CN104034765A - Electrochemical detection method through partial morphology scanning - Google Patents
Electrochemical detection method through partial morphology scanning Download PDFInfo
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- CN104034765A CN104034765A CN201410277284.9A CN201410277284A CN104034765A CN 104034765 A CN104034765 A CN 104034765A CN 201410277284 A CN201410277284 A CN 201410277284A CN 104034765 A CN104034765 A CN 104034765A
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Abstract
The invention provides an electrochemical detection method through partial morphology scanning by using an electrochemical detection device. The method comprises the following steps: performing rapid and long-distance control on a probe through a three-dimensional stepper motor, performing short-distance precise control through a piezoelectric ceramic sensor, keeping constant potential on a tested sample through a double-constant potential rectifier, meanwhile externally exerting an alternating current potential signal onto the testing probe, acquiring imaging information of three-dimensional spatial distribution of the electrochemical signal such as real part Zre, imaginary part -Zim, an absolute module value Z and a phase angle -Phase of a sample partial area through a data acquisition module, and acquiring element parameter information of an equivalent circuit. By adopting the method, the defects that a conventional scanning electrochemical microscope is weak in signal, hard in obtaining a feedback current density signal, single in detection signal and the like are overcome, partial microcosmic impedance distribution characteristics of the surface of a sample can be obtained, the information is rich, and the real characteristics of the sample can be studied and analyzed.
Description
Technical field
The present invention relates to Electrochemical Measurement Technology field, relate in particular to a kind of electrochemical detection method of regional area pattern scanning.
Background technology
Have based on image scan method part, microcosmic a variety of, such as atomic force microscope (AFM), scanning tunnel microscope (STM), contourgraph, scan-type electrochemical microscope (SECM) etc.For the harsh requirement under special study condition, researchist is combined atomic force microscope with Scanning electrochemical microscopy, atomic force microscope is combined with infrared spectrum technology etc., and the application of these partial sweep technology has significantly been expanded in the combination of technological means.Wherein, be mainly used in the Scanning electrochemical microscopy of electrochemical field through vicennial development in the past, become one of necessary means characterizing the reaction of material microcosmic surface and dynamics.
At present, scan-type electrochemical microscope is for multiple technologies field.Can obtain surperficial curent change feature image in the scanning of X-Y direction by probe; The performance of research ultramicroelectrode; Isomerization reaction dynamics; Homogeneous phase dynamics research; The research of biosystem, living cells or group; The research of surface reaction; Electro-catalysis application; Semiconductor surface research; Electrochemical research in slightly soluble liquid; Electro-deposition etc.
But the test request of scan-type electrochemical microscope is to have oxidation-reduction reaction to occur in the solution based on study sample, the feedback current density in test reaction process, the indirectly electrochemical properties of study sample.The test request of scan-type electrochemical microscope is comparatively harsh, and the distance that needs test probe and sample surfaces is between 10 μ m-20 μ m, and the feedback current density signal of testing a little less than, test process is subject to the interference of experiment condition and test environment.For corrosion research field etc., scan-type electrochemical microscope is difficult to the test surfaces pattern of original position, is also difficult to obtain real local Electrochemistry Information.For conventional corrosion experiment system, add oxidation-reduction material to cause great interference to the corrosion process of sample itself, the data that therefore scan-type electrochemical microscope can not synchronization gain corrosion process, this technology is not suitable for the application of corrosion field.These shortcomings have also limited the application of scan-type electrochemical microscope.
The problems that exist based on above scan-type electrochemical microscope test, as a little less than conventional scan-type electrochemical microscope signal, obtain the shortcomings such as feedback current density signal difficulty, detection signal are single, the present invention proposes a kind of electrochemical detection method for the scanning of regional area pattern, the local microcosmic distribution of impedance feature that it can obtain sample surfaces, mainly obtains the real part Z of the local pattern impedance spectrum of sample
re, imaginary part-Z
im, mould value | the three-dimensional spatial distribution of Z|, phasing degree-Phase, acquired information is abundant, is conducive to the genuine property of research analysis sample.The present invention combines ac impedance technology and three-dimensional fix technology, the present invention used the Techniques For Reducing such as signal amplifier, piezoelectric ceramics test signal noise, increased the precision that probe three dimensions moves.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of electrochemical detection method for the scanning of regional area pattern, its overcome the signal that conventional sweep electrochemical microscope exists weak, obtain the shortcomings such as feedback current density signal difficulty, detection signal are single, can obtain the local microcosmic distribution of impedance feature of sample surfaces, abundant information, is conducive to the genuine property of research analysis sample.
