CN102901846A - Device and method for preparing metal needle point - Google Patents
Device and method for preparing metal needle point Download PDFInfo
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- CN102901846A CN102901846A CN2012103133010A CN201210313301A CN102901846A CN 102901846 A CN102901846 A CN 102901846A CN 2012103133010 A CN2012103133010 A CN 2012103133010A CN 201210313301 A CN201210313301 A CN 201210313301A CN 102901846 A CN102901846 A CN 102901846A
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Abstract
The invention provides a device and a method for preparing a metal needle point. The device comprises a control circuit and an electrochemical pool, the control circuit comprises a power supply, a switch and a constant current source, the constant current source is used for maintaining constant current of the device, the electrochemical pool comprises a counter electrode, a metal wire to be prepared and an electrolyte, one end of the counter electrode is connected with a negative electrode end of the control circuit, and one end of the metal wire to be prepared is connected with a positive electrode end of the control circuit. The switch is closed, the constant current source maintains the constant current of the device, and the electrochemical pool starts reaction until the metal wire to be prepared is broken nearby the contact surface between the metal wire to be prepared and the electrolyte level. According to the device and the method for preparing the metal needle point, the constant current source is arranged in the control circuit, the constant current is maintained in the whole process of electrochemical corrosion, thereby the constant rate of electric charge reaching to the surface of the metal wire is maintained, the electrochemical reaction process is stable, the needle point with a small tip curvature radius and smooth surface can be obtained with a high repeatability, and the preparing method is simple in operation and high in success rate.
Description
Technical field
The present invention relates to the scanning probe microscopy technical field, relate in particular to the apparatus and method that a kind of Constant Electric Current chemical corrosion prepares the superfine metal needle point.
Background technology
Scanning probe microscopy (Scanning probe microscope, SPM)---comprise scanning tunnel microscope (Scanning tunneling microscope, STM) and atomic force microscope (Atomic force microscope)---since invention, become one of main laboratory facilities that characterize at nanoscale, obtained important achievement at the numerous areas that nanosecond science and technology relate to.And the preparation of needle point is one of key factor of SPM performance.In recent years on the basis of traditional SPM technology, along with single organic molecule conductance measurement and Tip-Enhanced Raman Spectroscopy (Tip-enhanced Raman Spectroscopy, the appearance of optically-coupled SPM technology such as TERS), the materials such as traditional tungsten, platinum, silicon prepare needle point and have demonstrated gradually limitation, need to use the New type of S PM needle point of the material such as gold, silver preparation.
This wherein particularly uses the needle point of gold preparation, has following advantage: on the one hand, the local enhancement effect to electromagnetic field near tens nanometer range most advanced and sophisticated that causes owing to its surface plasmon resonance and antenna effect is remarkable, and just in time be in visible light wave range, be applicable to carry out the TERS experiment, thereby increase substantially the spatial resolution of Raman spectrum.On the other hand, the chemistry of gold stable in properties, not can with atmosphere in oxygen etc. chemical reaction occurs, can directly in the environment such as atmosphere or solution, work, the electricity of measuring single organic molecule is led or the SPM that carries out TERS etc. and optically-coupled measures, and does not need the particular surroundingss such as ultrahigh vacuum.When carrying out surface topography and electrical measurement, for the requirement of acupuncture needle point be its terminal more point better, namely little tip curvature radius is to obtain high spatial resolution.And when utilizing the surface phasmon enhancement effect to carry out the experiment such as TERS, not only require its terminal radius-of-curvature little, and require smooth surface.In addition, all require the preparation of needle point to have high repetition rate, under the inducing of electron beam, pollute at the needle surface deposit carbon when avoiding before experiment using scanning electron microscope to detect tips quality.
The galvanic corrosion spun gold is one of method for preparing at present acupuncture needle point comparative maturity.This method is inserted one section spun gold in the mixed solution of concentrated hydrochloric acid and alcohol, be connected to the positive pole of a direct supply, another electrode (to electrode) in the solution is connected to the negative pole of power supply, DC voltage in addition between the two, spun gold is immersed in the following part of liquid level and is tapered, and near the corrosion speed liquid level is the fastest and form very thin company's neck.Company's neck at liquid level place finally disconnects under the acting in conjunction of galvanic corrosion and the following part spun gold of liquid level gravity, thereby forms a needle point.Such one section spun gold with needle point can be directly used in the STM feedback model, keeps the distance of needle point sample room with the tunnel current of needle point sample room; Also can stick on the arm of quartz tuning fork, keep the distance of needle point sample room with atomic force, work in the AFM feedback model.
