CN102650073A - Electrochemical etching method for directly obtaining micro nanowire at one end of macroscopic filament - Google Patents
Electrochemical etching method for directly obtaining micro nanowire at one end of macroscopic filament Download PDFInfo
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- CN102650073A CN102650073A CN2011100454782A CN201110045478A CN102650073A CN 102650073 A CN102650073 A CN 102650073A CN 2011100454782 A CN2011100454782 A CN 2011100454782A CN 201110045478 A CN201110045478 A CN 201110045478A CN 102650073 A CN102650073 A CN 102650073A
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Abstract
The invention discloses an electrochemical etching method for directly obtaining a micro nanowire at one end of a macroscopic filament, which belongs to the technical field of the electrochemical etching method. The method comprises the steps that (1) a macroscopic filament part is inserted into a container which contains chemical etching liquid; (2) the macroscopic filament is subjected to the etching treatment under alternating voltage until the diameter of a more uniform middle section of the filament which is soaked in the etching liquid is smaller than 100 mum; (3) the input voltage is lowered, the filament is continuously etched until bubbles on the surface of the filament which is soaked in the etching liquid are less or even disappeared; and (4) at the moment, the lowered input voltage can be maintained, the input voltage also can be appropriately increased, the filament is continuously etched so that the micro nanowire can be obtained, and the etching time is subject to the condition that the filament is not separated from the etching liquid level. The macroscopic filament with one end having the micro nanowire can be directly obtained through adopting the electrochemical etching method disclosed by the invention, and the electrochemical etching method has the characteristic of direct transition from macroscopic scale to micro nano-scale. The method is simple and practicable.
Description
Technical field
The invention belongs to the electrochemical etching method technical field, particularly a kind of electrochemical etching method that directly obtains the micro-nano rice noodles at macroscopical filament one end.
Background technology
Along with the micron/nano science and technology development; Nano wire and nano-probe be as the effective tool that leads to micro/nano-scale, make nano wire and nano-probe the micro-nano world is observed imaging, micro-nano structure is operated and the measurement of character such as physics, chemistry and electricity in bringing into play more and more important effect.
Have several different methods to obtain nano wire at present, comprise vapour deposition process, refer in specific substrate, prepare nano wire, nano belt and nanotube through vapour deposition, this method has become the important method of preparation monodimension nanometer material; The RF sputtering method is about to carrier gas and excites and be in substrate, the grow method of ad hoc structure of plasma bombardment target.General sputtering method is used for preparing thin-film material, but under some certain conditions, can grow nano wire or nanotube to specific element or compound; Template, exactly with material with nano aperture as template, obtain nano wire through corrosion or deposition; Electrochemical erosion method promptly corrodes whole being immersed in the corrosive fluid of wire; In addition, also have an emission revulsion and e-beam induced deposition method etc.Yet but also directly do not obtain an end and have the method for macroscopical filament of micro-nano rice noodles.And this macroscopical filament-micro-nano line structure has a wide range of applications with field operation in the micro-nano measurement.
Summary of the invention
For achieving the above object, the present invention proposes and a kind ofly directly obtain the electrochemical etching method of micro-nano rice noodles at macroscopical filament one end, it is characterized in that this method comprises:
(1) partly insert the container that chemical corrosion liquid is housed to macroscopical filament, inserted mode can be that vertical liquid level insertion also can be that oblique cutting is gone into;
(2) under alternating voltage, macroscopical filament is carried out corrosion treatment, more uniform one section diameter is less than 100 microns in the middle of the filament in being immersed in corrosive fluid;
(3) turn down input voltage, continue the corrosion filament, until be immersed in corrosive fluid under the filament surfaces bubble seldom even disappearance;
(4) can keep the input voltage after turning down this moment, can suitably transfer big input voltage yet, continue the corrosion filament, just can obtain the micro-nano rice noodles, etching time does not break away from the corrosion liquid level with filament and is as the criterion.
The all right sufficiently long of said (4) step etching time is until the nano wire completely dissolve, thus the acquisition nano-probe.
The VR of step (2) and step (3) can realize through the observation circuit corrosion current.
Step (2) also can increase following steps afterwards: the disconnection input voltage perhaps transfers to very little, raises filament to more even one section top then near the corrosion liquid level, and purpose is the micro-nano probe that the control acquisition has certain rigidity requirement;
The step that filament is raised in corrosion for some time then can repeat repeatedly, and in general, multiplicity is many more, and the rigidity of final micro-nano rice noodles that obtain or probe is just low more, for initial diameter less can not have the step of raising yet;
Raising the step of filament can carry out through the movable device that links to each other with filament, and movable device adopts the device that can control mobile accuracy, preferred screw micrometer.
