CN104020316B - One kind is with compound scanning microprobe of bipolar electrode and preparation method thereof - Google Patents
One kind is with compound scanning microprobe of bipolar electrode and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of with the compound scanning microprobe of bipolar electrode, including a platinum filament microelectrode, a piece tungsten microelectrode, a piece glass tube with two endoporus, platinum filament microelectrode and tungsten microelectrode are attached separately in two endoporus of glass tube, at least it is filled with epoxy resin to fix platinum filament microelectrode and tungsten microelectrode in the bottom of two endoporus of glass tube, taper is worn into the lower end of the glass tube after epoxy resin cure, platinum filament microelectrode and tungsten microelectrode lower end form tip and are in exposed to outside and platinum filament microelectrode lower end under glass tube at the tip of end toper, the tungsten microelectrode lower end is oxidized to WO3, form W/WO3The upper end of microelectrode, platinum filament microelectrode and tungsten microelectrode is electrically connected with a wire respectively；A stainless steel tube is also cased with outside the glass tube；Invention additionally discloses the preparation method of above-mentioned microprobe；The present invention can measure metal surface STM images and pH value distribution simultaneously, and resolution ratio is high with detection efficiency.
Description
Technical field
The present invention relates to PSTM（STM）Microprobe, especially one kind can measure metal watch simultaneously
What face STM images and pH value were distributed carries compound scanning microprobe of bipolar electrode and preparation method thereof.
Background technology
PSTM scanning tunneling microscope are abbreviated as STM.It is scanned as one kind
Probe microscopy instrument, PSTM can allow scientist to observe and position single atom, and it has more similar than it
The resolution ratio that AFM is more increased.The performance of the microprobe of PSTM determines PSTM
Performance.
PSTM（STM）The scanning microelectrode measurement of auxiliary（SMET）System is used to study metal local corrosion
When, because the pH value of surrounding medium is influence one of topmost factor of metal erosion, metal local corrosion process and metal/molten
The H at liquid interface+Concentration and its distribution are closely related.Traditional glass pH electrode is generally using one layer than relatively thin glass-film conduct
Hydrionic sensitive membrane, easily occurs broken；And glass electrode volume is big, cost is high, it is difficult to is miniaturized, can only typically measure
Average pH value in tank solution system, it is impossible to meet the pH value in site measurement that there is metal/solution interface micrometer air space to differentiate
Requirement.Other this traditional glass pH electrode can not also measure metal surface STM images simultaneously.
The content of the invention
The compound scanning microprobe of bipolar electrode is carried the technical problem to be solved in the present invention is to provide one kind, can be surveyed simultaneously
Metal surface STM images and pH value distribution are measured, resolution ratio is high with detection efficiency.
The present invention also provides the preparation method of above-mentioned microprobe.
To reach above-mentioned purpose, the technical scheme is that：One kind carries the compound scanning microprobe of bipolar electrode, including
Piece platinum filament microelectrode, tungsten microelectrode, a glass tube with two endoporus, platinum filament microelectrode and a tungsten microelectrode
It is attached separately in two endoporus of glass tube, at least is filled with epoxy resin to fix platinum filament in the bottom of two endoporus of glass tube
Taper is worn into the lower end of the glass tube after microelectrode and tungsten microelectrode, epoxy resin cure, and platinum filament microelectrode and tungsten filament are micro-
Electrode lower end forms tip and is in exposed to outside and platinum filament microelectrode lower end under glass tube at the tip of end toper, the tungsten filament
Microelectrode lower end is oxidized to WO3, form W/ WO3Led respectively with one the upper end of microelectrode, platinum filament microelectrode and tungsten microelectrode
Line is electrically connected.
It is preferred that a diameter of 10~50 μm of the platinum filament microelectrode, a diameter of 10~50 μm of tungsten microelectrode, platinum filament is micro-
The tip diameter of electrode and tungsten microelectrode lower end is 0.1~1.0 μm.Further improve microprobe performance so that the micro- electricity of tungsten filament
Pole lower end W/WO3Electrode has good stability, invertibity, reappearance and quick time-response.
It is preferred that the platinum filament microelectrode and tungsten microelectrode are set in parallel in two endoporus of glass tube, platinum filament microelectrode
Spacing with tungsten microelectrode is 30~50 μm, and the lower end of tungsten microelectrode is higher than the lower end of platinum filament microelectrode for 15~35 μm.
Further improve microprobe performance, improve detection accuracy, rationally set the spacing of platinum filament microelectrode and tungsten microelectrode can be with
Preferably compensation corrosion system potential change causes error to hydrogen ion concentration measurement.
