CN101118789A - Method for manufacturing platinum-iridium needlepoint and device thereof - Google Patents
Method for manufacturing platinum-iridium needlepoint and device thereof Download PDFInfo
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- CN101118789A CN101118789A CNA2007100093114A CN200710009311A CN101118789A CN 101118789 A CN101118789 A CN 101118789A CN A2007100093114 A CNA2007100093114 A CN A2007100093114A CN 200710009311 A CN200710009311 A CN 200710009311A CN 101118789 A CN101118789 A CN 101118789A
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Abstract
The present invention provides a Pt-Ir needle point production method and a device of the Pt-Ir needle point, relates to a scanning probe, and provides a method that can produce Pt-Ir needle points fast and safely. The present invention is provided with an alternating current voltage signal producing circuit, a power amplifier circuit, a corrosive current sensing circuit, an alternating current signal amplifier circuit, an alternating effective vale converter circuit, a direct current signal amplifier circuit, a data acquisition circuit, an actuator circuit and a corrosive electrolytic cell. A Pt-Ir thread set gets burnt on hydrogen flames and then anneals, then one end of the Pt-Ir thread is sealed, and the other end is sheathed onto the needle header and connected with a working electrode; two spectral pure carbon sticks, being taken as auxiliary electrodes, are parallel to the Pt-Ir thread and are vertically inserted into the corrosive solution, taking the Pt-Ir thread as the asymmetrical center; the sealed end is inserted into the corrosive solution and the depth of the exposed part in the corrosive solution is kept; The electric current in the crossover place between the exposed part of the Pt-Ir thread immersed in the corrosive solution and the sealed part is monitored and cut off; after further corrosion, a corrosion loop is cut off to control the length-width ratio of a needle point.
Description
Technical field
The present invention relates to a kind of scanning probe microscopy, especially relate to a kind of method and device thereof that can prepare scanning probe microscopy (SPM) platinum-iridium needle point fast and effectively.
Background technology
The probe of scanning probe microscopy is determining the performance of scanning probe microscopy to a great extent, the size of probe, shape and chemical constitution directly affect the quality of scanning probe microscopy image, the needle point tip is sharp-pointed more, shape is symmetrical more, and the quality of image and resolution are high more.At present, the material that is used to prepare the SPM needle point mainly contains tungsten filament (W), spun gold (Au) and platinoiridita silk (Pt-Ir) etc., and wherein tungsten tip is hard because of quality, can obtain full resolution pricture, but easily oxidized in air and solution; The acupuncture needle point is chemically comparatively stable, but quality is softer, is broken easily; And platinumiridio silk quality ground is harder, and resistance to corrosion is strong, has the potential window of broad in solution, has the advantage of tungsten tip and acupuncture needle point concurrently.Needle point preparation method relatively more commonly used in the laboratory has mechanical shearing method and electrochemical erosion method, and the most advanced and sophisticated pattern of the needle point that mechanical shearing method obtains is asymmetric, seals to the SPM needle point in the subsequent solution and brings difficulty; The equipment of electrochemical erosion method is simple, easy to operate, according to alive character, can be divided into the anodic etching method method and AC electrochemical etch again.Usually, the available the anodic etching method method of preparation of acupuncture needle point and tungsten tip makes the less and surperficial comparatively smooth needle point of radius-of-curvature easily.Yet the Pt-Ir material is because of its chemical stability height, and required corrosion voltage height, etching time are long, will use CN usually
-Complexing accelerate corrosion speed, it is all bigger no matter to adopt direct current still to be that the AC electrochemical etch prepares the difficulty of needle point, especially is difficult to control the needle point size and dimension.Therefore, a kind of method of making high quality P t-Ir needle point quickly and easily of development is very necessary.