Chemical corrosion liquid can adopt alkali lye, like potassium hydroxide solution.
The macroscopic view filament can be that wire also can be a spun glass etc.
The macroscopic view filament diameter is less than 2 millimeters.
Beneficial effect of the present invention is: adopt electrochemical etching method of the present invention can directly obtain macroscopical filament that an end has the micro-nano rice noodles; Its characteristics are that directly carrying out the transition to micro-nano from macroscopic view sees; Can be widely used in micro-nano measures and operation; Such as the electrical properties of four probe method micrometer micro-nano structure or device, and present method provides a kind of simple method for it.
Description of drawings
Fig. 1 is corrosion device figure according to a preferred embodiment of the invention;
Fig. 2-Fig. 5 is the tungsten filament that has the micro-nano rice noodles through the end that this law obtains;
Fig. 6 is most advanced and sophisticated for nano wire corrodes the remaining nano-probe in back, and 2 nano-probes have different cone angles.
Embodiment
Following embodiment can make those skilled in the art more comprehensively understand the present invention, but does not limit the present invention in any way.
Galvanic corrosion device as shown in Figure 1 comprises support 1, movable device 2, but amplitude modulation alternating current source 3, electrode 4, container 5, corrosive fluid 6, macroscopical filament 7.Wherein movable device links to each other with support, and macroscopical filament is clipped on the movable device, can control the degree of depth in macroscopical filament insertion corrosive fluid through moving movable device.In the present embodiment; The macroscopic view filament is about the polycrystalline tungsten filament of 2cm for diameter 0.30mm; Corrosive fluid is the KOH solution of concentration 5mol/L, and the initial optional 3-20mm of depth of penetration connects the input ac voltage source; In about 10 volts of following corrosion for some time of virtual value, stop corrosion in the middle of the tungsten filament in being immersed in corrosive fluid during about 50 microns of more uniform one section diameter; Then through movable device (movable device employing screw micrometer) raise tungsten filament until more even one section upper end near the corrosion liquid level; Connect alternating-current voltage source then, and corrode for some time the bubble collapse on the tungsten filament surface in being immersed in corrosive fluid at virtual value for about 1 volt down; Continue corrosion after about 10 minutes, turn off voltage source, promptly obtain needed micro-nano rice noodles; As shown in Figure 2, be the initial about 10mm of the degree of depth that inserts, the operation that repeats to raise for 3 times is arranged after step (2); Final about 20 nanometers of diameter that obtain nano wire, tens microns of length; Fig. 3 is the about 5mm of initial depth of penetration, once raises the result of operation, and the nanowire diameter of acquisition is less than 100nm; Fig. 4 is the about 20mm of initial depth of penetration, and follows the result of the operation of repeatedly raising.
A kind ofly directly obtain the electrochemical etching method of micro-nano rice noodles at macroscopical filament one end, this method comprises:
(1) partly inserts macroscopical tungsten filament the container that concentration is the Pottasium Hydroxide corrosive fluid of 4mol/L is housed;
(2) under the about 12 volts alternating voltage of virtual value, tungsten filament is carried out corrosion treatment, more uniform one section diameter is about 80 microns in the middle of the filament in being immersed in corrosive fluid;
(3) turn down input voltage, under the about 2 volts voltage of virtual value, continue the corrosion filament, until the filament surfaces bubble collapse that is immersed under the corrosive fluid;
(4) suitably transfer big input voltage, under the about 3 volts voltage of virtual value, continue the corrosion filament, after about 8 minutes, turn off voltage source, just can obtain the micro-nano rice noodles.Etching time does not break away from the corrosion liquid level with filament and is as the criterion.
Fig. 5 is respectively the result who is approximately 20mm and 5mm for initial depth of penetration, about 1 micron of the diameter of the middle micro wire of Fig. 5 (a), and length can reach the mm magnitude; Nanowire diameter is less than 200nm among Fig. 5 (b), and length can reach 20 microns.Fig. 6 continues the nano-probe that corrosion for some time obtains on the basis of micro-nano rice noodles, needle point is less than 100 nanometers, and also may command of needle point cone angle is spent (Fig. 6 (a)) from tens degree (Fig. 6 (b)) to more than 100.