For solving the problems of the technologies described above, the invention provides a kind of electrochemical detection device for regional area pattern scanning, it comprises double potentiostat, probe signals receiving trap, lock-in amplifier, sample signal collector, electrolytic tank level-off knob, test probe, sample fixed station, contrast electrode, test electrolytic tank, electrolytic tank upper cover, to electrode and computing machine.
Wherein, double potentiostat link probe signals receiving trap, lock-in amplifier, sample signal collector, test probe, contrast electrode, to electrode.Sample signal collector has data acquisition module, collecting test probe, contrast electrode, the monitor signal that electrode related electrode and probe are obtained, by lock-in amplifier, by test signal amplification, denoising, probe signals receiving trap imports the signal of lock-in amplifier test into double potentiostat and carries out data processing and information feedback.Test probe, contrast electrode, to electrode composition three-electrode system.In test process, test probe, contrast electrode, electrode is put into test electrolytic tank, electrolytic tank upper cover covers and on electrolytic tank, prevents test system disturbance in test process, the fixing test sample that will study of sample fixed station, and computing machine is for the signal of collecting test probe.
Described probe signals receiving trap further comprises three-dimensional stepper motor and piezoceramic transducer, and piezoceramic transducer is arranged on three-dimensional stepper motor, respectively by translational speed and moving step length in software control X, Y, Z direction.
Described contrast electrode is Ag/AgCl electrode.
The testing current precision of described double potentiostat is 0.1nA; Voltage tester precision is 0.001mV; Maximum output voltage is ± 30V; Maximum output current is ± 2A.
The maximum moving distance of described piezoceramic transducer in space X, Y, Z direction is 100 μ m, and minimum moving step length is apart from 100nm.
Described test probe is platinum disk electrode (Pt purity > 99.9%) and golden disk electrode (Au purity > 99.9%), the insulated glassy layer of metal-cored outside surface of platinum disk electrode and golden disk electrode or resin bed parcel.The diameter of probe is between 100nm-30 μ m.
The present invention also provides the electrochemical detection method that adopts above-mentioned electrochemical detection device to carry out the scanning of regional area pattern, it realizes the control of quick, the long distance of probe by three-dimensional stepper motor, realize short-range accurate control by piezoceramic transducer, utilize double potentiostat to maintain constant potential on test sample, simultaneously additional ac potential signal on test probe, obtains the real part Z of sample regional area by the data acquisition module on computing machine
re, imaginary part-Z
im, mould value | the image-forming information of the three-dimensional spatial distribution of the electrochemical signals such as Z|, phasing degree-Phase, and obtain each component parameters information of equivalent electrical circuit.
Further, described electrochemical detection method comprises the steps,
The first step, carries out pre-service by test probe;
Second step, puts into electrolytic tank by test sample fixing, by test platform level-off, test probe is fixed in draw-in groove, by test probe, to electrode, contrast electrode and double potentiostat wiring;
The 3rd step, arranges bipotentiostat instrument parameter;
The 4th step, by controlling three-dimensional stepper motor and piezoceramic transducer, moves to test zone by test probe, tests;
The 5th step, will set the running software of test parameter, by test probe image data successively in X-Y plane, obtains the real part Z of regional area pattern impedance spectrum
re, imaginary part-Z
im, mould value | the three-dimensional spatial distribution of Z|, phasing degree-Phase;
The 6th step, carries out Fitting Analysis by test data according to the equivalent electrical circuit of test sample, electrode, solution system.
The described first step is further specially test probe successively in acetone, alcohol, ultrapure water (resistance is greater than 18.0M Ω), each ultrasonic cleaning 30 minutes, use again ultrapure water cleaning down clean, dry up with nitrogen or argon gas, complete the pre-service of test probe.
