, and the spraying plating time is no less than 10s；When vacuum evaporation,
Plane where anodised aluminium nanochannel arrays (AAO) and the angular range between the base plane of vacuum coater cavity are
5 °~80 °, operating current is not less than 10A, and the spraying plating time is no less than 10s.
The anodised aluminium nanochannel arrays are bilateral type, include any aperture.
The carbon-coating and platinum layer of C-AAO-Pt electrode slice both side surface are separately connected using two conducting wires, using have viscosity and
The film material of waterproof is provided with engraved structure as insulating layer on insulating layer, insulating layer cladding is immersed in electrolyte solution
The connection contact portion of conductor part, conducting wire and C-AAO-Pt electrode slice and the C-AAO-Pt electrode slice in addition to engraved structure
Both side surface, C-AAO-Pt electrode slice only connect contact, C-AAO-Pt electrode slice two sides at engraved structure with electrolyte solution
Surface is provided with insulating layer, makes between electrolyte solution liquid level conductor part below and conducting wire and C-AAO-Pt electrode slice
Connection contact portion be not exposed to electrolyte solution.
C-AAO-Pt electrode slice both side surface is used as working electrode or C-AAO-Pt electrode slice side at engraved structure
Surface is used as working electrode at engraved structure and another side surface is used as reference electrode and to electrode at engraved structure.
The conducting wire includes but is not limited to spun gold, copper wire, platinum filament and aluminium foil.
The film material for having viscosity and waterproof includes but is not limited to dimethyl silicone polymer (PDMS) film and glue
Band.
Electrochemical analysis according to the present invention and test method include but is not limited to cyclic voltammetry, chronoamperometry and
Electrochemical impedance spectroscopy etc..
C-AAO-Pt electrode slice is immersed in conventional electrolyte solution in present invention specific implementation, constructs two-electrode system,
It can carry out conventional electro-chemical test (such as cyclic voltammetry, chronoamperometry, electrochemical impedance spectroscopy).
The C-AAO-Pt electrode chip size of specific implementation is limited in Nano grade.
In electrode system of the present invention, the carbon-coating of AAO one side is as working electrode, and the platinum layer of another side is as reference
Electrode and to electrode, to construct two-electrode system.The electrode system is suitable for conventional electrolyte solution, can be used for conventional electricity
Test chemical (such as cyclic voltammetry, Electrode with Electrochemical Impedance Spectroscopy, timing Amperometric).
The method have the benefit that:
1 compares conventional electrodes system, this electrode system metal and nonmetallic usage amount is small, preparation is easy, small in size, at
This and use aspect have significant advantage.
2 electrode systems of the present invention are suitable for Conventional electrochemical and analyze and measuring technology, in conjunction with nanochannel advantage,
Compared to conventional large volume electrode system, there is nanometer enhancement effect, be conducive to the sensitivity for improving electrochemical analysis and test, very
To the analysis and detection for realizing individual molecule.
3 electrode systems of the present invention are expected to be further developed into as micro-nano detection system.
For synthesis, electrode system of the present invention is integrated with nanochannel and electrode, has Conventional electrochemical system function, and
Its is simple for production, small in size and easy to carry, easy to operate, before micro-nano analysis and context of detection have innovative and application
Scape.
Detailed description of the invention
Fig. 1 is shown as electric based on nanochannel arrays surface spraying plating carbon/platinum integration type electrochemistry in the present invention
The component part figure of electrode systems.
Fig. 2 is shown as electric based on nanochannel arrays surface spraying plating carbon/platinum integration type electrochemistry in the present invention
The application method figure of electrode systems.
The scanning electron that Fig. 3 is shown as surface of the C-AAO-Pt electrode slice in the present invention before and after single face spraying plates platinum layer is aobvious
Micro mirror figure.
The scanning electron that Fig. 4 is shown as surface of the C-AAO-Pt electrode slice in the present invention before and after single side spraying plating carbon-coating is aobvious
Micro mirror figure.
Fig. 5 is shown as the scanning of longitudinal section of the C-AAO-Pt electrode slice in the present invention before and after two-sided spraying plating carbon/platinum layer
Electron microscope picture.