But what the galvanic corrosion spun gold used in the conventional art all is constant voltage mode, namely at spun gold and between to electrode in addition constant voltage corrode.In the bibliographical information best parameter be concentrated hydrochloric acid and alcohol with volume ratio 1:1 mixed preparing solution, corrosion voltage is 2.4 V.But the limitation of constant voltage corrosion is: hydrochloric acid can cover nearly surface with the electrochemical reaction product A uCl of gold on the one hand, thereby the ion that has influence in the solution arrives gold surface, so that reaction process is slack-off.The reaction product on spun gold surface is accumulated to a certain degree, can enter the solution from surface desorption, again so that gold surface expose so that reaction process is accelerated again.At periodicity deposition and the desorption of spun gold surface reaction product, meeting shows as the concussion of corrosion current so that the process of electrochemical reaction is sometimes fast and sometimes slow like this.On the other hand, spun gold and electrode and the direct contact resistance of their clamping device be difficult to guarantee can highly repeat when installing each time, this is so that the voltage drop that produces at this contact resistance becomes a uncertain factor.
Summary of the invention
Technical matters to be solved by this invention provides a kind of device and method for preparing the metal needle point.
In order to address the above problem, the invention provides a kind of device for preparing the metal needle point, comprise control circuit and electrochemical cell, described control circuit comprises power supply, switch, constant current source; Described power supply is used to described device that electric energy is provided, described switch is controlled the open and close of described device, described constant current source is used for keeping the described electrochemical cell of described device current constant and comprises electrode, tinsel to be prepared and electrolytic solution, described electrode one end linked to each other with the control circuit negative pole end, described tinsel to be prepared one end links to each other with the control circuit positive terminal, and a described end and the tinsel to be prepared that electrode is not linked to each other with the control circuit negative pole all do not insert in the electrolytic solution with the anodal end that links to each other of control circuit.
Further, described constant current source be arranged at power cathode and electrochemical cell between the electrode, further, described control circuit also comprises a voltage comparator, described voltage comparator has two input ends and an output terminal, input end and control circuit with the electrode link is linked to each other, be used for input to the potential value of electrode, another input end is set a reference potential, described output terminal links to each other with switch, described voltage comparator is used for relatively to electrode potential and reference potential, disconnects according to the comparative result gauge tap.
Further, the range of current of described constant current source output is 0.01 ~ 100mA.
Further, the scope of described reference potential be-15V ~+15V.
Further, to be immersed in the degree of depth under the liquid level of electrolyte be 0.1 ~ 10mm to described tinsel to be prepared.
Further, described material wiry to be prepared is a kind of in gold, silver, tungsten, the platinumiridio.
Further, described is a kind of in tungsten, platinum, gold or the carbon-point to electrode.
A kind of method that adopts said apparatus to prepare the metal needle point comprises the steps:
(1) provides a tinsel to be prepared;
(2) tinsel one end to be prepared is immersed under the liquid level of electrolyte of electrochemical cell, an end links to each other with the control circuit positive terminal;
(3) Closing Switch, the constant current source holdout device current constant of described control circuit, described electrochemical cell reacts, until near tinsel fracture to be prepared tinsel to be prepared and the liquid level of electrolyte surface of contact.
Further, described constant current source be arranged at power cathode and electrochemical cell between the electrode, further, described control circuit also comprises a voltage comparator, described voltage comparator has two input ends and an output terminal, input end and control circuit with the electrode link is linked to each other, be used for input to the potential value of electrode, another input end is set a reference potential, described output terminal links to each other with switch, described voltage comparator is used for relatively to electrode potential and reference potential, disconnects according to the comparative result gauge tap; Described method further comprises the steps:
(4) described voltage comparator is relatively to electrode potential value and reference potential value, if to the electrode potential value greater than the reference potential value, then continue execution in step (3); If less than the reference potential value, then switch disconnects to the electrode potential value, the device end of run.
Further, the range of current of described constant current source output is 0.01 ~ 100mA.
The invention has the advantages that, constant current source is set in control circuit, described constant current source is so that keep constant corrosion current in whole electrochemical corrosion course, thereby the speed that makes electric charge arrive wire surface is kept constant, make the process of electrochemical reaction more stable, can obtain the little and ganoid needle point of tip curvature radius with higher repeatability, this preparation method is simple to operate, and success ratio is high.
