CN104020316A - Composite type scanning microprobe with dual electrodes and preparation method thereof - Google Patents
Composite type scanning microprobe with dual electrodes and preparation method thereof Download PDFInfo
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- CN104020316A CN104020316A CN201410265812.9A CN201410265812A CN104020316A CN 104020316 A CN104020316 A CN 104020316A CN 201410265812 A CN201410265812 A CN 201410265812A CN 104020316 A CN104020316 A CN 104020316A
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Abstract
The invention discloses a composite type scanning microprobe with dual electrodes. The composite type scanning microprobe comprises a platinum filament microelectrode, a tungsten filament microelectrode and a glass tube with two inner holes. The platinum filament microelectrode and the tungsten filament microelectrode are arranged in the two inner holes of the glass tube respectively, and the lower portions of the two inner holes of the glass tube are at least respectively filled with epoxy resin to fix the platinum filament microelectrode and the tungsten filament microelectrode. After the epoxy resin is solidified, the lower end of the glass tube is ground to be in a cone shape, sharp ends are formed at the lower end of the platinum filament microelectrode and the lower end of the tungsten filament microelectrode and are exposed to the outside, and the lower end of the platinum filament microelectrode is placed at the conical sharp end of the lower end of the glass tube. WO3 is formed at the lower end of the tungsten filament microelectrode in an oxidation mode, a W/WO3 microelectrode is formed, and the upper end of the platinum filament microelectrode and the upper end of the tungsten filament microelectrode are respectively and electrically connected with a wire. The glass tube is further sleeved with a stainless steel tube. The invention further discloses a preparation method of the composite type scanning microprobe. According to the composite type scanning microprobe with the dual electrodes and the preparation method thereof, STM images and pH value distribution can be measured on a metal surface at the same time, and the resolution ratio and the detection efficiency are high.
Description
Technical field
The present invention relates to the microprobe of scanning tunnel microscope (STM) use, especially a kind of can measure that metal surface STM image and pH value distribute simultaneously with compound scanning microprobe of bipolar electrode and preparation method thereof.
Background technology
Scanning tunnel microscope scanning tunneling microscope is abbreviated as STM.It is as a kind of Scanning Probe Microscopy instrument, and scanning tunnel microscope can allow scientist observe and locate single atom, and it has the resolution of more increasing than its similar atomic force microscope.The performance of the microprobe that scanning tunnel microscope is used has determined scanning tunnel microscope performance.
When auxiliary scanning microelectrode measurement (SMET) system of scanning tunnel microscope (STM) is used for studying metal local corrosion, because the pH value of surrounding medium is to affect one of topmost factor of metal erosion, the H of metal local corrosion process and metal/solution interface
+concentration and distribute closely related.Traditional glass pH electrode adopts glass-film that one deck is thinner as hydrionic sensitive membrane conventionally, very easily occurs broken; And glass electrode volume is large, cost is high, is difficult to microminiaturization, generally can only measure pH value average in tank solution system, cannot meet metal/solution interface and have the requirement of the pH value in site measurement of micron spatial discrimination.This traditional glass pH electrode also cannot be measured metal surface STM image simultaneously in addition.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of with the compound scanning microprobe of bipolar electrode, can measure metal surface STM image and pH value simultaneously and distribute, and resolution and detection efficiency are high.
The present invention also provides the preparation method of above-mentioned microprobe.
For achieving the above object, technical scheme of the present invention is: a kind of with the compound scanning microprobe of bipolar electrode, comprise a platinum filament microelectrode, a tungsten microelectrode, a glass tube with two endoporus, platinum filament microelectrode and tungsten microelectrode are contained in respectively in two endoporus of glass tube, at least be filled with epoxy resin to fix platinum filament microelectrode and tungsten microelectrode in the bottom of two endoporus of glass tube, after epoxy resin cure, taper is worn in the lower end of described glass tube, platinum filament microelectrode and tungsten microelectrode lower end taper off to a point and are exposed to the tip place of outside and platinum filament microelectrode lower end end toper under glass tube, described tungsten microelectrode lower end is oxidized to WO
3, form W/ WO
3microelectrode, the upper end of platinum filament microelectrode and tungsten microelectrode is electrically connected with a wire respectively.