Fig. 6 is shown as the integration type electrochemical electrode system single side in the present invention as in three electrode test systems
Cyclic voltammetric (CV) curve graph tested in potassium ferricyanide solution when working electrode use, wherein figure A is integration type
CV curve graph of the electrochemical electrode system carbon-coating as working electrode schemes B for integration type electrochemical electrode system platinum layer work
For the CV curve graph of working electrode,.
Fig. 7 is shown as integration type electrochemical electrode system and rodlike commercialization glass-carbon electrode/platinum electricity in embodiment 1
Pole constructs two-electrode system respectively in 0.1M phosphate buffer solution and tests resulting electrochemical profiles figure, wherein figure A is CV
Curve graph, figure B are electrochemical impedance spectroscopy (EIS) curve graph, and figure C is timing ampere (i-t) curve graph.Dashed curve in figure is
The test result of C-AAO-Pt electrode system, block curve are commercialization glass-carbon electrode/platinum electrode test result.
The integration type electrochemical electrode system and be commercialized rodlike glass-carbon electrode/platinum electricity that Fig. 8 is shown as in embodiment 2
Pole constructs bipolar electrode in the solution (1mM potassium ferrocyanide/potassium ferricyanide solution) of the reduction electricity pair containing a pair of of inorganic oxide respectively
The resulting electrochemical profiles figure of system testing, wherein figure A is CV curve graph, figure B is EIS curve graph, and figure C is i-t curve graph.Figure
In dashed curve be C-AAO-Pt electrode system test result, block curve be commercialized the survey of glass-carbon electrode/platinum electrode
Test result.
The integration type electrochemical electrode system and be commercialized rodlike glass-carbon electrode/platinum electricity that Fig. 9 is shown as in embodiment 3
Building two-electrode system tests resulting electrochemical profiles figure in a kind of organic solution (5mM 1,4-benzoquinone solution) respectively for pole,
Wherein figure A is CV curve graph, and figure B is EIS curve graph, and figure C is i-t curve graph.Dashed curve in figure is C-AAO-Pt electrode
The test result of system, block curve are commercialization glass-carbon electrode/platinum electrode test result.
Figure 10 is shown as the integration type electrochemical electrode system in embodiment 4 before and after BSA closing respectively at the Asia 1mM
Two-electrode system is constructed in the potassium ferricyanide/potassium ferricyanide solution and tests resulting electrochemical profiles figure, wherein figure A is CV curve
Figure, figure B are EIS curve graph, and figure C is i-t curve graph.Solid line song in figure is the electrode test curve before BSA processing, and dotted line is bent
Line is BSA treated electrode test curve.
Rodlike glass-carbon electrode/the platinum electrode of the commercialization that Figure 11 is shown as in embodiment 4 is before and after BSA closing respectively at 1mM
Two-electrode system is constructed in potassium ferrocyanide/potassium ferricyanide solution and tests resulting electrochemical profiles figure, wherein figure A is CV curve
Figure, figure B are EIS curve graph, and figure C is i-t curve graph.Solid line song in figure is the electrode test curve before BSA processing, and dotted line is bent
Line is BSA treated electrode test curve.
In figure: 1 represents anodised aluminium nanochannel arrays, and 2 represent carbon-coating, and 3 represent platinum layer, and 4 represent conducting wire, and 5 represent
Insulating layer.
Specific embodiment
Below by way of specific specific example combination attached drawing, embodiments of the present invention will be described, but may be noted that
Implementation of the invention embodiment not limited to the following.
The embodiment of the present invention is as follows:
(1) production of integrative electrochemical electrode system:
As shown in Figure 1, in the sheet material both side surface spraying plating carbon-coating 2 and platinum of anodised aluminium nanochannel arrays (AAO) 1
Layer 3 forms C-AAO-Pt electrode slice, and C-AAO-Pt electrode slice both ends are connected by the encapsulation of insulating layer 5 and with conducting wire 4, and conducting wire 4 connects
Connect electrochemical workstation.Two conducting wires 4 are separately connected C-AAO-Pt electrode slice both ends, and insulating layer is the film with viscosity and waterproof
Shape material, using spun gold as conducting wire in embodiment, using adhesive tape as insulating layer.
