CN104483512A - Scanning tunneling microscope needle point corrosion instrument - Google Patents
Scanning tunneling microscope needle point corrosion instrument Download PDFInfo
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- CN104483512A CN104483512A CN201410836854.3A CN201410836854A CN104483512A CN 104483512 A CN104483512 A CN 104483512A CN 201410836854 A CN201410836854 A CN 201410836854A CN 104483512 A CN104483512 A CN 104483512A
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Abstract
The invention discloses a scanning tunneling microscope needle point corrosion instrument which comprises a mechanical component, a working circuit and a control power source. The control power source comprises a control circuit and a control panel. The control circuit comprises a voltage regulating and stabilizing module, a voltage measuring module, a current measuring module, a threshold value setting module, a sampling comparison module and a voltage output module. A sampling resistor R2 adopted by the voltage regulating and stabilizing module is located at a high-potential position, and an LM319 type comparator is adopted by the sampling comparison module. Due to the facts that a sampling resistor in a control circuit of an original needle point corrosion instrument is moved away from a whole load voltage collecting system according to the design control circuit of the scanning tunneling microscope needle point corrosion instrument, and the sampling resistor is changed to be located at the high-potential position, real-time current can be precisely measured, constant-voltage output at the two ends of a load resistor is guaranteed, current is gradually reduced along with increasing of load resistance, single-parameter changing is easy to control and analyze, stability in the corrosion process is improved, and the manufacturing successful rate of needle points is improved.
Description
Technical field
The present invention relates to a kind of needle tip of scanning tunnel microscope producing device, particularly a kind of needle tip of scanning tunnel microscope corrosion tester.
Background technology
Scanning tunnel microscope (STM) is the study of surfaces instrument that a kind of resolution is very high, and it makes people first time in the real space, observe atom.In recent years, along with the development of Surface Science, be widely used, and became the research means of condensed state and surface physics laboratory indispensability gradually.As the parts that directly contact surperficial with research, needle point plays extremely important role in each ingredient of STM.For most STM experiment, conventional tip point material is tungsten W or platinoiridita Pt-Ir, and the quality of needle point directly has influence on the resolution of STM.
Because scanning probe microscopy is to the demand of high-quality needle point, a variety of method is used to probe manufacturing.Wherein, most convenient and economical be theoretical based on galvanic corrosion and development needle point manufacturing technology out.Electrochemical method corrosion needle point, can be divided into AC and DC to corrode two kinds of different approach, and its needle point profile obtained is similar to parabolic type and hyperbolic type.Comparatively speaking, the bubble that DC corrosion process produces only occurs at negative electrode, and the fluctuation that generally can not cause anode liquid level thus advantageously, is often used in the making of tungsten (W) needle point.A kind of technology the most frequently used in DC corrosion is exactly that direct current breaks the method that falls.In the method, needle point immerses among solution, and near liquid level, form thinner neck and final fracture, the first half of tungsten filament forms required needle point.The major defect of this method is, will continue reaction and cause needle point rust, therefore need the Circuits System designing a kind of auto-breaking to meet its requirement if can not cut off circuit timely.The corrosion potentials of the Circuits System designed by tradition needle point corrosion tester, pull-up resistor and corrosion current all will change, the uncertainty of multiple response parameter and lasting change can increase the difficulty of experiment control, cause the instability of experimental result, reduce the success ratio that needle point makes.
Summary of the invention
For solving the problems referred to above that prior art exists, the present invention will design one can overcome change in voltage in corrosion process, improves the needle tip of scanning tunnel microscope corrosion tester that needle point is made into power.
To achieve these goals, technical scheme of the present invention is as follows: a kind of needle tip of scanning tunnel microscope corrosion tester, comprises mechanical component, operating circuit and control power supply.
Described mechanical component comprises base, support, upper cover, top cover knob, copper sheathing A, threaded rod, pointer, lifting fixed block, anode electrode bar, fixed knob, electrode stiff end, three-jaw jig A, knob, three-jaw jig B, negative electrode bar, disk, electrode retaining collar, beaker and copper sheathing B.