The diameter of preferred described platinum filament microelectrode is 10~50 μ m, and the diameter of tungsten microelectrode is 10~50 μ m, and the tip diameter of platinum filament microelectrode and tungsten microelectrode lower end is 0.1~1.0 μ m.Further improve microprobe performance, make tungsten microelectrode lower end W/WO
3electrode has good stability, reversibility, reappearance and time-response fast.
Preferred described platinum filament microelectrode 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 μ m, and the lower end of tungsten microelectrode is 15~35 μ m higher than the lower end of platinum filament microelectrode.Further improve microprobe performance, improve detection accuracy, the spacing that platinum filament microelectrode and tungsten microelectrode are rationally set can better compensate corrosion system potential change, and to pH, measurement causes error.
The upper end of preferred described platinum filament microelectrode and tungsten microelectrode is connected with a copper conductor respectively by conducting resinl.Facilitate the upper end of platinum filament microelectrode and tungsten microelectrode to be connected with external unit, guarantee reliability of electrical connection.
Further improve, the bottom drawn undergauge of described glass tube becomes kapillary, and the wedge angle of glass tube lower end taper axial section is 30 °~60 °.Further facilitate the use of probe.
Further improve, described glass tube outside is also overlapped a stainless-steel tube.Both microprobe was played a protective role, and also can in detection, play shielding action, further improved the accuracy detecting.
The preparation method of above-mentioned microprobe is as follows: comprise the following steps:
(1) intercept respectively diameter 10~50 μ m, platinum filament and diameter 10~50 μ m of long 3 cm, the tungsten filament of long 3cm;
(2) choose the glass tube with two endoporus, glass tube bottom utilizes glass tube tensilometer stretching undergauge to become kapillary;
(3) platinum filament and tungsten filament are respectively charged in two endoporus of glass tube, and in the bottom packing ring epoxy resins of two endoporus of glass tube to fix platinum filament and tungsten filament, platinum filament and tungsten filament are parallel to each other and the spacing of controlling platinum filament and tungsten filament is 30~50 μ m;
(4) after epoxy resin solidifies completely, by the glass instrument of polishing, polished in the lower end of glass tube, taper is worn into in the lower end of glass tube, the wedge angle of controlling glass tube lower end taper axial section is 30 °~60 °, platinum filament microelectrode and tungsten microelectrode lower end are tapered off to a point be exposed to the tip place of outside and platinum filament microelectrode lower end end toper under glass tube, the tip diameter of controlling platinum filament and tungsten filament lower end is 0.1~1.0 μ m, the tip height of platinum filament and tungsten filament lower end is poor is 15~35 μ m, and the lower end of tungsten filament is 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) be oxidized being exposed to outside tungsten filament tip, form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3;
(7) microprobe preparing is soaked and hangs over 2 mol/L H
2sO
4in carry out 1~4 week aging, make WO
xrete is all converted into WO
3, wherein X=1~3, make the most advanced and sophisticated complete formation W/ WO of tungsten filament
3microelectrode.
Further, before described platinum filament and tungsten filament are packing two endoporus of glass tube into, need with acetone, absolute ethyl alcohol ultrasonic cleaning and dry; Described glass tube needs the 30%H through 1:4 before use
2o
2clean and dry with concentrated sulphuric acid mixed liquor.Guarantee the preparation quality of microprobe.