Testing sample in described second step is further specially the solid materials such as metal material, semiconductor material, conductive material, insulating material, can be also biomaterial, biologically active sample etc., and it is smooth, smooth that the test zone of sample surfaces keeps as far as possible.
The parameter of the double potentiostat arranging in described the 3rd step comprises additional constant voltage, additional alternating voltage amplitude, additional alternating current voltage frequency, number of test points etc., further additional constant voltage adjustable extent is-5.0V-5.0V, additional alternating voltage amplitude adjustable extent is-5.0V-5.0V, additional alternating current voltage frequency adjustable extent 0.0001Hz-120000Hz is that number of test points is any.
Test process in described the 4th step is specially probe along the vertical slow decreasing of Z-direction to sample surfaces, by the feedback current approximating curve decline probe of scan-type electrochemical microscope, until current density is uprushed, stops inserting needle.
The position that described test probe inserting needle can utilize the asymptotic curve of scan-type electrochemical microscope to carry out test probe is fixed, and also can artificially observe manual inserting needle, does not encounter sample surfaces.
Each element of the equivalent electrical circuit in described the 6th step comprises: probe interface resistance (R
tip), probe interface capacitance (C
tip), the example interface resistance (R of probe place
sample), the example interface electric capacity (C of probe place
sample), solution resistance (R
s), contrast electrode place example interface resistance (R '
sample), contrast electrode place example interface electric capacity (C '
sample).
Beneficial effect of the present invention:
The present invention is lower to the requirement of test probe diameter, and the test probe diameter of scan-type electrochemical microscope is 10 μ m or 25 μ m conventionally, and the minor increment of the local pattern that can differentiate must be greater than the diameter of probe.The present invention uses diameter 25 μ m probe test surface topographies, distinguishable go out the pattern of 5 μ m interval variation, significantly improve the resolution of local pattern.Reduced the requirement to test probe diameter simultaneously.
Test process of the present invention need to complete in conducting solution, without must rely on the material of oxidation-reduction reaction in solution to realize the detection of feedback current density as method of testings such as scan-type electrochemical microscopes.According to this feature, the present invention can realize the in situ detection of bulk solution, can truly reflect the electrochemical characteristic of testing sample.
The present invention can arrange arbitrarily the sweep frequency of impedance, can special sweep frequency be set for the feature of sample.
The present invention can obtain real part Zre, imaginary part-Zim, the mould value of local pattern impedance spectrum | the three-dimensional spatial distribution of Z|, phasing degree-Phase, and the corresponding data analysis software of combination is obtained the numerical value of the each element in equivalent electrical circuit.
Brief description of the drawings
Fig. 1 electrochemical detection device structural drawing for the scanning of regional area pattern provided by the invention;
Fig. 2 tests the equivalent circuit diagram of sample;
The platinized platinum sample depositing on Fig. 3 silicon chip;
The topographic profile of the conventional SECM test of Fig. 4 sample, unit: nA
The approximating curve of Fig. 5 test probe;
The impedance real part Z of the sample topography of Fig. 6 local ac sweep electro-chemical test of the present invention
redistributed in three dimensions, unit: Ω;
Imaginary impedance-the Z of the sample topography of Fig. 7 local ac sweep electro-chemical test of the present invention
imdistributed in three dimensions, unit: Ω;
The impedance magnitude of the sample topography of Fig. 8 local ac sweep electro-chemical test of the present invention | Z| distributed in three dimensions, unit: Ω;
Impedance phase angle-Phase distributed in three dimensions of the sample topography of Fig. 9 local ac sweep electro-chemical test of the present invention, unit: °.
Embodiment
The invention provides a kind of electrochemical detection device for regional area pattern scanning, it comprises double potentiostat, probe signals receiving trap, lock-in amplifier, sample signal collector, electrolytic tank level-off knob, test probe, sample fixed station, contrast electrode, test electrolytic tank, electrolytic tank upper cover, to electrode.And computing machine.