Described base adopts screw to be connected and fixed with support, disk respectively, plays overall supporting role; Described upper cover and support adopt screw to be connected and fixed; Described threaded rod two ends respectively with copper sheathing A and copper sheathing B clearance fit, copper sheathing A and copper sheathing B is separately fixed on upper cover and base; Described top cover knob is marked with scale, adopts screw and threaded rod to be fastenedly connected; Described pointer is fixed by screws in and covers, and it coordinates the anglec of rotation of the scale determination top cover knob on top cover knob.Described electrode stiff end is fixed by screws on lifting fixed block, and be threaded engagement between fixed knob and electrode stiff end, anode electrode bar is fixed on electrode stiff end by fixed knob; Described three-jaw jig A and three-jaw jig B is fixed on anode electrode bar respectively by screw, and three-jaw jig A and three-jaw jig B is by tungsten filament vertical clamping; Described negative electrode bar adopts screw to be fixed on base, knob and negative electrode bar threaded engagement, rotates knob and is fixedly clamped by electrode retaining collar on negative electrode bar; Described disk adopts screw to be fixed on base, and the beaker filling etchant solution is placed among the circular hole of disk, and below liquid level of solution contained by the electrode retaining collar beaker that submerges.
Described operating circuit comprises anode electrode bar, electrode stiff end, three-jaw jig A, knob, three-jaw jig B, negative electrode bar, disk, electrode retaining collar and beaker.Electrode stiff end connects positive source by electric wire, and electric current is transmitted to the tungsten filament clamped by three-jaw jig A and three-jaw jig B by the anode electrode bar be connected with electrode stiff end; Described negative electrode bar connects power cathode, and is connected by screw with electrode retaining collar; Three-jaw jig A and the tungsten filament clamped by three-jaw jig B and electrode retaining collar to be co-located in the etchant solution that beaker contains but directly not to contact, and during energising, tungsten filament electrolytic reaction occurs in etchant solution makes circuit form loop.
Described control power supply comprises control circuit and control panel.Described control circuit comprises voltage-regulation voltage-stabilization module, voltage measurement module, current measurement module, threshold value setting module, sampling comparison module, differential comparison module and voltage output module, described voltage-regulation voltage-stabilization module is connected with voltage measurement module and current measurement module respectively, and described voltage measurement module is also connected with voltage output module; Described voltage output module by K switch 1B respectively with sampling comparison module and differential comparison model calling; Described sampling comparison module is connected with current measurement module after threshold value setting module, K switch 1C, and the other end of described differential comparison module is connected with current measurement module after K switch 1C.Described voltage-regulation voltage-stabilization module sampling resistor R2 used is positioned at noble potential place, and described sampling comparison module adopts LM319 type comparer.
Described voltage-regulation voltage-stabilization module exports 0 ~ 10v DC voltage by rheostat RT1, and output voltage connects load by P1 interface, i.e. the both positive and negative polarity of needle point corrosion tester.
Described voltage measurement module gathers load voltage, is then shown on control panel by the load voltage of reality by P2 interface external power supply inner integrated processing module.
Described current measurement module gathers the voltage at sampling resistor R2 two ends, is then obtained by the electric current of sampling resistor R2 and corrosion current by the inner integrated processing module of P3 interface external power supply and is presented on control panel.
Described control panel is one piece and is positioned at the touch-screen controlling centre position, outer casing of power supply front, control panel is provided with voltage sets voltage, current monitoring current, failure of current threshold value setting threshold, difference setting Differential, tip height adjustment monitoring TipAdj, mode of operation and switch display box.