In preferred described step (6), the method for oxidation at tungsten filament tip is electrochemical cyclic voltammetry, at the H of 2mol/L
2sO
4in solution, taking tungsten filament as working electrode, platinum filament is to electrode, and choosing saturated calomel electrode is contrast electrode, and gated sweep potential range is 1.0~2.0V, and scan round number of times is 50~80 circles, and sweep velocity is 20~50 mV/s; Thereby form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3.Employing electrochemical cyclic voltammetry has the following advantages: the one, and equipment is simple, easy to operate, and conditional parameter is accurately controlled; The 2nd, prepared oxidation film densification, combination are firm; The 3rd, can be at the standby oxidation film to hydrogen ion sensitivity of the surperficial positioning of complex contour.And the parameter control through optimizing is more convenient at the fine and close WO of tungsten filament tip end surface formation one deck
xrete.
Further, said method is also included in a stainless-steel tube in the outer cover of the microprobe glass tube preparing.
The present invention is because the tip portion in tungsten microelectrode lower end forms W/ WO
3microelectrode, when temperature-resistant, WO
3can there is reversible reaction, W/WO along with pH in solution changes
3the current potential of electrode is also along with WO
3the difference of content and change W/WO
3electrode potential depends on H in medium
+activity.Therefore, when passing through scanning survey metal surface diverse location W/WO
3the Potential distribution of microprobe, the pH value that can indirectly obtain metal/solution interface distributes.
On the other hand, in scanning survey process, the tip of microprobe and sample surfaces distance are basic keeps constant, not only play the detection of tunnel current, distance effect with accurate gated sweep probe tip and sample surfaces near the platinum filament microelectrode of sample surfaces, in addition platinum filament microelectrode also plays the used of contrast electrode in measuring process, with W/WO
3microelectrode forms electrode system, by measuring the potential difference (PD) at bipolar electrode tip, can obtain sample two dimension pH value distribution plan.Platinum filament microelectrode can responsively detect tunnel current simultaneously, and can measure sample surfaces structure and morphology image is STM image.In fact platinum filament microelectrode has triple functions: (a) can responsive tunnel current, and accuracy controlling probe tip and sample surfaces distance; (b) in site measurement surface STM image; (c) as W/WO
3the reference electrode of microelectrode, accurately measures surperficial microcell pH value Two dimensional Distribution.
Therefore, the present invention can measure metal surface STM image simultaneously and pH value distributes, and resolution and detection efficiency are high.
Brief description of the drawings
Fig. 1 is axial cut-open view of the present invention;
Fig. 2 is that the present invention is applied to the auxiliary scanning microelectrode measuring system principle schematic of STM;
Fig. 3 is that the present invention measures R235 carbon steel at pH=10.6, the gray scale equipotential diagram that the surface pH value in 0.01M NaCl solution distributes;
Fig. 4 is that the present invention measures R235 carbon steel at pH=10.6, the 3 D stereo potential image that the surface pH value in 0.01M NaCl solution distributes;
Fig. 5 is the STM figure that the present invention measures R235 carbon steel sample surfaces.
Embodiment
Below in conjunction with accompanying drawing and concrete embodiment, the present invention is described in further detail.
Shown in Fig. 1, a kind of with the compound scanning microprobe of bipolar electrode, it is characterized in that: comprise a platinum filament microelectrode 1, a tungsten microelectrode 2, one with two endoporus 31, 32 glass tube 3, the bottom drawn undergauge of described glass tube 3 becomes kapillary, platinum filament microelectrode 1 and tungsten microelectrode 2 are contained in respectively two endoporus 31 of glass tube 3, in 32, be filled with epoxy resin 4 in the bottom of 3 two endoporus of glass tube to fix platinum filament microelectrode 1 and tungsten microelectrode 2, after epoxy resin 4 solidifies, taper is worn in the lower end of described glass tube 3, platinum filament microelectrode 1 and tungsten microelectrode 2 lower ends taper off to a point and are exposed to outside and the platinum filament microelectrode 1 lower end tip place in 3 times end topers of glass tube, described tungsten microelectrode 2 lower ends are oxidized to WO
3, form W/ WO
3microelectrode, the upper end of platinum filament microelectrode 1 and tungsten microelectrode 2 is electrically connected with a copper conductor 6 respectively by conducting resinl 5.