Wherein, double potentiostat link probe signals receiving trap, lock-in amplifier, sample signal collector, test probe, contrast electrode, to electrode.Sample signal collector has data acquisition module, collecting test probe, contrast electrode, the monitor signal that electrode related electrode and probe are obtained, by lock-in amplifier, by test signal amplification, denoising, probe signals receiving trap imports the signal of lock-in amplifier test into double potentiostat and carries out data processing and information feedback.Test probe, contrast electrode, to electrode composition three-electrode system.In test process, test probe, contrast electrode, electrode is put into test electrolytic tank, electrolytic tank upper cover covers and on electrolytic tank, prevents test system disturbance in test process, the fixing test sample that will study of sample fixed station, and computing machine is for the signal of collecting test probe.
Described probe signals receiving trap comprises three-dimensional stepper motor and piezoceramic transducer, and piezoceramic transducer is arranged on three-dimensional stepper motor, respectively by translational speed and moving step length in software control X, Y, Z direction.
Further, described electrochemical detection device is only made up of above-mentioned parts.
Described contrast electrode is Ag/AgCl electrode.
The testing current precision of described double potentiostat is 0.1nA; Voltage tester precision is 0.001mV; Maximum output voltage is ± 30V; Maximum output current is ± 2A.
The maximum moving distance of described piezoceramic transducer in space X, Y, Z direction is 100 μ m, and minimum moving step length is apart from 100nm.
Described test probe is platinum disk electrode (Pt purity > 99.9%) and golden disk electrode (Au purity > 99.9%), the insulated glassy layer of metal-cored outside surface of platinum disk electrode and golden disk electrode or resin bed parcel.The diameter of probe is between 100nm-30 μ m.
By utilizing additional AC impedance signal on the test probe of double potentiostat, and by the control of three-dimensional stepper motor and piezoceramic transducer, obtain the distributed in three dimensions of electrochemical signals.
The present invention also provides the electrochemical detection method that adopts above-mentioned electrochemical detection device to carry out the scanning of regional area pattern, it realizes the control of quick, the long distance of probe by three-dimensional stepper motor, realize short-range accurate control by piezoceramic transducer, utilize double potentiostat to maintain constant potential on test sample, simultaneously additional ac potential signal on test probe, obtains the real part Z of sample regional area by the data acquisition module on computing machine
re, imaginary part-Z
im, mould value | the image-forming information of the three-dimensional spatial distribution of the electrochemical signals such as Z|, phasing degree-Phase, and obtain each component parameters information of equivalent electrical circuit.
Further, described electrochemical detection method comprises the steps,
The first step, carries out pre-service by test probe;
Second step, puts into electrolytic tank by test sample fixing, by test platform level-off, test probe is fixed in draw-in groove, by test probe, to electrode, contrast electrode and double potentiostat wiring;
The 3rd step, arranges bipotentiostat instrument parameter;
The 4th step, by controlling three-dimensional stepper motor and piezoceramic transducer, moves to test zone by test probe, tests;
The 5th step, will set the running software of test parameter, by test probe image data successively in X-Y plane, obtains the real part Z of regional area pattern impedance spectrum
re, imaginary part-Z
im, mould value | the three-dimensional spatial distribution of Z|, phasing degree-Phase;
The 6th step, carries out Fitting Analysis by test data according to the equivalent electrical circuit of test sample, electrode, solution system.
Adopt the method, can obtain the three-dimensional distribution map with the microcell impedance signal of space distribution.
The described first step is further specially test probe successively in acetone, alcohol, ultrapure water (resistance is greater than 18.0M Ω), each ultrasonic cleaning 30 minutes, use again ultrapure water cleaning down clean, dry up with nitrogen or argon gas, complete the pre-service of test probe.
Testing sample in described second step is further specially the solid materials such as metal material, semiconductor material, conductive material, insulating material, can be also biomaterial, biologically active sample etc., and it is smooth, smooth that the test zone of sample surfaces keeps as far as possible.
The parameter of the double potentiostat arranging in described the 3rd step comprises additional constant voltage, additional alternating voltage amplitude, additional alternating current voltage frequency, number of test points etc.