Top cover knob of the present invention is marked with scale, adopts screw and threaded rod to be fastenedly connected, and during work, rotating cap knob can make the threaded rod linked together with it rotate, thus makes to be elevated with the lifting fixed block of threaded rod threaded engagement; Rotating cap knob makes threaded rod rotate, thus makes to move up and down with the lifting fixed block of threaded rod threaded engagement, thus can adjust tungsten filament immerse beaker contain the length of solution.TipAdj display box on touch operation panel before adjustment tungsten filament length, the hummer buzzing prompting of TipAdj power source internal when tungsten filament just contacts liquid level, observes scale on lid knob afterwards again to adjust the length of tungsten filament immersed in liquid level; After adjusting tungsten filament length, touch voltage setting voltage and failure of current threshold value setting threshold display box set corrosion potentials and cut off electric current; In corrosion process, current monitoring current display box can show the size variation of corrosion current in real time.
When the present invention works, the principle of work of each module is as follows:
Voltage-regulation voltage-stabilization module exports 0 ~ 10v DC voltage by rheostat RT1, and this magnitude of voltage is for presetting load voltage, and the present invention in use predeterminated voltage is generally set to 4 ~ 10v, and output voltage connects load by P1 interface, i.e. the both positive and negative polarity of needle point corrosion tester.Rheostat RT1 can be controlled by Voltage option on touch-screen and regulate default load voltage.
Voltage measurement module gathers load voltage, then by P2 interface external power supply inner integrated processing module then the load voltage of reality is shown as the value (touch-screen Voltage option regulates the function preset load voltage and course of reaction and show actual load voltage before having reaction concurrently) of touch-screen Voltage, the position changing sampling resistor R2 due to this circuit makes the load voltage in real reaction process very stable, be substantially equal to predeterminated voltage, so the value can seeing Voltage in course of reaction is only in some instantaneous fluctuation up and down had within 0.02v.
Current measurement module gathers the voltage at sampling resistor R2 two ends, by then being obtained by the electric current of R2 and corrosion current by the inner integrated processing module of P3 interface external power supply and being shown as the value of touch-screen Current, thus achieves the real-time display of corrosion current.
Threshold value setting module and sampling comparison module: when corrosion tester mode of operation being adjusted to Thr. pattern by Touch Screen, in circuit, threshold value setting module and sampling comparison module are linked in circuit, control threshold value setting module rheostat RT2 change the size preset and cut off electric current by regulating the value of Threshold option on touch-screen; Then sampling comparison module collection is cut off electric current and is compared with presetting by comparer IC2B by the size of the electric current of sampling resistor R2 and actual corrosion current, if actual corrosion current is less than to preset cut off electric current, then the triode Q1 of P1 interface series connection closes, load cut off from circuit, namely needle point corrosion tester quits work.
Differential comparison module: when corrosion tester mode of operation being adjusted to Diff. pattern by touch-screen, sample in circuit comparison module and threshold value setting module cut off from circuit, and in difference block place in circuit.By regulating the value of Differential on touch-screen to control the size that rheostat RT3 in differential comparison module changes electric capacity C5 right-hand member preset voltage value, thus change the sensitivity of differential comparison module; When the moment that needle point corrosion terminates and tungsten filament break to fall moment, corrosion current has a larger saltus step, and differential comparison module can judge the size of corrosion current saltus step, when the size of saltus step is greater than certain value time, then the triode Q1 of P1 interface series connection closes, load cut off from circuit, namely needle point corrosion tester quits work.
After setting corrosion parameter, touch " ON " on touch-screen, corrosion tester is started working, and " ON " becomes " OFF ", and corrosion tester work can stop by touch-control again.
Compared with prior art, the present invention has following improvement effect:
1, designed by the present invention, the sampling resistor in needle point corrosion tester control circuit is in the past removed by control circuit from whole load voltage acquisition system, change into the noble potential place as shown in R2 in Fig. 2, accurately can measure real-time current by such mode, the constant voltage at proof load resistance two ends exports simultaneously.The designed modular method of control circuit gives the concrete function of Circuits System each several part and the program of work.Actual corrosion potentials is constant, and electric current reduces gradually along with the increase of pull-up resistor, and the change of so single parameter easily controls and analyzes, and enhances the stability of corrosion process, thus improve the success ratio of needle point making.