The preparation method of tungsten tip comparative maturity (1, Shanghai Communications University. needle tip of scanning tunnel microscope is controlled the etching instrument automatically: China, 03116028.X[P] 2003-08-27; 2, Shanghai Communications University. scanning tunnel microscope prepares control circuit with the tungsten tip direct current: China, 02218157.1[P] 2003-04-16).Utilize this method can make the tungsten tip of radius-of-curvature for 10nm.But directly make the platinoiridita needle point with this method, not only the time of Zhi Zuoing elongated, and the needlepoint type looks that obtain are undesirable, can't be applied to the imaging of the micro-sight mirror of scan-type electrochemical.(I.H.Musselman and P.E.Russell such as Musselman, Platinum/Iridium Tips with Controlled Geometry for Scanning Tunneling Microscopy, J.Vac.Sci.Technol.1990, A, 8 (4): 3558) adopt two-step approach to prepare the platinum-iridium needle point: to obtain the bigger platinoiridita needle point of radius-of-curvature with electrochemical erosion method earlier, fast moving makes that needle point is more sharp-pointed, the surface is more smooth in the thin film corrosive agent then, and can obtain radius-of-curvature is the platinoiridita needle point of 50nm.The step of the method is various, and the instrument and equipment of using is more, makes trouble, is not suitable for the laboratory and uses.
Summary of the invention
The object of the present invention is to provide a kind of comparatively simply, can prepare the method for platinum-iridium needle point quickly and safely.
Another object of the present invention is to provide a kind of device for preparing platinum-iridium needle point.
Technical scheme of the present invention is to adopt AC electrochemical etch corrosion Pt-Ir needle point, and the terminal point by computing machine and control circuit control corrosion makes the needle point of preparation keep pattern preferably, and has higher success ratio and reappearance preferably.
The device of preparation platinum of the present invention-iridium needle point is provided with ac voltage signal generation circuit, power amplification circuit, corrosion current sample circuit, AC signal amplifying circuit, AC value change-over circuit, direct current signal amplifying circuit, data acquisition circuit, braking circuit and corrosion electrolytic cell.Ac voltage signal generation circuit input end connects the computing machine USB interface, ac voltage signal generation circuit output end connects the power amplification circuit input end, the power amplification circuit output terminal connects braking circuit input end and corrosion current sample circuit input end respectively, braking circuit output terminal and corrosion current sample circuit current signal output end connect the corrosion electrolytic cell respectively, the braking circuit signal input end connects the computing machine USB interface, corrosion current sample circuit voltage output end connects the AC signal input amplifier, the AC signal amplification circuit output end connects AC value change-over circuit input end, AC value change-over circuit output termination direct current signal input amplifier, the direct current signal amplification circuit output end connects the data acquisition circuit input end, data acquisition circuit output termination computing machine USB interface.
The preparation method of platinum of the present invention-iridium needle point may further comprise the steps:
1) get one section Pt-Ir silk,, the one end insulated with polymethylstyrene seal through after the hydrogen flame annealing, but the other end be enclosed within on the syringe needle and be fixed on the iron stand of up-down adjustment, link to each other by the working electrode of lead with the device of preparation platinum-iridium needle point;
2) getting two spectroscopic pure carbon-points connects and is fixed on teflon with lead and cover as auxiliary electrode, link to each other with the auxiliary electrode of device of preparation platinum-iridium needle point, two spectroscopic pure carbon-points are parallel to the Pt-Ir silk and are that symcenter is vertically inserted in the etchant solution with the Pt-Ir silk;
3) regulate iron stand transfer arm above-below direction, the end of sealing of Pt-Ir silk is inserted in the etchant solution vertically downward and keeps the degree of depth of exposed part in etchant solution;
4) output voltage of regulating between working electrode and auxiliary electrode is 10～20V alternating voltage and passes through current acquisition circuit monitors corrosion current, seals the disconnection of part intersection until exposed part and insulation that the Pt-Ir silk is dipped in the etchant solution;
5) the top needle point that forms is continued to restart braking circuit behind the etch polishing and cut off corrosion loop, remove burr and control the length breadth ratio of needle point, obtain sharp-pointed platinum-iridium needle point.
In step 1), the length of Pt-Ir silk is preferably 8～25mm, and diameter is preferably 0.2～0.3mm.Be preferably 0.5mm with the insulate length of the end sealed of polymethylstyrene.