Description of drawings
Accompanying drawing 1 is depicted as the structural representation that first embodiment of the invention prepares the device of metal needle point;
Accompanying drawing 2 is depicted as the structural representation of device of the preparation metal needle point of second embodiment of the invention;
Accompanying drawing 3A and accompanying drawing 3B are depicted as the scanning electron microscope diagram sheet of the acupuncture needle point that adopts apparatus of the present invention and method preparation.
Embodiment
Elaborate below in conjunction with the embodiment of accompanying drawing to the device and method of preparation metal needle point provided by the invention.
Described control circuit 1 comprises power supply, switch 3 and constant current source 4.Described power supply provides electric energy for described device, and in the present embodiment, described positive source is positive direct-current source 5, and its electromotive force is+15V, and described power cathode is negative DC source 6, and its electromotive force is-15V.Described switch 3 is arranged at any position in the control circuit 1, controls the open and close of described device.Described constant current source 4 is connected with described power supply and switch 3, is used for keeping described device current constant, and preferably, the range of current of described constant current source 4 outputs is 0.01 ~ 100mA.
Described electrochemical cell 2 comprises electrode 7, tinsel to be prepared 8 and electrolytic solution 9.In the present embodiment, described electrolytic solution 9 is positioned in the U-shaped glass tube 10, and in other embodiments of the present invention, the container that holds electrolytic solution 9 can choose at random, and is not limited to U-shaped glass tube.Described electrode 7 one ends are linked to each other with the negative pole end of control circuit 1, the other end is immersed under the liquid level of electrolytic solution 9 of an end that is positioned at U-shaped glass tube 10.Described two electrodes that electrode 7 are used for forming with tinsel 8 to be prepared electrolytic cell are realized the corrosion to tinsel 8 to be prepared.Described to electrode 7 can be in tungsten, platinum, gold or the carbon-point a kind of.
One end of described tinsel to be prepared 8 links to each other with the positive terminal of control circuit 1, and the other end is immersed under the liquid level of electrolytic solution 9 of the other end that is positioned at U-shaped glass tube 10.The subsurface degree of depth that tinsel 8 to be prepared is immersed in electrolytic solution 9 can set up on their own according to actual needs, can prepare again well behaved metal needle point in order neither to waste tinsel, preferably, to be immersed in the degree of depth of electrolytic solution 9 be 0.1 ~ 10mm to described tinsel to be prepared 8.
In the present embodiment, the course of work of the device of preparation metal needle point is as follows: Closing Switch 3, described power supply provides electric energy for device, described constant current source 4 holdout device current constants, tinsel to be prepared 8 in the described electrochemical cell 2 is immersed in electrolytic solution 9 subsurface parts and begins the corrosion reaction, more and more thinner, and near the tinsel corrosion speed to be prepared electrolytic solution 9 liquid levels is the fastest, therefore, form very soon very thin company's neck at this place, along with the carrying out of corrosion reaction, connect neck more and more thinner, at last in galvanic corrosion be positioned under the electrolytic solution 9 subsurface Action of Gravity Fields wiry and rupture, thereby form a needle point.
The metal needle point all can adopt device of the present invention preparation, is a kind of in gold, silver, tungsten, the platinumiridio such as the material of tinsel 8 to be prepared.But for different metal materials, the electrolytic solution of employing is different, such as, the electrolytic solution that preparation acupuncture needle point adopts is the mixed liquor of concentrated hydrochloric acid and alcohol, preferably, the volume ratio of concentrated hydrochloric acid and alcohol is 1:1; The electrolytic solution that the preparation tungsten tip adopts is the sodium hydroxide solution of 1 ~ 5mol/L; The electrolytic solution that preparation platinumiridio needle point adopts is calcium chloride solution.
The device that the present invention prepares the metal needle point arranges constant current source in control circuit, thereby so that electrochemical cell is kept constant corrosion current in whole electrochemical corrosion course, thereby the speed that makes electric charge arrive wire surface is kept constant, make the process of electrochemical reaction more stable, can obtain the little and ganoid needle point of tip curvature radius with higher repeatability.
Preferably, also comprise a voltage comparator at control circuit described in the second embodiment of the invention 1, be used for relatively potential value and reference potential value to electrode, thereby the excessive erosion of metal needle point is avoided in the disconnection of gauge tap 3.