It is discussed in detail taking the embodiment as an example below novel based on nanochannel arrays surface spraying plating carbon/platinum in the present invention
The production method and characterization result of integrative electrochemical electrode system.
Firstly, the AAO that aperture is 160-200nm is fixed on the glass sheet, it is put into the cavity of ion sputtering instrument, sheet glass
It is in 20 ° of angles with base plane.Charging and discharging currents in metallization process are 15 μ A, and the spraying plating time is 200s.By a side of AAO
After the parameter spraying plating platinum layer, AAO is removed, the cavity of vacuum coater is put into, the one side of spraying plating will not carried out in face of carbon target
It fixes on the glass sheet.Operating current in metallization process is 20~50A, repeats vapor deposition 25 times, and each evaporation time is 10s.
After spraying plating, one side spraying plating platinum layer is removed, on one side the C-AAO-Pt electrode slice of spraying plating carbon-coating.
Electron microscope and element are scanned to the C-AAO-Pt electrode slice after the AAO and spraying plating carbon/platinum layer before spraying plating
Distribution characterization.As it can be seen that the scanning electron microscope on surface of the comparison C-AAO-Pt electrode slice before and after single face spraying plates platinum layer in Fig. 3
Figure, it can be found that the C-AAO-Pt electrode slice after spray platinum platinum layer occurs compared to the surface AAO；As it can be seen that comparison C-AAO- in Fig. 4
The scanning electron microscope diagram on surface of the Pt electrode slice before and after single side spraying plating carbon-coating, it can be found that the C-AAO-Pt electricity after spray carbon
There is carbon-coating compared to the surface AAO in pole piece；As it can be seen that comparison C-AAO-Pt electrode slice is before and after two-sided spraying plating carbon/platinum layer in Fig. 5
Longitudinal section scanning electron microscope diagram, cut it can be found that C-AAO-Pt electrode slice after spraying plating carbon/platinum layer is vertical compared to AAO
Face does not have significant difference.According to Elemental redistribution in table characterize as a result, it can be found that C-AAO-Pt electrode after spraying plating carbon/platinum
Piece increases compared to AAO electric conductivity, and surface platinum content rises to 2.04% from 0%, and carbon contents rise to from 5.00%
71.52%.
Then, it is separately connected two sides of C-AAO-Pt electrode slice using two spun golds, is coated under lid spun gold with adhesive tape
End and the contact portion between spun gold and electrode slice, adhesive tape are sheet, and tape surface opens up circular hole, and make C-AAO-Pt electric simultaneously
Plating carbon-coating or plating platinum layer exposure at the circular hole of pole piece both side surface are used as electrode.Adhesive tape has viscosity, and spun gold is sealed, gold is made
Silk does not contact solution.
Two sides difference spraying plating carbon of AAO and platinum layer, the i.e. two sides AAO are integrated with a carbon electrode and a platinum electricity respectively
C-AAO-Pt electrode slice is collectively formed in pole, AAO and C, Pt.Integrated C-AAO-Pt electrode slice and spun gold and adhesive tape are packaged with
The volume of entire electrode system is reduced to effect, this is a kind of based on nanochannel arrays surface spraying plating carbon/platinum integration type
Electrochemical electrode system meets integrated, portability requirements, has innovative and application prospect.
Using the carbon-coating of C-AAO-Pt electrode slice one side or platinum layer as working electrode, using standard calomel electrode as reference electricity
Pole is to carry out electrochemical Characterization, electrolyte solution in three electrode test systems with cyclic voltammetric (CV) method to electrode with carbon-point
For the phosphate buffer solution containing the potassium ferricyanide, characterization result is as shown in Figure 6.As can be known from Fig. 6, two sides is individually as work
Make electrode, the CV curve measured in three-electrode system can completely show a pair of of redox character of the potassium ferricyanide
Peak, and the peak voltage difference in A figure is about 1100mV, the peak voltage difference in B figure is about 150mV, illustrates C-AAO-Pt electrode slice two
Electrode (C/Pt) electric conductivity at end is good, can be used as the use of routine work electrode.