In described the 3rd step, further according to testing requirement, utilize double potentiostat on sample, to apply constant voltage, executing alive precision is 0.001mV, AC impedance signal is added on test probe, utilize software that the electric signal output of double potentiostat is set, the AC impedance signal loading of output is on probe.Comprise: additional constant voltage (adjustable extent-10.0V-10.0V, precision 0.001mV), additional alternating voltage amplitude (adjustable extent-10.0V-10.0V, precision 0.001mV), additional alternating current voltage frequency (adjustable extent 0.0001Hz-120000Hz), electric current resolution 0.1nA, can increase arbitrarily or reduce test according to testing requirement and get and count etc.
Test process in described the 4th step is specially probe along the vertical slow decreasing of Z-direction to sample surfaces, by the feedback current approximating curve decline probe of scan-type electrochemical microscope, until current density is uprushed, stops inserting needle.
In described the 4th step, be to adopt the three-dimensional stepper motor of software control and piezoceramic transducer.
The position that described test probe inserting needle can utilize the asymptotic curve of scan-type electrochemical microscope to carry out test probe is fixed, and also can artificially observe manual inserting needle, does not encounter sample surfaces.
Each element of the equivalent electrical circuit in described the 6th step comprises: probe interface resistance (R
tip), probe interface capacitance (C
tip), the example interface resistance (R of probe place
sample), the example interface electric capacity (C of probe place
sample), solution resistance (R
s), contrast electrode place example interface resistance (R '
sample), contrast electrode place example interface electric capacity (C '
sample).
The present invention is additional AC signal on original probe, obtains the electrochemical impedance signal of microcosmic, and the feature such as pattern, Electrochemistry Information of this strong characterization sample surfaces has higher reliability and identity.
The present invention only needs solution conductivity, in solution, without the material that oxidation-reduction reaction significantly can occur, still can realize detection.
The present invention has overcome test probe need be from sample surfaces 10 μ m-20 μ m distances, probe of the present invention apart from sample surfaces 50 μ m with the interior signal that all can detect.
The present invention requires to reduce to the smooth finish of detecting probe surface, can make up test probe polishing totally do not cause cannot detection signal problem.
Below adopt embodiment to describe embodiments of the present invention in detail, to the present invention, how application technology means solve technical matters whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.
Embodiment 1
As shown in Figure 1, this electrochemical testing device comprises: (1) double potentiostat, (2) probe signals receiving trap, (3) lock-in amplifier, (4) sample signal collector, (5) electrolytic tank level-off knob, (6) test probe, (7) sample fixed station, (8) test sample, (9) contrast electrode, (10) test electrolytic tank, (11) electrolytic tank upper cover, (12) are to electrode.Wherein, (2) probe signals receiving trap also comprises three-dimensional stepper motor and piezoceramic transducer, (6) test probe can make platinum disk electrode (Pt purity > 99.9%) and golden disk electrode (Au purity > 99.9%), and (9) contrast electrode is Ag/AgCl electrode.As shown in Figure 2, by test probe, successively in acetone, alcohol, ultrapure water, each ultrasonic cleaning 30 minutes, then use ultrapure water cleaning down clean, dries up with nitrogen or argon gas the equivalent circuit diagram of test sample.Testing sample is adopted to the sample that deposits platinum on glass sheet, sample surfaces does not wash clean clearly, impurity is more.Every block of platinum is of a size of 49 μ m × 49 μ m, and the distance of every two blocks of platinum is spaced apart 24 μ m, as Fig. 3.It is the Pt probe of 25 μ m that test probe is selected diameter, and there is residual Al polishing rear surface
2o
3polishing powder.Use conventional SECM method of testing, the sample surfaces signal distribution plots recording is as Fig. 3.Because sample does not wash clean clearly, impurity is more, detecting probe surface does not wash clean clearly, cause test result not there is distinguishing, can not tell sample topography, as Fig. 4.Utilize device provided by the invention to set the external signal information on probe.Number of test points: 3.Additional constant voltage: 0.01V, additional alternating voltage amplitude: 0.1V, additional alternating current voltage frequency: 1000Hz-100000Hz.The position that utilizes the asymptotic curve of SECM to carry out test probe is fixed.The scanning area of test is of a size of 200 μ m × 200 μ m, and the step-length that probe moves is 25 μ m.The position that utilizes the asymptotic curve of SECM to carry out test probe is fixed, and as the approximating curve that Fig. 5 is test probe, along with moving down of probe, current density is the fixed position that can determine probe after exponential type rises or declines.After test, result is respectively real part Zre, imaginary part-Zim, the mould value of the local pattern impedance spectrum of sample as Fig. 6-Fig. 9 | the three-dimensional spatial distribution of Z|, phasing degree-Phase.The present invention can, in the situation that probe and sample have interference problem to exist, tell the electrochemical characteristic of Pt sheet, has embodied advantage of the present invention.