2, the design of contact panel of the present invention, shows the parameters such as corrosion potentials, circuital current, cut-off current, tip height adjustment in real time, easy to operate.
3, control circuit of the present invention adopts LM319 type comparer, is swift in response, can judges within 200ns, improve the speed of circuit judges and action.
Accompanying drawing explanation
The present invention has 3, accompanying drawing, wherein:
Fig. 1 is mechanical part general assembly drawing of the present invention.
Fig. 2 is control circuit schematic diagram of the present invention.
Fig. 3 is guidance panel schematic diagram of the present invention.
In figure: 1, base; 2, support; 3, upper cover; 4, top cover knob; 5, copper sheathing; 6, threaded rod; 7, pointer; 8, fixed block is elevated; 9, anode electrode bar; 10, fixed knob; 11, electrode stiff end; 12, three-jaw jig A; 13, knob; 14, three-jaw jig B; 15, negative electrode bar; 16, disk; 17, electrode retaining collar; 18, beaker; 19, copper sheathing B.
Embodiment
For making the object of embodiments of the invention, technical scheme and advantage clearly, below in conjunction with the accompanying drawing in the embodiment of the present invention, clear complete description is carried out to the technical scheme in the embodiment of the present invention.
As Figure 1-3, a kind of needle tip of scanning tunnel microscope corrosion tester, comprises mechanical component, operating circuit and control power supply.
Described mechanical component comprises base 1, support 2, upper cover 3, top cover knob 4, copper sheathing A5, threaded rod 6, pointer 7, lifting fixed block 8, anode electrode bar 9, fixed knob 10, electrode stiff end 11, three-jaw jig A12, knob 13, three-jaw jig B14, negative electrode bar 15, disk 16, electrode retaining collar 17, beaker 18 and copper sheathing B19.
Described base 1 adopts screw to be connected and fixed with support 2, disk 16 respectively, plays overall supporting role; Described upper cover 3 adopts screw to be connected and fixed with support 2; Described threaded rod 6 two ends respectively with copper sheathing A5 and copper sheathing B19 clearance fit, copper sheathing A5 and copper sheathing B19 is separately fixed on upper cover 3 and base 1; Described top cover knob 4 is marked with scale, adopts screw and threaded rod 6 to be fastenedly connected; Described pointer 7 is fixed by screws on upper cover 3, and it coordinates the anglec of rotation of the scale determination top cover knob 4 on top cover knob 4.Described electrode stiff end 11 is fixed by screws on lifting fixed block 8, and be threaded engagement between fixed knob 10 and electrode stiff end 11, anode electrode bar 9 is fixed on electrode stiff end 11 by fixed knob 10; Described three-jaw jig A12 and three-jaw jig B14 is fixed on anode electrode bar 9 respectively by screw, and three-jaw jig A12 and three-jaw jig B14 is by tungsten filament vertical clamping; Described negative electrode bar 15 adopts screw to be fixed on base 1, knob 13 and negative electrode bar 15 threaded engagement, rotates knob 13 and is fixedly clamped on negative electrode bar 15 by electrode retaining collar 17; Described disk 16 adopts screw to be fixed on base 1, and the beaker 18 filling etchant solution is placed among the circular hole of disk 16, electrode retaining collar 17 submerge beaker 18 contain below liquid level of solution.
Described operating circuit comprises anode electrode bar 9, electrode stiff end 11, three-jaw jig A12, knob 13, three-jaw jig B14, negative electrode bar 15, disk 16, electrode retaining collar 17 and beaker 18.Electrode stiff end 11 connects positive source by electric wire, and electric current is transmitted to the tungsten filament clamped by three-jaw jig A12 and three-jaw jig B14 by the anode electrode bar 9 be connected with electrode stiff end 11; Described negative electrode bar 15 connects power cathode, and is connected by screw with electrode retaining collar 17; Three-jaw jig A12 and the tungsten filament clamped by three-jaw jig B14 and electrode retaining collar 17 to be co-located in the etchant solution that beaker 18 contains but directly not to contact, and during energising, tungsten filament electrolytic reaction occurs in etchant solution makes circuit form loop.