(2) use of integrative electrochemical electrode system:
As shown in Fig. 2, the substance in beaker represents conventional electrolyte solution.By the C-AAO-Pt electrode slice in electrode system
Electrolyte solution is immersed, the carbon-coating of C-AAO-Pt electrode slice one side is as working electrode, and the platinum layer of another side is as reference
Electrode and to electrode, constitutes two-electrode system.C-AAO-Pt electrode slice, conducting wire, electrolyte solution and electrochemical workstation are in electricity
Access is constituted when test chemical, carries out the measurement of cross-film electric signal, test method includes but is not limited to cyclic voltammetric (CV) method, electricity
Chemical impedance composes (EIS) method, timing ampere (i-t) method.
Embodiment 1:
In this instance, the conventional electrolyte solution used is the phosphate buffer solution of 0.1M.It will be in novel electrode system
C-AAO-Pt electrode slice immerse electrolyte solution, with the conducting wire of carbon-coating in the working electrode connection electrode of electrochemical workstation,
Reference electrode and conducting wire to platinum layer in electrode connection electrode constitute two-electrode system, carry out electro-chemical test, test result is such as
The dashed curve of Fig. 7.
One of purchase rodlike commercialization glass-carbon electrode and a rodlike commercialization platinum electrode are immersed into the electrolyte solution,
For rodlike commercialization electrode sources in Tianjin joint Science and Technology Ltd. of English section, glass-carbon electrode connects the work electricity of electrochemical workstation
Pole, platinum electrode connect the reference electrode of electrochemical workstation and to electrodes, constitute two-electrode system, carry out and C-AAO-Pt electrode
Identical electro-chemical test, the block curve of test result such as Fig. 7.
What Fig. 7 A was represented is CV curve, and specific measurement parameter: scanning voltage is -0.4V~0.4V, sweep speed 0.1V/
s；What Fig. 7 B was represented is EIS curve, specific measurement parameter: frequency range is 1~10^5Hz, initial voltage 0V, and amplitude is
0.01V；What Fig. 7 C was represented is i-t curve, and specific measurement parameter: initial voltage is -0.2V, testing time 600s.
It can be seen that from Fig. 7 A, 7B since the size of carbon particle is larger, affect the circulation of electrolyte solution, so that C-
The ionic current of AAO-Pt electrode system is reduced, and solution resistance increases.It can be seen that the electricity of C-AAO-Pt electrode system from Fig. 7 C
Stream is identical relative to rodlike commercialization glass-carbon electrode/platinum electrode system power trend, but electric current may be significantly smaller, and be consistent with 7A result
It closes.Illustrate that C-AAO-Pt electrode system successfully can carry out electrochemistry letter as two-electrode system in 0.1M phosphate buffer solution
Number measurement, show electro-chemical systems of the present invention be suitable for using conventional buffers electrochemical system.
Embodiment 2:
In this instance, the conventional electrolyte solution used is that (a pair of of inorganic oxide is also for 1mM potassium ferrocyanide/potassium ferricyanide
Former electricity to) solution.The mode such as embodiment 1 of electrochemical signals measurement, Electrochemical results are as shown in figure 8, dotted line in figure
Curve is the test result of C-AAO-Pt electrode system, and block curve is commercialization glass-carbon electrode/platinum electrode test result.
What Fig. 8 A was represented is CV curve, and specific measurement parameter: scanning voltage is respectively -1V~1V and -0.4V~0.4V, is swept
Retouching rate is 0.1V/s；What Fig. 8 B was represented is EIS curve, and what Fig. 8 C was represented is i-t curve, and specific measurement parameter is and embodiment
1 is identical.As can be seen that C-AAO-Pt electrode system can be symbolized successfully with commercialization glass-carbon electrode/platinum electrode from Fig. 8 A
The characteristic peak of this oxidation-reduction pair illustrates that two kinds of electrodes can be successfully to inorganic oxide reduction electricity to characterizing.