In the present embodiment, the course of work of the device of preparation metal needle point is as follows: Closing Switch 3, described power supply provides electric energy for device, described constant current source 4 holdout device current constants, tinsel to be prepared 8 in the described electrochemical cell 2 is immersed in electrolytic solution 9 subsurface parts and begins the corrosion reaction, the potential value V that described voltage comparator 11 gathers electrode 7
CDAnd will be to the potential value V of electrode 7
CDWith reference potential value V
REFCompare, if V
CD＞V
REFThen voltage comparator is not taked any action, and along with the carrying out of corrosion, the tinsel subsurface to be prepared 8 that is immersed in electrolytic solution 9 is more and more thinner, and near the tinsel corrosion speed to be prepared liquid level of electrolytic solution 9 is the fastest, therefore, form very soon very thin company's neck at this place, along with the carrying out of corrosion reaction, connect neck more and more thinner, resistance becomes greatly gradually, and being carried in increases gradually to the voltage between electrode 7 and the tinsel to be prepared 8, then to the potential value V of electrode 7
CDReduce gradually, connect at last neck in galvanic corrosion and be positioned under the electrolytic solution 9 subsurface Action of Gravity Fields wiry and rupture, in the moment that connects the neck fracture, can produce an electromotive force sudden change, V
CDSharply reduce, work as V
CDLess than reference potential V
REFThe time, voltage comparator 11 gauge tap 3 disconnect, and corrosion process finishes, and forms needle point.
In the present embodiment, the device of preparation metal needle point further arranges voltage comparator 11 in control circuit 1, by relatively to the potential value of electrode and default reference potential value, in the moment that connects the neck fracture, cut off open circuit potential, thereby the needle point of avoiding just having formed further is corroded, and affects the quality of needle point.If after connecting the neck fracture, open circuit potential does not still cut off, then electrochemical cell can work on, and the needle point that is positioned under the liquid level of electrolyte can continue to be corroded, so that the shape of needle point or smoothness be affected, thereby affects the needle point quality.
The present invention also provides and has adopted said apparatus to prepare the method for metal needle point, and concrete steps are as follows: step S31: a tinsel to be prepared is provided; Step S32: tinsel one end to be prepared is immersed under the liquid level of electrolyte of electrochemical cell, an end links to each other with the control circuit positive terminal; Step S33: Closing Switch, the constant current source holdout device current constant of described control circuit, described electrochemical cell reacts, until near tinsel fracture to be prepared tinsel to be prepared and the liquid level of electrolyte surface of contact; Step S34: voltage comparator is relatively to electrode potential value and reference potential value, if to the electrode potential value greater than the reference potential value, then continue execution in step S33; If less than the reference potential value, then switch disconnects to the electrode potential value, the device end of run.
Referring to step S31, provide a tinsel to be prepared.Metal needle point commonly used all can adopt device preparation of the present invention in the general scanning probe microscopy, such as the metal needle point can be sharp for acupuncture needle point, acupuncture needle, a kind of in the tungsten tip, platinumiridio needle point.But for the material of different preparation metal needle points, the electrolytic solution of employing is different, such as, the electrolytic solution that preparation acupuncture needle point adopts is the mixed liquor of concentrated hydrochloric acid and alcohol, preferably, the volume ratio of concentrated hydrochloric acid and alcohol is 1:1; The electrolytic solution that the preparation tungsten tip adopts is the sodium hydroxide solution of 1 ~ 5mol/L; The electrolytic solution that preparation platinumiridio needle point adopts is calcium chloride solution.
Referring to step S32: tinsel one end to be prepared is immersed under the liquid level of electrolyte of electrochemical cell, an end links to each other with the control circuit positive terminal.The subsurface degree of depth that tinsel to be prepared is immersed in electrolytic solution can set up on their own according to actual needs, can prepare again well behaved metal needle point in order neither to waste tinsel, preferably, to be immersed in the degree of depth under the liquid level of electrolyte be 0.1 ~ 10mm to described tinsel to be prepared.
Referring to step S33: Closing Switch, the constant current source of described control circuit are kept tinsel corrosion process current constant to be prepared, and described electrochemical cell reacts, until near tinsel fracture to be prepared tinsel to be prepared and the liquid level of electrolyte surface of contact.Preferably, the range of current of described constant current source 4 outputs is 0.01 ~ 100mA.In this step, Closing Switch, described power supply provides electric energy for device, described constant current source holdout device current constant, the part that tinsel to be prepared in the described electrochemical cell is immersed under the liquid level of electrolyte begins the corrosion reaction, more and more thinner, and near the tinsel corrosion speed to be prepared liquid level of electrolyte is the fastest, therefore, form very soon very thin company's neck at this place, along with the carrying out of corrosion reaction, connect neck more and more thinner, at last in galvanic corrosion be positioned under the Action of Gravity Field wiry under the liquid level of electrolyte and rupture, thereby form a needle point.