The diameter of preferred described platinum filament microelectrode 1 is 10~50 μ m, and the diameter of tungsten microelectrode 2 is 10~50 μ m, and the tip diameter of platinum filament microelectrode 1 and tungsten microelectrode 2 lower ends is 0.1~1.0 μ m.
Preferred described platinum filament microelectrode 1 and tungsten microelectrode 2 are set in parallel in two endoporus 31,32 of glass tube 3, preferably the spacing of platinum filament microelectrode 1 and tungsten microelectrode 2 is 30~50 μ m, and the lower end of tungsten microelectrode 2 is 15~35 μ m higher than the lower end of platinum filament microelectrode 1.
The wedge angle of preferred glass pipe 3 lower end taper axial sections is 30 °~60 °.
Described glass tube 3 outsides are also overlapped a stainless-steel tube 7.
The preparation method of above-mentioned microprobe is as follows:
(1) intercept respectively diameter 10~50 μ m, platinum filament (content >=99.9 % of Pt) and diameter 10~50 μ m of long 3 cm, the tungsten filament (content >=99.9 % of W) of long 3cm, adopts acetone, absolute ethyl alcohol ultrasonic cleaning and dries;
(2) choose the glass tube with two endoporus, glass tube bottom utilizes glass tube tensilometer stretching undergauge to become kapillary, with the 30%H of 1:4
2o
2clean and dry with concentrated sulphuric acid mixed liquor;
(3) platinum filament and tungsten filament are respectively charged in two endoporus of glass tube, and in the bottom packing ring epoxy resins of two endoporus of glass tube to fix platinum filament and tungsten filament, platinum filament and tungsten filament are parallel to each other and the spacing of controlling platinum filament and tungsten filament is 30~50 μ m;
(4) after epoxy resin solidifies completely, by the glass instrument of polishing, polished in the lower end of glass tube, taper is worn into in the lower end of glass tube, the wedge angle of controlling glass tube lower end taper axial section is 30 °~60 °, platinum filament microelectrode and tungsten microelectrode lower end are tapered off to a point be exposed to the tip place of outside and platinum filament microelectrode lower end end toper under glass tube, the tip diameter of controlling platinum filament and tungsten filament lower end is 0.1~1.0 μ m, the tip height of platinum filament and tungsten filament lower end is poor is 15~35 μ m, and the lower end of tungsten filament is 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) be oxidized being exposed to outside tungsten filament tip, form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3; Concrete method for oxidation is electrochemical cyclic voltammetry, at the H of 2mol/L
2sO
4in solution, taking tungsten filament as working electrode, platinum filament is to electrode, and choosing saturated calomel electrode is contrast electrode, and gated sweep potential range is 1.0~2.0V, and scan round number of times is 50~80 circles, and sweep velocity is 20~50 mV/s; Thereby form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3;
(7) microprobe preparing is soaked and hangs over 2 mol/L H
2sO
4in carry out 1~4 week aging, make WO
xrete is all converted into WO
3, wherein X=1~3, make the most advanced and sophisticated complete formation W/ WO of tungsten filament
3microelectrode;
(8) stainless-steel tube in the outer cover of the microprobe glass tube preparing.
Fig. 2 is that the present invention is applied to the auxiliary scanning microelectrode measuring system principle schematic of STM, and it comprises that detected sample 9, computing machine 10, scanning microprobe 11, the three-dimensional piezoelectric micromotor scanner 12 of X-Y-Z, stepper motor drive the advance signal conversion/amplifying circuit 15 of X-Y two-dimentional machinery scanner 13, advance signal conversion/amplification and feedback circuit 14, micro-potential signals.