It can be seen from fig. 8b that C-AAO-Pt electrode system is compared to business polarizing electrode, solution resistance is similar, but charge
Transfer resistance significantly increases, this is carbon-coating and platinum layer by C-AAO-Pt electrode system as electrode and the rodlike glass carbon of commercialization
Caused by the difference of electrode/platinum electrode charge transport capability.The test curve trend of two kinds of electrodes is consistent in Fig. 8 C, further
It illustrates the similitude of two kinds of electrodes and the practicability of C-AAO-Pt electrode system, also indicates that electro-chemical systems of the present invention are suitable for
Using the electrochemical system of inorganic oxide reduzate.
Embodiment 3:
In this instance, the conventional electrolyte solution used is 5mM 1,4-benzoquinone (classical oxidation-reduction quality organic matter) solution.
The mode such as embodiment 1 of electrochemical signals measurement, Electrochemical results are as shown in Figure 9.
Dashed curve in figure is the test result of C-AAO-Pt electrode system, block curve be commercialization glass-carbon electrode/
The test result of platinum electrode.What Fig. 9 A was represented is CV curve, and specific measurement parameter: scanning voltage is -1.5V~1.5V, scanning speed
Rate is 0.1V/s；What Fig. 9 B was represented is EIS curve, and specific measurement parameter is same as Example 1；What Fig. 9 C was represented is i-t curve,
Specific measurement parameter: initial voltage is -0.8V, testing time 600s.As can be seen from Figure 9A, C-AAO-Pt electrode system and
Rodlike commercialization glass-carbon electrode/platinum electrode successfully symbolizes the characteristic peak of 1,4-benzoquinone, but the number of characteristic peak has difference, the two
There is difference on charge transport capability, but the characterization of electrolyte solution is not influenced.The difference of EIS curve both in Fig. 9 B
The difference of its bright surface charge transfer resistance of dissenting views, it is consistent with Fig. 9 A.I-t curvilinear trend both in Fig. 9 C is identical, further
Prove the similitude of two kinds of electrodes.
By the comparison of Fig. 9 it is found that C-AAO-Pt electrode system and rodlike commercialization glass-carbon electrode/platinum electrode successful can exist
The measurement of feature electric signal and the characterization of electrode surface situation are carried out in 1,4-benzoquinone solution, show that electro-chemical systems of the present invention are applicable in
In the electrochemical system using redox organic matter.
Embodiment 4:
By the C-AAO-Pt electrode slice in novel electrode system, a rodlike commercialization glass-carbon electrode and a rodlike business
Change platinum electrode to impregnate one hour in 4%BSA solution respectively, after taking-up with milli-Q water three times, then dry up electrode surface.
C-AAO-Pt electrode slice and commercialization glass-carbon electrode/platinum electrode after will be processed is respectively at 1mM potassium ferrocyanide/potassium ferricyanide
Measured in solution, what figure A was represented is CV curve, specific measurement parameter: scanning voltage be respectively -1V~1V and -0.4V~
0.4V, sweep speed 0.1V/s；Scheme B representative is EIS curve, and what figure C was represented is i-t curve, measurement method and specific survey
Measure parameter such as embodiment 2.
C-AAO-Pt electrode system is as shown in Figure 10 in the electric signal comparison diagram of BSA before and after the processing, and commercialization glass-carbon electrode/
Platinum electrode is as shown in figure 11 in the electric signal comparison diagram of BSA before and after the processing, and Figure 10, the block curve in 11 represent BSA processing
Preceding electrode test curve, dashed curve represent BSA treated electrode test curve.
Schemed from the two CV of Figure 10 A, 11A as can be seen that two kinds of electrodes can not after BSA processing before relative to processing
The characteristic peak for symbolizing this oxidation-reduction pair illustrates the charge transport capability decline of electrode.From Figure 10 B, 11B the two
EIS figure illustrates electricity as can be seen that BSA treated two kinds of electrodes are significantly increased relative to electric charge transfer steric hindrance before handling
The charge transport capability of pole surface declines, consistent with CV figure result.From the two i-t of Figure 10 C, 11C figure as can be seen that from BSA
The i-t curve for managing two kinds of electrodes of front and back is also varied.