It is preferred that the upper end of the platinum filament microelectrode and tungsten microelectrode is connected with a copper conductor respectively by conducting resinl.
The upper end of platinum filament microelectrode and tungsten microelectrode is facilitated to be connected with external equipment, it is ensured that reliability of electrical connection.
Further improve, the bottom drawn undergauge of the glass tube is into capillary, glass tube lower end taper axial section
Wedge angle be 30 °~60 °.Further facilitate the use of probe.
Further improve, a stainless steel tube is also cased with outside the glass tube.Both microprobe was played a protective role,
Shielding action can be played in the detection, further improve the accuracy of detection.
The preparation method of above-mentioned microprobe is as follows：Comprise the following steps：
（1）10~50 μm of diameter, long 3 cm 10~50 μm of platinum filament and diameter, long 3cm tungsten filament are intercepted respectively；
（2）The glass tube with two endoporus is chosen, glass tube bottom stretches undergauge into capillary using glass tube tensilometer
Pipe；
（3）Platinum filament and tungsten filament are respectively charged into two endoporus of glass tube, and the bottom of two endoporus in glass tube
Filling epoxy resin to fix platinum filament and tungsten filament, make platinum filament and tungsten filament be parallel to each other and control the spacing of platinum filament and tungsten filament for 30~
50μm；
（4）After epoxy resin is fully cured, the lower end of glass tube is polished by glass polishing instrument, glass tube
Lower end wear into taper, control glass tube lower end taper axial section wedge angle be 30 °~60 ° so that platinum filament microelectrode and tungsten
Silk microelectrode lower end forms tip and is in exposed to outside and platinum filament microelectrode lower end under glass tube at the tip of end toper, control
The tip diameter of platinum filament and tungsten filament lower end is 0.1~1.0 μm, and the tip height difference of platinum filament and tungsten filament lower end is 15~35 μm, tungsten
The lower end of silk is in above platinum filament lower end；
（5）The upper end of platinum filament and tungsten filament is connected with a copper conductor respectively with conducting resinl；
（6）To being aoxidized exposed to outside tungsten filament tip, in one layer of densification WO of tungsten filament tip end surface formationXFilm layer,
Wherein X=1~3；
（7）The microprobe leaching prepared is hung over 2 mol/L H2SO4The middle aging for carrying out 1~4 week so that WOXFilm layer is equal
It is converted into WO3, wherein X=1~3 make tungsten filament tip completely form W/ WO3Microelectrode.
Further, needed in the platinum filament and tungsten filament before two endoporus of glass tube are loaded with acetone, absolute ethyl alcohol ultrasound
Clean and dry；The glass tube is using preceding needing by 1:4 30%H2O2Clean and dry with concentrated sulfuric acid mixed liquor.Ensure micro-
The preparation quality of probe.
It is preferred that the step（6）The method for oxidation at middle tungsten filament tip is electrochemical cyclic voltammetry, in 2mol/L H2SO4
In solution, using tungsten filament as working electrode, platinum filament is that, to electrode, selection saturated calomel electrode is reference electrode, control scanning current potential
Scope is 1.0~2.0V, and scan round number of times is 50~80 circles, and sweep speed is 20~50 mV/s；So as in the sophisticated table of tungsten filament
Face forms one layer of densification WOXFilm layer, wherein X=1~3.There is advantages below using electrochemical cyclic voltammetry：One is equipment letter
It is single, easy to operate, conditional parameter controllable precise；Two it is that prepared oxidation film is fine and close, is firmly combined with；Three be that can be answered in profile
Miscellaneous surface positioning prepares the oxidation film sensitive to hydrogen ion.And optimized state modulator is more convenient in tungsten filament tip end surface
Form one layer of densification WOXFilm layer.
Further, the above method is additionally included in a stainless steel tube in the outer cover of the microprobe glass tube prepared.
The present invention is due to the tip portion formation W/ WO in tungsten microelectrode lower end3Microelectrode, when temperature-resistant, WO3
Can be with hydrogen ion concentration change generation reversible reaction, W/WO in solution3The current potential of electrode is also with WO3Content difference and become
Change, W/WO3Electrode potential depends on H in medium+Activity.Therefore, when passing through scanning survey metal surface diverse location W/WO3
The Potential distribution of microprobe, the pH value distribution of metal/solution interface can be obtained indirectly.