The method for preparing the metal needle point of the present invention is kept current constant in electrochemical corrosion course, from but electric charge arrives the speed of wire surface to be prepared keeps constant, so that the process of electrochemical reaction is more stable, can obtain the little and ganoid needle point of tip curvature radius with higher repeatability.
Preferably, referring to step S34: voltage comparator is relatively to electrode potential value and reference potential value, if to the electrode potential value greater than the reference potential value, then continue execution in step S33; If less than the reference potential value, then switch disconnects to the electrode potential value, the device end of run.This step is optional step.Described constant current source is arranged between negative direct supply and the electrochemical cell.The power supply comparer has two input ends and an output terminal, and a described input end is used for input to the potential value of electrode; Another input end is set a reference potential, is used for comparing with potential value to electrode, and output terminal directly is connected with switch.Definition is used V to the potential value of electrode
CDExpression, the value of reference potential is used V
REFExpression, the value V of described reference potential
REFSetting range be between the electromotive force of the electromotive force in positive direct-current source 5 and negative DC source 6, such as, in the present embodiment, the electromotive force in positive direct-current source 5 is+15V, the electromotive force of negative DC source 6 is-15V, then the value V of reference potential
REFScope be-15V ~+15V.
Described voltage comparator collection is to the potential value V of electrode
CDAnd will be to the potential value V of electrode
CDWith reference potential value V
REFCompare, if V
CD＞V
REFThen voltage comparator is not taked any action, and along with the carrying out of corrosion, the tinsel subsurface to be prepared that is immersed in electrolytic solution is more and more thinner, and near the tinsel corrosion speed to be prepared liquid level of electrolytic solution is the fastest, therefore, form very soon very thin company's neck at this place, along with the carrying out of corrosion reaction, connect neck more and more thinner, resistance becomes greatly gradually, and being carried in increases gradually to the voltage between electrode and the tinsel to be prepared, then to the potential value V of electrode
CDReduce gradually, connect at last neck in galvanic corrosion and be positioned under the Action of Gravity Field wiry under the liquid level of electrolyte and rupture, in the moment that connects the neck fracture, can produce an electromotive force sudden change, V
CDSharply reduce, work as V
CDLess than reference potential V
REFThe time, the voltage comparator gauge tap disconnects, and corrosion process finishes, and forms needle point.
Adopt voltage comparator relatively to the potential value of electrode and default reference potential value, in the moment that connects the neck fracture, meeting is so that sharply reduce the electromotive force of electrode, thereby less than default reference potential, voltage comparator cuts off open circuit potential according to comparative result, thereby the needle point of avoiding just having formed further is corroded, and affects the quality of needle point.
The below enumerates embodiments of the invention take preparation acupuncture needle point as example.
One spun gold is provided, the diameter of described spun gold is 0.2mm, spun gold is immersed in 2mm under the liquid level of electrolyte, and described electrolytic solution is that the volume ratio of concentrated hydrochloric acid and alcohol is 1:1, and the setting reference potential is 0V, setting described constant current source control open circuit potential is 6mA, opening switch, galvanic corrosion reaction carry out, in the moment of company's neck fracture of spun gold, voltage comparator cuts off open circuit potential according to comparative result, thereby prepares the acupuncture needle point.Accompanying drawing 3A and accompanying drawing 3B are depicted as the scanning electron microscope diagram sheet of an acupuncture needle point of apparatus of the present invention and method preparation, and wherein accompanying drawing 3A is the low power picture, and accompanying drawing 3B is the high power picture.Upper as seen from picture accompanying drawing 3B, the tip diameter of acupuncture needle point only has 25nm.In the present embodiment, adopt identical parameter to prepare 13 needle points, wherein have the tip diameter of 11 acupuncture needle points to be no more than 40nm, in these 11 acupuncture needle points, the tip diameter of 4 acupuncture needle points is arranged in 20 ~ 30nm scope.In the present embodiment, the preparation of each needle point is finished within 5.5 ~ 6 minutes time automatically, and the acupuncture needle point of preparation can be directly used in without scanning electron microscope detects the TERS experiment of Single Walled Carbon Nanotube, obtained the spatial resolution of 15nm on the Raman light intensity picture.