All above-mentioned these intellecture properties of primary enforcement, do not set restriction this new product of other forms of enforcement and/or new method.Those skilled in the art will utilize this important information, and foregoing amendment, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above, be only preferred embodiment of the present invention, is not the restriction of the present invention being made to other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (7)
1. the electrochemical detection method that adopts electrochemical detection device to carry out the scanning of regional area pattern, it is characterized in that: described electrochemical detection device comprises double potentiostat, probe signals receiving trap, lock-in amplifier, sample signal collector, electrolytic tank level-off knob, test probe, sample fixed station, contrast electrode, test electrolytic tank, electrolytic tank upper cover, to electrode and computing machine, described probe signals receiving trap comprises three-dimensional stepper motor and piezoceramic transducer;
Realize the control of quick, the long distance of probe by three-dimensional stepper motor, realize short-range accurate control by piezoceramic transducer, utilize double potentiostat to maintain constant potential on test sample, simultaneously additional ac potential signal on test probe, obtains the real part Z of sample regional area by the data acquisition module on computing machine
re, imaginary part-Z
im, mould value | the image-forming information of the three-dimensional spatial distribution of the electrochemical signals such as Z|, phasing degree-Phase, and obtain each component parameters information of equivalent electrical circuit.
2. electrochemical detection method as claimed in claim 1, is characterized in that: described electrochemical detection method comprises the steps,
The first step, carries out pre-service by test probe;
Second step, puts into electrolytic tank by test sample fixing, by test platform level-off, test probe is fixed in draw-in groove, by test probe, to electrode, contrast electrode and double potentiostat wiring;
The 3rd step, arranges bipotentiostat instrument parameter;
The 4th step, by controlling three-dimensional stepper motor and piezoceramic transducer, moves to test zone by test probe, tests;
The 5th step, will set the running software of test parameter, by test probe image data successively in X-Y plane, obtains the real part Z of regional area pattern impedance spectrum
re, imaginary part-Z
im, mould value | the three-dimensional spatial distribution of Z|, phasing degree-Phase.
3. electrochemical detection method as claimed in claim 1 or 2, it is characterized in that: the described first step is further specially test probe successively in acetone, alcohol, ultrapure water (resistance is greater than 18.0M Ω), each ultrasonic cleaning 30 minutes, use again ultrapure water cleaning down clean, dry up with nitrogen or argon gas, complete the pre-service of test probe.
4. the electrochemical detection method as described in claims 1 to 3, it is characterized in that: the testing sample in described second step is further specially the solid materials such as metal material, semiconductor material, conductive material, insulating material, also can be biomaterial, biologically active sample etc., it is smooth, smooth that the test zone of sample surfaces keeps as far as possible.
5. the electrochemical detection method as described in claim 1 to 4, is characterized in that: the parameter of the double potentiostat arranging in described the 3rd step comprises additional constant voltage, additional alternating voltage amplitude, additional alternating current voltage frequency, number of test points etc.
6. the electrochemical detection method as described in claim 1 to 5, it is characterized in that: the test process in described the 4th step is specially probe along the vertical slow decreasing of Z-direction to sample surfaces, by the feedback current approximating curve decline probe of scan-type electrochemical microscope, until current density is uprushed, stop inserting needle.
7. the electrochemical detection method as described in claim 1 to 6, it is characterized in that: the position that described test probe inserting needle can utilize the asymptotic curve of scan-type electrochemical microscope to carry out test probe is fixed, also can artificially observe manual inserting needle, not encounter sample surfaces.
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