In step 2) in, be parallel to the Pt-Ir silk and be that symcenter is vertically inserted two spectroscopic pure carbon-points in the etchant solution and preferably kept distance 10～50mm with the Pt-Ir silk with the Pt-Ir silk.By mass percentage, etchant solution consist of saturated lime chloride 10%～30%, acetone 10%～30%, Yu Weishui, wherein lime chloride is mordant, its concentration affects corrosion speed, the effect of acetone are that the fining air bubbles that corrosion is produced also spreads to auxiliary electrode equably, and the needle surface of preparation is comparatively smooth.
In step 3), with the Pt-Ir silk to seal that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution be 0.5～1mm.Regulate the degree of depth of Pt-Ir silk, can finely tune corrosion current, the pattern of control corrosion speed and needle point at etchant solution.
In step 4), can pass through the Control Software of the device of preparation platinum-iridium needle point, the output voltage of regulating between working electrode and auxiliary electrode is 10～20V alternating voltage and passes through current acquisition circuit monitors corrosion current; In corrosion process, the current ratio that flows through corrosion loop is more steady, seals the moment that the part intersection disconnects, needle point forms, corrosion current bust until exposed part and insulation that the Pt-Ir silk is dipped in the corrosive liquid; After computing machine carried out the formation and definite terminal point of differential calculation judgement needle point to corrosion current, starting the braking circuit action also can be in 1ms internal cutting off corrosion loop.
In step 5), the time of described continuation etch polishing is preferably 10～80ms.The time of time-delay etch polishing can be done meticulous adjustment, to be fit to the SPM imaging of different demands.
The present invention has that the preparation method is simple, easy to operate, preparation cost is cheap, yield rate is high, high repeatability and other advantages, and it is minimum for 10nm, length breadth ratio are 0.7～5 Pt-Ir needle point to make the front end radius-of-curvature, can be applicable to STM and SECM imaging.
Description of drawings
Fig. 1 is the block diagram of the preparation platinum-iridium needle tip device of the embodiment of the invention.
Fig. 2 is the structural representation of the corrosion electrolytic cell among Fig. 1.
Fig. 3 is the theory of constitution figure of the control circuit of the embodiment of the invention.
Embodiment
Referring to Fig. 1, preparation platinum of the present invention-iridium needle tip device is provided with computing machine 1, ac voltage signal generation circuit 2, power amplification circuit 3, braking circuit 4, corrosion current sample circuit 5, AC signal amplifying circuit 6, AC value change-over circuit 7, direct current signal amplifying circuit 8, data acquisition circuit 9 and corrosion electrolytic cell 10.The USB interface of ac voltage signal generation circuit 2 input termination computing machines 1, ac voltage signal generation circuit 2 output termination power amplification circuits 3 input ends, power amplification circuit 3 output terminals connect braking circuit 4 input ends and corrosion current sample circuit 5 input ends respectively, braking circuit 4 output terminals and corrosion current sample circuit 5 current signal output ends connect corrosion electrolytic cell 10 respectively, braking circuit 4 signal input end connect the USB interface of computing machine 1, corrosion current sample circuit 5 voltage output ends connect AC signal amplifying circuit 6 input ends, AC signal amplifying circuit 6 output termination AC value change-over circuits 7 input ends, AC value change-over circuit 7 output termination direct current signal amplifying circuits 8 input ends, direct current signal amplifying circuit 8 output termination data acquisition circuits 9 input ends, the USB interface of data acquisition circuit 9 output termination computing machines 1.
Ac voltage signal generation circuit can produce 0～30V, and (10～500Hz) alternating voltage, exportable rated current are 300mA.String has braking circuit control terminal point in corrosion loop, the AC signal that the corrosion current sample circuit obtains is converted to d. c. voltage signal through the voltage amplification and the AC value change-over circuit of AC signal amplifying circuit, convert digital signal to through data acquisition circuit again, computing machine calculates judgement and cuts off corrosion loop through producing control signal after the suitable time-delay according to the current signal of gathering, and finishes the whole process that needle point is made.