Detected sample 9 is selected R235 carbon steel, and use silicon carbide paper is from coarse to fine polishes to 2000# for sample 9, then is polished to minute surface with the alumina powder of 1 μ m and 0.3 μ m respectively, by ethanol and washed with de-ionized water, natural drying.Then measure sample 9 at pH=10.6, surface pH value Two dimensional Distribution image in the NaCl solution of 0.01M.When measurement, microprobe 11 auto-feeding sample 9 surfaces, first detect tunnel current signal (now the tip of platinum filament microelectrode and sample 9 surface distances only have nanoscale) by the tip of platinum filament microelectrode, are automatically controlled and stop inserting needle by feedback circuit; Then by computer program, microprobe 11 is upwards raised to 5 μ m, after adding test solution, fall again microprobe 11, carry out the scanning survey that surperficial microcell pH value distributes, scan area is 4mm x 4mm, surface p H two-dimensional distribution measurement result is shown in Fig. 3, Fig. 4, Fig. 3 is gray scale equipotential diagram, Fig. 4 is corresponding 3 D stereo potential image, result proves, compound scanning microprobe of the present invention can detect the two-dimentional distributed image of metal sample surface microcell pH value sensitively, measures resolution high; Simultaneously all right in site measurement sample surfaces STM feature image, STM is illustrated in Fig. 5, and result shows that its sharpness is also better.
Below be only preferred embodiment of the present invention, the change that those skilled in the art does to be equal to by claim all falls into the protection domain of this case.
Claims (10)
1. one kind with the compound scanning microprobe of bipolar electrode, it is characterized in that: comprise a platinum filament microelectrode, a tungsten microelectrode, a glass tube with two endoporus, platinum filament microelectrode and tungsten microelectrode are contained in respectively in two endoporus of glass tube, at least be filled with epoxy resin to fix platinum filament microelectrode and tungsten microelectrode in the bottom of two endoporus of glass tube, after epoxy resin cure, taper is worn in the lower end of described glass tube, platinum filament microelectrode and tungsten microelectrode lower end taper off to a point and are exposed to the tip place of outside and platinum filament microelectrode lower end end toper under glass tube, described tungsten microelectrode lower end is oxidized to WO
3, form W/ WO
3microelectrode, the upper end of platinum filament microelectrode and tungsten microelectrode is electrically connected with a wire respectively.
2. one according to claim 1 is with the compound scanning microprobe of bipolar electrode, it is characterized in that: the diameter of described platinum filament microelectrode is 10~50 μ m, the diameter of tungsten microelectrode is 10~50 μ m, and the tip diameter of platinum filament microelectrode and tungsten microelectrode lower end is 0.1~1.0 μ m.
3. one according to claim 1 is with the compound scanning microprobe of bipolar electrode, it is characterized in that: described platinum filament microelectrode and tungsten microelectrode are set in parallel in two endoporus of glass tube, the spacing of platinum filament microelectrode and tungsten microelectrode is 30~50 μ m, and the lower end of tungsten microelectrode is 15~35 μ m higher than the lower end of platinum filament microelectrode.
4. one according to claim 1, with the compound scanning microprobe of bipolar electrode, is characterized in that: the upper end of described platinum filament microelectrode and tungsten microelectrode is connected with a copper conductor respectively by conducting resinl.
5. one according to claim 1, with the compound scanning microprobe of bipolar electrode, is characterized in that: the bottom drawn undergauge of described glass tube becomes kapillary, and the wedge angle of glass tube lower end taper axial section is 30 °~60 °.
According to the one described in claim 1 to 5 any one with the compound scanning microprobe of bipolar electrode, it is characterized in that: described glass tube outside is also overlapped a stainless-steel tube.