Described control power supply comprises control circuit and control panel.Described control circuit comprises voltage-regulation voltage-stabilization module, voltage measurement module, current measurement module, threshold value setting module, sampling comparison module, differential comparison module and voltage output module, described voltage-regulation voltage-stabilization module is connected with voltage measurement module and current measurement module respectively, and described voltage measurement module is also connected with voltage output module; Described voltage output module by K switch 1B respectively with sampling comparison module and differential comparison model calling; Described sampling comparison module is connected with current measurement module after threshold value setting module, K switch 1C, and the other end of described differential comparison module is connected with current measurement module after K switch 1C.Described voltage-regulation voltage-stabilization module sampling resistor R2 used is positioned at noble potential place, and described sampling comparison module adopts LM319 type comparer.
Described voltage-regulation voltage-stabilization module exports 0 ~ 10v DC voltage by rheostat RT1, and output voltage connects load by P1 interface, i.e. the both positive and negative polarity of needle point corrosion tester.
Described voltage measurement module gathers load voltage, is then shown on control panel by the load voltage of reality by P2 interface external power supply inner integrated processing module.
Described current measurement module gathers the voltage at sampling resistor R2 two ends, is then obtained by the electric current of sampling resistor R2 and corrosion current by the inner integrated processing module of P3 interface external power supply and is presented on control panel.
Described control panel is one piece and is positioned at the touch-screen controlling centre position, outer casing of power supply front, control panel is provided with voltage sets voltage, current monitoring current, failure of current threshold value setting threshold, difference setting Differential, tip height adjustment monitoring TipAdj, mode of operation and switch display box.
Following electrolytic reaction is there is in tungsten filament of the present invention after immersing and switching on power among etchant solution:
Anode: W+8OH
-→ WO
4 2-+ 4H
2o+6e
-
Negative electrode: 6H
2o+6e
-→ 3H
2+ 6OH
-
Overall reaction: W+2OH
-+ 2H
2o → WO
4 2-+ 3H
2
Tungsten filament forms thinner neck and final fracture because generation electrolytic reaction is consumed near liquid level, and the first half of tungsten filament forms required needle point.
Claims (1)
1. a needle tip of scanning tunnel microscope corrosion tester, is characterized in that: comprise mechanical component, operating circuit and control power supply;
Described mechanical component comprises base (1), support (2), upper cover (3), top cover knob (4), copper sheathing A (5), threaded rod (6), pointer (7), lifting fixed block (8), anode electrode bar (9), fixed knob (10), electrode stiff end (11), three-jaw jig A (12), knob (13), three-jaw jig B (14), negative electrode bar (15), disk (16), electrode retaining collar (17), beaker (18) and copper sheathing B (19),
Described base (1) adopts screw to be connected and fixed with support (2), disk (16) respectively, plays overall supporting role; Described upper cover (3) and support (2) adopt screw to be connected and fixed; Described threaded rod (6) two ends respectively with copper sheathing A (5) and copper sheathing B (19) clearance fit, copper sheathing A (5) and copper sheathing B (19) is separately fixed on upper cover (3) and base (1); Described top cover knob (4) is marked with scale, adopts screw and threaded rod (6) to be fastenedly connected; Described pointer (7) is fixed by screws on upper cover (3), and it coordinates the anglec of rotation of scale determination top cover knob (4) on top cover knob (4); Described electrode stiff end (11) is fixed by screws in lifting fixed block (8), be threaded engagement between fixed knob (10) and electrode stiff end (11), anode electrode bar (9) is fixed on electrode stiff end (11) by fixed knob (10); Described three-jaw jig A (12) and three-jaw jig B (14) are fixed on anode electrode bar (9) respectively by screw, and three-jaw jig A (12) and three-jaw jig B (14) is by tungsten filament vertical clamping; Described negative electrode bar (15) adopts screw to be fixed on base (1), knob (13) and negative electrode bar (15) threaded engagement, rotate knob (13) and be fixedly clamped on negative electrode bar (15) by electrode retaining collar (17); Described disk (16) adopts screw to be fixed on base (1), the beaker (18) filling etchant solution is placed among the circular hole of disk (16), electrode retaining collar (17) submerge beaker (18) contain below liquid level of solution;