Below provide and adopt the above-mentioned preparation platinum-device of iridium needle point to prepare the embodiment of platinum-iridium needle point.
Get the long 8mm that is, diameter is one section Pt-Ir silk of 0.2mm, after the hydrogen flame annealing, its length for insulating with polymethylstyrene, is sealed at the end of 0.5mm, but the other end is enclosed within on the syringe needle and is fixed on the iron stand of up-down adjustment, links to each other by the working electrode of lead with the device of preparation platinum-iridium needle point.
Getting two spectroscopic pure carbon-points connects and is fixed on teflon with lead and cover as auxiliary electrode, link to each other with the auxiliary electrode of device of preparation platinum-iridium needle point, two spectroscopic pure carbon-points are parallel to the Pt-Ir silk and are that symcenter is vertically inserted in the etchant solution with the Pt-Ir silk.Be parallel to the Pt-Ir silk and with the Pt-Ir silk be symcenter vertically insert two spectroscopic pure carbon-points in the etchant solution preferably keep with the Pt-Ir silk apart from 10mm.By mass percentage, etchant solution consist of saturated lime chloride 10%, acetone 30%, deionized water are 60%.
Regulate iron stand transfer arm above-below direction, the end of sealing of Pt-Ir silk is inserted in the etchant solution vertically downward and keeps the degree of depth of exposed part in etchant solution.With the Pt-Ir silk to seal that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution be 1mm.
The output voltage of regulating between working electrode and auxiliary electrode is 10～20V alternating voltage and passes through current acquisition circuit monitors corrosion current, seals the disconnection of part intersection until exposed part and insulation that the Pt-Ir silk is dipped in the etchant solution.Can pass through the Control Software of the device of preparation platinum-iridium needle point, regulate the output voltage between working electrode and auxiliary electrode.
The top needle point that forms is continued to restart braking circuit behind the etch polishing cut off corrosion loop, remove burr and control the length breadth ratio of needle point, obtain sharp-pointed platinum-iridium needle point.The time of continuing etch polishing is 10ms.
Get the long 25mm that is, diameter is one section Pt-Ir silk of 0.3mm, after the hydrogen flame annealing, its length for insulating with polymethylstyrene, is sealed at the end of 0.5mm, but the other end is enclosed within on the syringe needle and is fixed on the iron stand of up-down adjustment, links to each other by the working electrode of lead with the device of preparation platinum-iridium needle point.
Getting two spectroscopic pure carbon-points connects and is fixed on teflon with lead and cover as auxiliary electrode, link to each other with the auxiliary electrode of device of preparation platinum-iridium needle point, two spectroscopic pure carbon-points are parallel to the Pt-Ir silk and are that symcenter is vertically inserted in the etchant solution with the Pt-Ir silk.Be parallel to the Pt-Ir silk and with the Pt-Ir silk be symcenter vertically insert two spectroscopic pure carbon-points in the etchant solution preferably keep with the Pt-Ir silk apart from 50mm.By mass percentage, etchant solution consist of saturated lime chloride 30%, acetone 10%, deionized water are 60%.
Regulate iron stand transfer arm above-below direction, the end of sealing of Pt-Ir silk is inserted in the etchant solution vertically downward and keeps the degree of depth of exposed part in etchant solution.With the Pt-Ir silk to seal that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution be 0.5mm.
The output voltage of regulating between working electrode and auxiliary electrode is 10～20V alternating voltage and passes through current acquisition circuit monitors corrosion current, seals the disconnection of part intersection until exposed part and insulation that the Pt-Ir silk is dipped in the etchant solution.Can pass through the Control Software of the device of preparation platinum-iridium needle point, regulate the output voltage between working electrode and auxiliary electrode.
The top needle point that forms is continued to restart braking circuit behind the etch polishing cut off corrosion loop, remove burr and control the length breadth ratio of needle point, obtain sharp-pointed platinum-iridium needle point.The time of continuing etch polishing is 80ms.