The above; Be merely the preferable embodiment of the present invention; But protection scope of the present invention is not limited thereto, any technician who is familiar with the present technique field in the technical scope that the present invention discloses, the variation that can expect easily or replacement; Become certain shape to carry out above-mentioned corrosion or the like again like the macroscopical filament of bending, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (10)
1. one kind directly obtains the electrochemical etching method of micro-nano rice noodles at macroscopical filament one end, it is characterized in that this method comprises:
(1) partly inserts the container that chemical corrosion liquid is housed to macroscopical filament;
(2) under alternating voltage, macroscopical filament is carried out corrosion treatment, more uniform one section diameter is less than 100 microns in the middle of the filament in being immersed in corrosive fluid;
(3) turn down input voltage, continue the corrosion filament, until be immersed in corrosive fluid under the filament surfaces bubble seldom even disappearance;
(4) input voltage of keeping after turning down is perhaps suitably transferred big input voltage, continues the corrosion filament, acquisition micro-nano rice noodles.
2. method according to claim 1 is characterized in that: in the step (4), etching time is with carefully
Silk does not break away from the corrosion liquid level and is as the criterion.
3. method according to claim 1 is characterized in that: the etching time sufficiently long disappears until nano wire, obtains nano-probe.
4. method according to claim 1 is characterized in that: the adjusting of magnitude of voltage realizes through the monitoring corrosion current.
5. method according to claim 1 is characterized in that: step (2) increases following steps afterwards: the disconnection input voltage perhaps transfers to very little, raises filament to more even one section top then near the corrosion liquid level.
6. method according to claim 5 is characterized in that: the step that corrosion for some time is raised filament then repeats repeatedly.
7. method according to claim 5 is characterized in that: the step of raising filament is carried out through the movable device that links to each other with filament.
8. method according to claim 7 is characterized in that: movable device adopts screw micrometer.
9. method according to claim 1 is characterized in that: said macroscopical filament is wire or spun glass.
10. method according to claim 1 is characterized in that: said macroscopical filament diameter is less than 2 millimeters.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021491A (en) * | 2017-05-31 | 2017-08-08 | 华北电力大学（保定） | A kind of Ti5Si3Intermetallic compound micro-nano rice noodles and preparation method thereof |
| CN112831785A (en) * | 2020-12-28 | 2021-05-25 | 江苏兴达钢帘线股份有限公司 | Iron-based micro monofilament sharpening liquid and using method thereof |
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| JPS63313000A (en) * | 1987-06-15 | 1988-12-21 | Seiko Instr & Electronics Ltd | Production of probe |
| JPH04344403A (en) * | 1991-05-21 | 1992-12-01 | Mitsubishi Kasei Corp | Manufacture of chip for scanning type tunnel microscope |
| CN101324785A (en) * | 2008-07-17 | 2008-12-17 | 浙江大学 | Pure tungsten material micro-nano probe preparation control system for scanning tunnel microscope |
| CN101692100A (en) * | 2009-10-09 | 2010-04-07 | 南京大学 | Method and device for preparing pinpoint of scanning tunnel microscope (STM) |
| CN101696980A (en) * | 2009-10-27 | 2010-04-21 | 北京大学 | Method for preparing pinpoint of nano-tungsten probe |
| CN101701352A (en) * | 2008-12-15 | 2010-05-05 | 中国矿业大学(北京) | Method for preparing high-resolution emitter tungsten tip and device thereof |
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2011
- 2011-02-24 CN CN2011100454782A patent/CN102650073A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63313000A (en) * | 1987-06-15 | 1988-12-21 | Seiko Instr & Electronics Ltd | Production of probe |
| JPH04344403A (en) * | 1991-05-21 | 1992-12-01 | Mitsubishi Kasei Corp | Manufacture of chip for scanning type tunnel microscope |
| CN101324785A (en) * | 2008-07-17 | 2008-12-17 | 浙江大学 | Pure tungsten material micro-nano probe preparation control system for scanning tunnel microscope |
| CN101701352A (en) * | 2008-12-15 | 2010-05-05 | 中国矿业大学(北京) | Method for preparing high-resolution emitter tungsten tip and device thereof |
| CN101692100A (en) * | 2009-10-09 | 2010-04-07 | 南京大学 | Method and device for preparing pinpoint of scanning tunnel microscope (STM) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021491A (en) * | 2017-05-31 | 2017-08-08 | 华北电力大学（保定） | A kind of Ti5Si3Intermetallic compound micro-nano rice noodles and preparation method thereof |
| CN107021491B (en) * | 2017-05-31 | 2019-04-02 | 华北电力大学（保定） | A kind of Ti5Si3Intermetallic compound micro-nano rice noodles and preparation method thereof |
| CN112831785A (en) * | 2020-12-28 | 2021-05-25 | 江苏兴达钢帘线股份有限公司 | Iron-based micro monofilament sharpening liquid and using method thereof |
| CN112831785B (en) * | 2020-12-28 | 2023-03-21 | 江苏兴达钢帘线股份有限公司 | Iron-based micro monofilament sharpening liquid and using method thereof |
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Application publication date: 20120829 |