By the comparison of Figure 10, Figure 11 it is found that C-AAO-Pt electrode system, rodlike commercialization glass-carbon electrode/platinum electrode are in BSA
Treated, and variation tendency is identical, shows that the electrode surface of electro-chemical systems of the present invention has and commercialization glass-carbon electrode/platinum electricity
The extremely similar adsorption capacity to protein, suitable for the electrochemical system that need to be surface modified.
These results suggest that one of present invention is based on nanochannel arrays surface spraying plating carbon/platinum integration type
Electrochemical electrode system can apply in conventional electrolyte solution, carry out the measurement of electrochemical signals, and chemical property
It can match in excellence or beauty in common rodlike commercialization glass-carbon electrode/platinum electrode.
Claims (9)
1. a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode system, the integrated electric
Chemical electrode system is three electrode test systems or bipolar electrode test macro, it is characterised in that: at least described working electrode is
C-AAO-Pt electrode slice, C-AAO-Pt electrode slice are by anodised aluminium nanochannel arrays (AAO) (1) and spraying plating in anodic oxygen
The carbon-coating (2) and platinum layer (3) for changing aluminium nanochannel arrays (1) both side surface are constituted.
2. according to claim 1 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: the C-AAO-Pt electrode slice is encapsulated by insulating layer (5) and connects electrochemistry work through conducting wire (4)
It stands.
3. according to claim 1 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: be sprayed with carbon-coating (2) and platinum respectively on two surface of lamella of anodised aluminium nanochannel arrays (1)
Layer (3), carbon-coating (2) and platinum layer (3) completely cover respective surface respectively.
4. according to claim 1 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: the C-AAO-Pt electrode slice is using ion sputtering process anodised aluminium nanochannel arrays (AAO)
It is intracavitary that it is placed in ion sputtering at a certain angle, by adjusting sputtering current and time, in anodised aluminium nanochannel arrays
(AAO) a side surface spraying plating platinum layer；Anodised aluminium nanochannel arrays (AAO) are set at a certain angle using vacuum vapour deposition
It is intracavitary in vacuum coater, by adjusting electric current and time, in anodised aluminium nanochannel arrays (AAO) side surface spraying plating
Carbon-coating；To obtain C-AAO-Pt electrode slice.
5. according to claim 4 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: when ion sputtering, plane and ion sputtering instrument chamber where anodised aluminium nanochannel arrays (AAO)
Angular range between the base plane of body is 5 °~80 °, and charging and discharging currents are not less than 3 μ A, and the spraying plating time is no less than 10s；Very
When sky vapor deposition, where anodised aluminium nanochannel arrays (AAO) between plane and the base plane of vacuum coater cavity
Angular range is 5 °~80 °, and operating current is not less than 10A, and the spraying plating time is no less than 10s.
6. according to claim 1 or 2 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electricity
Electrode systems, it is characterised in that: the carbon-coating and platinum layer of C-AAO-Pt electrode slice both side surface are separately connected using two conducting wires (4),
Insulating layer is used as using the film material with viscosity and waterproof, engraved structure is provided on insulating layer, insulating layer is coated and is immersed in
The connection contact portion of conductor part, conducting wire and C-AAO-Pt electrode slice in electrolyte solution and in addition to engraved structure
C-AAO-Pt electrode slice both side surface, C-AAO-Pt electrode slice only connect contact at engraved structure with electrolyte solution.
7. according to claim 6 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: C-AAO-Pt electrode slice both side surface is at engraved structure as working electrode or C-AAO-Pt electricity
One side surface of pole piece at engraved structure as working electrode and another side surface at engraved structure as reference electrode and right
Electrode.
8. according to claim 1 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: the conducting wire (4) includes but is not limited to spun gold, copper wire, platinum filament and aluminium foil.
9. according to claim 1 a kind of based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode
System, it is characterised in that: the film material with viscosity and waterproof includes but is not limited to dimethyl silicone polymer
(PDMS) film and adhesive tape.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810709681.7A CN108982613A (en) | 2018-07-02 | 2018-07-02 | Based on nanochannel arrays surface spraying plating carbon/platinum integrative electrochemical electrode system |
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| CN109725025A (en) * | 2019-02-22 | 2019-05-07 | 清华大学 | A kind of test equipment and method of the membrane electrode of solid oxide fuel cell |
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