To a segment length 15mm, the length of an end 0.5mm of the Pt-Ir silk of diameter 0.25mm insulate with polymethylstyrene and seals, and is 0.5mm with sealing that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution.The saturated lime chloride that consists of of etchant solution is 15mL, and water is 65mL, and acetone is 20mL.Corrode under the alternating voltage of 10V, 50Hz, this moment, corrosion current was 110mA, control terminal point time-delay 15ms, and obtaining the front end radius-of-curvature is that 15nm, length breadth ratio are 4 Pt-Ir needle point, is fit to be applied to the STM imaging.
Embodiment 4: to a segment length 15mm, diameter is that the length of an end 0.5mm of the Pt-Ir silk of 0.2mm insulate with polymethylstyrene and seals, and is 0.5mm with sealing that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution.The saturated lime chloride that consists of of etchant solution is 15mL, and water is 65mL, and acetone is 20mL; Corrode under the alternating voltage of 15V, 50Hz, this moment, corrosion current was 120mA, control terminal point time-delay 40ms, and obtaining the front end radius-of-curvature is that 30nm, length breadth ratio are 2 Pt-Ir needle point, not only is fit to STM but also be fit to the SECM imaging.
To a segment length 15mm, the length of an end 0.5mm of the Pt-Ir silk of diameter 0.3mm insulate with polymethylstyrene and seals, and is 0.5mm with sealing that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution.The saturated lime chloride that consists of of etchant solution is 15mL, and water is 65mL, and acetone is 20mL; Corrode under the alternating voltage of 15V, 50Hz, this moment, corrosion current was 160mA, control terminal point time-delay 70ms, and obtaining the front end radius-of-curvature is that 50nm, length breadth ratio are 1 Pt-Ir needle point, is fit to the SECM imaging.
Through experiment, gained Pt-Ir needle point is suitable for scanning tunneling microscopic and sees mirror (STM) or/and the micro-sight mirror of scan-type electrochemical (SECM) imaging.
Below provide the reference model and the referential data of the main components and parts among Fig. 3.
Potentiometer RP1:10K;
Integrated circuit U1～U6:OP07 type, U7, U10:TDA2030 type, U8, U9:INA121 type;
Triode Q1:9014C type;
K switch 1A, K1B:TQ4-L-5V;
Diode D1-D5:IN4148;
Combination hub J1: connect ac signal which, J2: connect electrolytic cell, J3: connect radiator fan;
JP1: connect the USB acquisition module, JP2: connect the USB acquisition module.
Claims (9)
1. the device for preparing platinum-iridium needle point, it is characterized in that being provided with ac voltage signal generation circuit, power amplification circuit, the corrosion current sample circuit, the AC signal amplifying circuit, the AC value change-over circuit, the direct current signal amplifying circuit, data acquisition circuit, braking circuit and corrosion electrolytic cell, ac voltage signal generation circuit input end connects the computing machine USB interface, ac voltage signal generation circuit output end connects the power amplification circuit input end, the power amplification circuit output terminal connects braking circuit input end and corrosion current sample circuit input end respectively, braking circuit output terminal and corrosion current sample circuit current signal output end connect the corrosion electrolytic cell respectively, the braking circuit signal input end connects the computing machine USB interface, corrosion current sample circuit voltage output end connects the AC signal input amplifier, the AC signal amplification circuit output end connects AC value change-over circuit input end, AC value change-over circuit output termination direct current signal input amplifier, the direct current signal amplification circuit output end connects the data acquisition circuit input end, data acquisition circuit output termination computing machine USB interface.