On the other hand, during scanning survey, the tip of microprobe is held essentially constant with sample surfaces distance, close to sample
The platinum filament microelectrode on product surface not only act as tunnel current detection, with accurately control probe tips and sample surfaces away from
From effect, platinum filament microelectrode also acts as the effect of reference electrode in measurement process in addition, with W/WO3Microelectrode formation electrode
System, by the potential difference for measuring bipolar electrode tip, you can obtain sample light scanning figure.Platinum filament microelectrode can be quick simultaneously
Sense detection tunnel current, can measure sample surfaces structure and morphology image i.e. STM images.Actually platinum filament microelectrode has triple
Function：（a）Can sensitive tunnel current, accuracy controlling probe tip and sample surfaces distance；（b）In site measurement surface STM images；
(c) as W/WO3The reference electrode of microelectrode, accurate measurement surface microcell pH value Two dimensional Distribution.
Therefore, the present invention can measure metal surface STM images and pH value distribution simultaneously, and resolution ratio is high with detection efficiency.
Brief description of the drawings
Fig. 1 is the axial sectional view of the present invention；
Fig. 2 is the scanning microelectrode measuring system principle schematic that the present invention is aided in applied to STM；
Fig. 3 is the gray scale of surface pH value distribution of the present invention measurement R235 carbon steels in pH=10.6,0.01M NaCl solutions
Equipotential diagram；
Fig. 4 is the three-dimensional of surface pH value distribution of the present invention measurement R235 carbon steels in pH=10.6,0.01M NaCl solutions
Three-dimensional potential image；
Fig. 5 is the STM figures of present invention measurement R235 carbon steel sample surfaces.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Shown in Fig. 1, one kind carries the compound scanning microprobe of bipolar electrode, it is characterised in that：Including a platinum filament microelectrode
1st, tungsten microelectrode 2, a glass tube 3 with two endoporus 31,32, the bottom drawn undergauge of the glass tube 3
Into capillary, platinum filament microelectrode 1 and tungsten microelectrode 2 are attached separately in two endoporus 31,32 of glass tube 3, in 3 liang of glass tube
The bottom of individual endoporus is filled with epoxy resin 4 to fix platinum filament microelectrode 1 and tungsten microelectrode 2, and epoxy resin 4 is described after solidifying
Taper is worn into the lower end of glass tube 3, and platinum filament microelectrode 1 and the lower end of tungsten microelectrode 2 form tip exposed to outside and platinum filament is micro-
The lower end of electrode 1 is at the tip of 3 times end topers of glass tube, and the lower end of tungsten microelectrode 2 is oxidized to WO3, form W/ WO3It is micro-
The upper end of electrode, platinum filament microelectrode 1 and tungsten microelectrode 2 is electrically connected with a copper conductor 6 respectively by conducting resinl 5.
It is preferred that a diameter of 10~50 μm of the platinum filament microelectrode 1, a diameter of 10~50 μm of tungsten microelectrode 2, platinum filament
The tip diameter of microelectrode 1 and the lower end of tungsten microelectrode 2 is 0.1~1.0 μm.
It is preferred that the platinum filament microelectrode 1 and tungsten microelectrode 2 are set in parallel in two endoporus 31,32 of glass tube 3, it is excellent
The spacing for selecting platinum filament microelectrode 1 and tungsten microelectrode 2 is 30~50 μm, and the lower end of tungsten microelectrode 2 is higher than platinum filament microelectrode 1
Lower end is 15~35 μm.
It is preferred that the wedge angle of the lower end taper axial section of glass tube 3 is 30 °~60 °.
A stainless steel tube 7 is also cased with outside the glass tube 3.