Described in claim 1 to 5 any one with a preparation method for the compound scanning microprobe of bipolar electrode, it is characterized in that: comprise the following steps:
(1) intercept respectively diameter 10~50 μ m, platinum filament and diameter 10~50 μ m of long 3 cm, the tungsten filament of long 3cm;
(2) choose the glass tube with two endoporus, glass tube bottom utilizes glass tube tensilometer stretching undergauge to become kapillary;
(3) platinum filament and tungsten filament are respectively charged in two endoporus of glass tube, and in the bottom packing ring epoxy resins of two endoporus of glass tube to fix platinum filament and tungsten filament, platinum filament and tungsten filament are parallel to each other and the spacing of controlling platinum filament and tungsten filament is 30~50 μ m;
(4) after epoxy resin solidifies completely, by the glass instrument of polishing, polished in the lower end of glass tube, taper is worn into in the lower end of glass tube, the wedge angle of controlling glass tube lower end taper axial section is 30 °~60 °, platinum filament microelectrode and tungsten microelectrode lower end are tapered off to a point be exposed to the tip place of outside and platinum filament microelectrode lower end end toper under glass tube, the tip diameter of controlling platinum filament and tungsten filament lower end is 0.1~1.0 μ m, the tip height of platinum filament and tungsten filament lower end is poor is 15~35 μ m, and the lower end of tungsten filament is 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) be oxidized being exposed to outside tungsten filament tip, form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3;
(7) microprobe preparing is soaked and hangs over 2 mol/L H
2sO
4in carry out 1~4 week aging, make WO
xrete is all converted into WO
3, wherein X=1~3, make the most advanced and sophisticated complete formation W/ WO of tungsten filament
3microelectrode.
8. preparation method according to claim 7, is characterized in that: described platinum filament and tungsten filament need with acetone, absolute ethyl alcohol ultrasonic cleaning and dry packing into before two endoporus of glass tube; Described glass tube needs the 30%H through 1:4 before use
2o
2clean and dry with concentrated sulphuric acid mixed liquor.
9. preparation method according to claim 7, is characterized in that: in described step (6), the method for oxidation at tungsten filament tip is electrochemical cyclic voltammetry, at the H of 2mol/L
2sO
4in solution, taking tungsten filament as working electrode, platinum filament is to electrode, and choosing saturated calomel electrode is contrast electrode, and gated sweep potential range is 1.0~2.0V, and scan round number of times is 50~80 circles, and sweep velocity is 20~50 mV/s; Thereby form the fine and close WO of one deck in tungsten filament tip end surface
xrete, wherein X=1~3.
10. preparation method according to claim 7, is characterized in that: be also included in a stainless-steel tube in the outer cover of the microprobe glass tube preparing.
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Cited By (4)
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CN110373708A (en) * | 2019-07-31 | 2019-10-25 | 东南大学 | Adjustable concentration realizes that the nanometer pinpoint of needle point cone angle control prepares platform and method |
CN110462711A (en) * | 2017-03-22 | 2019-11-15 | 波士顿科学医学有限公司 | Electrified anatomical model |
CN111257596A (en) * | 2020-02-25 | 2020-06-09 | 西南交通大学 | Scanning probe microscope narrow and small experiment chamber environment atmosphere accurate control device |
CN114354707A (en) * | 2021-12-16 | 2022-04-15 | 中国石油大学(华东) | Preparation method of flexible platinum-based electrochemical probe |
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CN110462711A (en) * | 2017-03-22 | 2019-11-15 | 波士顿科学医学有限公司 | Electrified anatomical model |
CN110373708A (en) * | 2019-07-31 | 2019-10-25 | 东南大学 | Adjustable concentration realizes that the nanometer pinpoint of needle point cone angle control prepares platform and method |
CN110373708B (en) * | 2019-07-31 | 2021-04-30 | 东南大学 | Nano needle tip preparation platform and method for adjusting concentration to realize needle tip cone angle control |
CN111257596A (en) * | 2020-02-25 | 2020-06-09 | 西南交通大学 | Scanning probe microscope narrow and small experiment chamber environment atmosphere accurate control device |
CN114354707A (en) * | 2021-12-16 | 2022-04-15 | 中国石油大学(华东) | Preparation method of flexible platinum-based electrochemical probe |
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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