2. the preparation method of platinum-iridium needle point is characterized in that may further comprise the steps:
1) get one section Pt-Ir silk,, the one end insulated with polymethylstyrene seal through after the hydrogen flame annealing, but the other end be enclosed within on the syringe needle and be fixed on the iron stand of up-down adjustment, link to each other by the working electrode of lead with the device of preparation platinum-iridium needle point;
2) getting two spectroscopic pure carbon-points connects and is fixed on teflon with lead and cover as auxiliary electrode, link to each other with the auxiliary electrode of device of preparation platinum-iridium needle point, two spectroscopic pure carbon-points are parallel to the Pt-Ir silk and are that symcenter is vertically inserted in the etchant solution with the Pt-Ir silk;
3) regulate iron stand transfer arm above-below direction, the end of sealing of Pt-Ir silk is inserted in the etchant solution vertically downward and keeps the degree of depth of exposed part in etchant solution;
4) output voltage of regulating between working electrode and auxiliary electrode is 10～20V alternating voltage and passes through current acquisition circuit monitors corrosion current, seals the disconnection of part intersection until exposed part and insulation that the Pt-Ir silk is dipped in the etchant solution;
5) the top needle point that forms is continued to restart braking circuit behind the etch polishing and cut off corrosion loop, remove burr and control the length breadth ratio of needle point, obtain sharp-pointed platinum-iridium needle point.
3. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 1), and the length of Pt-Ir silk is 8～25mm, and diameter is 0.2～0.3mm.
4. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 1), is 0.5mm with the insulate length of the end sealed of polymethylstyrene.
5. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 2) in, be parallel to the Pt-Ir silk and be that symcenter is vertically inserted two spectroscopic pure carbon-points in the etchant solution and kept distance 10～50mm with the Pt-Ir silk with the Pt-Ir silk.
6. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 2) in, by mass percentage, etchant solution consist of saturated lime chloride 10%～30%, acetone 10%～30%, Yu Weishui.
7. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 3), with the Pt-Ir silk to seal that end inserts in the etchant solution vertically downward and keep the degree of depth of exposed part in etchant solution be 0.5～1mm.
8. the preparation method of platinum as claimed in claim 2-iridium needle point, it is characterized in that in step 4), by the Control Software of device of preparation platinum-iridium needle point, regulate output voltage between working electrode and auxiliary electrode and be 10～20V alternating voltage and by current acquisition circuit monitors corrosion current.
9. the preparation method of platinum as claimed in claim 2-iridium needle point is characterized in that in step 5), and the time of described continuation etch polishing is 10～80ms.
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| CNB2007100093114A CN100527285C (en) | 2007-07-31 | 2007-07-31 | Method for manufacturing platinum-iridium needlepoint and device thereof |
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| CNB2007100093114A CN100527285C (en) | 2007-07-31 | 2007-07-31 | Method for manufacturing platinum-iridium needlepoint and device thereof |
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Cited By (4)
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| CN104101738A (en) * | 2014-07-10 | 2014-10-15 | 华中科技大学 | Preparation device and preparation method of nanometer probe controllable and large in length to diameter ratio |
| 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 |
| CN108196093A (en) * | 2017-12-26 | 2018-06-22 | 北京阳光凯特科技有限公司 | A kind of auxiliary device of preparation for metallic nano detecting probe |
| CN109709353A (en) * | 2019-01-11 | 2019-05-03 | 中国电子科技集团公司第三十八研究所 | A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302586A (en) * | 2000-01-03 | 2001-07-11 | 林陆山 | Method for positioning channel and collateral and process for preparing probe |
| US7507320B2 (en) * | 2004-10-09 | 2009-03-24 | Academia Sinica | Single-atom tip and preparation method thereof |
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2007
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104101738A (en) * | 2014-07-10 | 2014-10-15 | 华中科技大学 | Preparation device and preparation method of nanometer probe controllable and large in length to diameter ratio |
| CN104101738B (en) * | 2014-07-10 | 2016-08-24 | 华中科技大学 | The preparation facilities of a kind of controlled big L/D ratio nano-probe and preparation method |
| 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 |
| CN108196093A (en) * | 2017-12-26 | 2018-06-22 | 北京阳光凯特科技有限公司 | A kind of auxiliary device of preparation for metallic nano detecting probe |
| CN109709353A (en) * | 2019-01-11 | 2019-05-03 | 中国电子科技集团公司第三十八研究所 | A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point |
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