Described operating circuit comprises anode electrode bar (9), electrode stiff end (11), three-jaw jig A (12), knob (13), three-jaw jig B (14), negative electrode bar (15), disk (16), electrode retaining collar (17) and beaker (18); Electrode stiff end (11) connects positive source by electric wire, and electric current is transmitted to the tungsten filament clamped by three-jaw jig A (12) and three-jaw jig B (14) by the anode electrode bar (9) be connected with electrode stiff end (11); Described negative electrode bar (15) connects power cathode, and is connected by screw with electrode retaining collar (17); Three-jaw jig A (12) and the tungsten filament clamped by three-jaw jig B (14) and electrode retaining collar (17) to be co-located in the etchant solution that beaker (18) contains but directly not to contact, and during energising, tungsten filament electrolytic reaction occurs in etchant solution makes circuit form loop;
Described control power supply comprises control circuit and control panel.Described control circuit comprises voltage-regulation voltage-stabilization module, voltage measurement module, current measurement module, threshold value setting module, sampling comparison module, differential comparison module and voltage output module, described voltage-regulation voltage-stabilization module is connected with voltage measurement module and current measurement module respectively, and described voltage measurement module is also connected with voltage output module; Described voltage output module by K switch 1B respectively with sampling comparison module and differential comparison model calling; Described sampling comparison module is connected with current measurement module after threshold value setting module, K switch 1C, and the other end of described differential comparison module is connected with current measurement module after K switch 1C; Described voltage-regulation voltage-stabilization module sampling resistor R2 used is positioned at noble potential place, and described sampling comparison module adopts LM319 type comparer;
Described voltage-regulation voltage-stabilization module exports 0 ~ 10v DC voltage by rheostat RT1, and output voltage connects load by P1 interface, i.e. the both positive and negative polarity of needle point corrosion tester;
Described voltage measurement module gathers load voltage, is then shown on control panel by the inner integrated processing module of P2 interface external power supply by the load voltage of reality;
Described current measurement module gathers the voltage at sampling resistor R2 two ends, is then obtained by the electric current of sampling resistor R2 and corrosion current by the inner integrated processing module of P3 interface external power supply and is presented on control panel;
Described control panel is one piece and is positioned at the touch-screen controlling centre position, outer casing of power supply front, control panel is provided with voltage sets voltage, current monitoring current, failure of current threshold value setting threshold, difference setting Differential, tip height adjustment monitoring TipAdj, mode of operation and switch display box.
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| CN201410836854.3A CN104483512B (en) | 2014-12-29 | 2014-12-29 | Scanning tunneling microscope needle point corrosion instrument |
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|---|---|---|---|
| CN201410836854.3A CN104483512B (en) | 2014-12-29 | 2014-12-29 | Scanning tunneling microscope needle point corrosion instrument |
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| CN106093473A (en) * | 2016-07-27 | 2016-11-09 | 大连交通大学 | A kind of Pt Ir needle point corrosion device and method of work thereof |
| CN106757297A (en) * | 2017-02-17 | 2017-05-31 | 科斗（苏州）脑机科技有限公司 | A kind of Novel electric polar filament electrolytic cell |
| CN109490580A (en) * | 2018-11-09 | 2019-03-19 | 昆明理工大学 | A kind of annealing device of needle tip of scanning tunnel microscope |
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| CN104483512B (en) | 2017-02-01 |
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