The preparation method of above-mentioned microprobe is as follows：
（1）10~50 μm of diameter, long 3 cm platinum filament are intercepted respectively（The % of Pt content >=99.9）With 10~50 μm of diameter,
Long 3cm tungsten filament（The % of W content >=99.9）, it is cleaned by ultrasonic and dries using acetone, absolute ethyl alcohol；
（2）The glass tube with two endoporus is chosen, glass tube bottom stretches undergauge into capillary using glass tube tensilometer
Pipe, with 1:4 30%H2O2Clean and dry with concentrated sulfuric acid mixed liquor；
（3）Platinum filament and tungsten filament are respectively charged into two endoporus of glass tube, and the bottom of two endoporus in glass tube
Filling epoxy resin to fix platinum filament and tungsten filament, make platinum filament and tungsten filament be parallel to each other and control the spacing of platinum filament and tungsten filament for 30~
50μm；
（4）After epoxy resin is fully cured, the lower end of glass tube is polished by glass polishing instrument, glass tube
Lower end wear into taper, control glass tube lower end taper axial section wedge angle be 30 °~60 ° so that platinum filament microelectrode and tungsten
Silk microelectrode lower end forms tip and is in exposed to outside and platinum filament microelectrode lower end under glass tube at the tip of end toper, control
The tip diameter of platinum filament and tungsten filament lower end is 0.1~1.0 μm, and the tip height difference of platinum filament and tungsten filament lower end is 15~35 μm, tungsten
The lower end of silk is in above platinum filament lower end；
（5）The upper end of platinum filament and tungsten filament is connected with a copper conductor respectively with conducting resinl；
（6）To being aoxidized exposed to outside tungsten filament tip, in one layer of densification WO of tungsten filament tip end surface formationXFilm layer,
Wherein X=1~3；Specific method for oxidation is electrochemical cyclic voltammetry, in 2mol/L H2SO4In solution, using tungsten filament as work
Electrode, platinum filament is that, to electrode, selection saturated calomel electrode is reference electrode, and it is 1.0~2.0V, circulation to control scanning potential range
Scanning times are 50~80 circles, and sweep speed is 20~50 mV/s；So as in one layer of densification WO of tungsten filament tip end surface formationXFilm
Layer, wherein X=1~3；
（7）The microprobe leaching prepared is hung over 2 mol/L H2SO4The middle aging for carrying out 1~4 week so that WOXFilm layer is equal
It is converted into WO3, wherein X=1~3 make tungsten filament tip completely form W/ WO3Microelectrode；
（8）A stainless steel tube in the outer cover of the microprobe glass tube prepared.
Fig. 2 is the scanning microelectrode measuring system principle schematic that the present invention is aided in applied to STM, and it includes test sample to be checked
Product 9, computer 10, scanning microprobe 11, X-Y-Z three-dimensional piezoelectrics micro scanner 12, the scanning of driving stepper motor X-Y two-dimentional machineries
Advance signal conversion/amplifying circuit 15 of device 13, advance signal conversion/amplification and feedback circuit 14, micro-potential signals.
Detected sample 9 selects R235 carbon steels, and sample 9 is polishing to 2000# with silicon carbide paper is from coarse to fine, then uses 1 μ respectively
M and 0.3 μm of alumina powder is polished to minute surface, is cleaned with ethanol and deionized water, spontaneously dries.Then measurement sample 9 pH=
Surface pH value Two dimensional Distribution image in 10.6,0.01M NaCl solution.During measurement, the surface of 11 auto-feeding sample of microprobe 9,
Tunneling current signal is detected by the tip of platinum filament microelectrode first（Now platinum filament microelectrode tip with the surface distance of sample 9
Only nanoscale）, stopping inserting needle being automatically controlled by feedback circuit；Then microprobe 11 is raised upwards by computer program
5 μm, microprobe 11 is fallen again after adding test solution, the scanning survey of surface microcell pH value distribution is carried out, scan area is 4mm
X 4mm, surface p H two-dimensional distribution measurement results are shown in Fig. 3, Fig. 4, and Fig. 3 is gray scale equipotential diagram, and Fig. 4 is corresponding three-dimensional vertical
Bulk potential distribution map, is as a result proved, compound scanning microprobe of the invention can sensitively detect metal sample surface microcell
The distributed image of pH value two dimension, measurement resolution is high；Simultaneously can be with site measurement sample surfaces STM feature images, STM diagrams
In Fig. 5, as a result show that its definition is also preferable.
It the above is only a preferred embodiment of the invention, those skilled in the art is made equivalent change by claim
Both fall within the protection domain of this case.
Claims (7)
1. one kind carries the compound scanning microprobe of bipolar electrode, it is characterised in that：It is micro- including a platinum filament microelectrode, a tungsten filament
Electrode, a glass tube with two endoporus, platinum filament microelectrode and tungsten microelectrode are attached separately to two endoporus of glass tube
In, at least it is filled with epoxy resin to fix platinum filament microelectrode and tungsten microelectrode, epoxy in the bottom of two endoporus of glass tube
Taper is worn into the lower end of the glass tube after resin solidification, and platinum filament microelectrode and tungsten microelectrode lower end form tip exposure outside
At the tip of portion and platinum filament microelectrode lower end in end toper under glass tube, the tungsten microelectrode lower end is oxidized to WO3, formed
W/WO3The upper end of microelectrode, platinum filament microelectrode and tungsten microelectrode is electrically connected with a wire respectively；
A diameter of 10~50 μm of the platinum filament microelectrode, a diameter of 10~50 μm of tungsten microelectrode, platinum filament microelectrode and tungsten
The tip diameter of silk microelectrode lower end is 0.1~1.0 μm；
The bottom drawn undergauge of the glass tube into capillary, the wedge angle of glass tube lower end taper axial section for 30 °~
60°。
2. it is according to claim 1 a kind of with the compound scanning microprobe of bipolar electrode, it is characterised in that：The platinum filament is micro-
Electrode and tungsten microelectrode are set in parallel in two endoporus of glass tube, and the spacing of platinum filament microelectrode and tungsten microelectrode is 30
~50 μm, the lower end of tungsten microelectrode is higher than the lower end of platinum filament microelectrode for 15~35 μm.
3. it is according to claim 1 a kind of with the compound scanning microprobe of bipolar electrode, it is characterised in that：The platinum filament is micro-
The upper end of electrode and tungsten microelectrode is connected with a copper conductor respectively by conducting resinl.
4. one kind according to any one of claims 1 to 3 carries the compound scanning microprobe of bipolar electrode, it is characterised in that：
A stainless steel tube is also cased with outside the glass tube.
5. carrying the preparation method of the compound scanning microprobe of bipolar electrode described in a kind of any one of claims 1 to 3, its feature exists
In：Comprise the following steps：
(1) 10~50 μm of diameter, long 3cm 10~50 μm of platinum filament and diameter, long 3cm tungsten filament are intercepted respectively；
(2) glass tube with two endoporus is chosen, glass tube bottom stretches undergauge into capillary using glass tube tensilometer；
(3) platinum filament and tungsten filament are respectively charged into two endoporus of glass tube, and the bottom filling of two endoporus in glass tube
Epoxy resin makes platinum filament and tungsten filament be parallel to each other and control the spacing of platinum filament and tungsten filament to be 30~50 μ to fix platinum filament and tungsten filament
m；
(4) after epoxy resin is fully cured, the lower end of glass tube is polished by glass polishing instrument, under glass tube
Taper is worn at end, and the wedge angle for controlling glass tube lower end taper axial section is 30 °~60 ° so that platinum filament microelectrode and tungsten filament are micro-
Electrode lower end forms tip and is in exposed to outside and platinum filament microelectrode lower end under glass tube at the tip of end toper, controls platinum filament
Tip diameter with tungsten filament lower end is 0.1~1.0 μm, and the tip height difference of platinum filament and tungsten filament lower end is 15~35 μm, tungsten filament
Lower end is in above platinum filament lower end；
(5) upper end of platinum filament and tungsten filament is connected with a copper conductor respectively with conducting resinl；
(6) to being aoxidized exposed to outside tungsten filament tip, in one layer of densification WO of tungsten filament tip end surface formationXFilm layer, wherein X
=1~3；
(7) the microprobe leaching prepared is hung over 2mol/L H2SO4The middle aging for carrying out 1~4 week so that WOXFilm layer is converted
For WO3, wherein X=1~3 make tungsten filament tip completely form W/WO3Microelectrode；
The method for oxidation at tungsten filament tip is electrochemical cyclic voltammetry in the step (6), in 2mol/L H2SO4In solution, with
Tungsten filament is working electrode, and platinum filament is that, to electrode, selection saturated calomel electrode is reference electrode, and it is 1.0 to control scanning potential range
~2.0V, scan round number of times is 50~80 circles, and sweep speed is 20~50mV/s；So as in one layer of tungsten filament tip end surface formation
Fine and close WOXFilm layer, wherein X=1~3.
6. preparation method according to claim 5, it is characterised in that：The platinum filament and tungsten filament are loading two of glass tube
Need to be cleaned by ultrasonic and dried with acetone, absolute ethyl alcohol before endoporus；The glass tube is using preceding needing by 1:4 30%H2O2With
Concentrated sulfuric acid mixed liquor is cleaned and dried.
7. preparation method according to claim 5, it is characterised in that：It is additionally included in the outer of the microprobe glass tube for preparing
Portion puts a stainless steel tube.
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| CN111257596B (en) * | 2020-02-25 | 2021-09-14 | 西南交通大学 | Scanning probe microscope narrow and small experiment chamber environment atmosphere accurate control device |
| CN114354707B (en) * | 2021-12-16 | 2024-04-05 | 中国石油大学(华东) | Preparation method of flexible platinum-based electrochemical probe |
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| CN103439532A (en) * | 2013-09-02 | 2013-12-11 | 厦门乐钢材料科技有限公司 | Microelectrode technology for metal surface microcell current distribution in-situ detection |
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| "复合针型钨/氧化钨微pH传感器的研制";苗文方 等;《传感器技术》;19951231(第4期);第33页右栏最后一段至第34页左栏第3段及图1 * |
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