Numerical value and the numerical range mentioned in the description of above-mentioned instructions are not limited to the present invention, just for the invention provides preferred embodiment.
The above only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a device for preparing the metal needle point comprises control circuit and electrochemical cell, it is characterized in that, described control circuit comprises power supply, switch, constant current source; Described power supply is used to described device that electric energy is provided, and described switch is controlled the open and close of described device, and described constant current source is used for keeping described device current constant; Described electrochemical cell comprises electrode, tinsel to be prepared and electrolytic solution, described electrode one end is linked to each other with the control circuit negative pole end, the other end inserts in the electrolytic solution, and described tinsel one end to be prepared links to each other with the control circuit positive terminal, and the other end inserts in the electrolytic solution.
2. the device of preparation metal needle point according to claim 1, it is characterized in that, described constant current source be arranged at power cathode and electrochemical cell between the electrode, further, described control circuit also comprises a voltage comparator, described voltage comparator has two input ends and an output terminal, input end and control circuit with the electrode link is linked to each other, be used for input to the potential value of electrode, another input end is set a reference potential, described output terminal links to each other with switch, and described voltage comparator is used for relatively to electrode potential and reference potential, disconnects according to the comparative result gauge tap.
3. the device of preparation metal needle point according to claim 1 and 2 is characterized in that, the range of current of described constant current source output is 0.01 ~ 100mA.
4. the device of preparation metal needle point according to claim 2 is characterized in that, the scope of described reference potential is-and 15V ~+15V.
5. the device of preparation metal needle point according to claim 1 and 2 is characterized in that, the degree of depth that described tinsel to be prepared is immersed under the liquid level of electrolyte is 0.1 ~ 10mm.
6. the device of preparation metal needle point according to claim 1 and 2 is characterized in that, described material wiry to be prepared is a kind of in gold, silver, tungsten, the platinumiridio.
7. the device of preparation metal needle point according to claim 1 and 2 is characterized in that, described is a kind of in tungsten, platinum, gold or the carbon-point to electrode.
8. a method that adopts the described device of claim 1 to prepare the metal needle point is characterized in that, comprises the steps: that (1) provides a tinsel to be prepared; (2) tinsel one end to be prepared is immersed under the liquid level of electrolyte of electrochemical cell, an end links to each other with the control circuit positive terminal; (3) Closing Switch, the constant current source holdout device current constant of described control circuit, described electrochemical cell reacts, until near tinsel fracture to be prepared tinsel to be prepared and the liquid level of electrolyte surface of contact.
9. the method for preparing the metal needle point according to claim 8, it is characterized in that, described constant current source be arranged at power cathode and electrochemical cell between the electrode, further, described control circuit also comprises a voltage comparator, described voltage comparator has two input ends and an output terminal, input end and control circuit with the electrode link is linked to each other, be used for input to the potential value of electrode, another input end is set a reference potential, described output terminal links to each other with switch, and described voltage comparator is used for relatively to electrode potential and reference potential, disconnects according to the comparative result gauge tap; Described method further comprises the steps: (4) described voltage comparator relatively to electrode potential value and reference potential value, if to the electrode potential value greater than the reference potential value, then continue execution in step (3); If less than the reference potential value, then switch disconnects to the electrode potential value, the device end of run.
10. according to claim 8 or the 9 described methods that prepare the metal needle point, it is characterized in that, the range of current of described constant current source output is 0.01 ~ 100mA.
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| CN104785871A (en) * | 2015-04-17 | 2015-07-22 | 清华大学深圳研究生院 | Probe manufacturing method and device |
| 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 |
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| CN109706515A (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 preparation facilities and preparation method of the tungsten wire needle point of controllable draw ratio |
| 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 |
| CN110568226A (en) * | 2019-08-16 | 2019-12-13 | 南方科技大学 | Method and device for preparing metal probe based on electrochemical etching |
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| CN104345178A (en) * | 2013-07-24 | 2015-02-11 | 国家纳米科学中心 | Preparation method of metal probe |
| CN105301288B (en) * | 2014-06-13 | 2019-04-05 | 中国科学院物理研究所 | A kind of device and method preparing metal needle point |
| CN104785871A (en) * | 2015-04-17 | 2015-07-22 | 清华大学深圳研究生院 | Probe manufacturing method and device |
| 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 |
| CN109706515A (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 preparation facilities and preparation method of the tungsten wire needle point of controllable draw ratio |
| 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 |
| CN110568226A (en) * | 2019-08-16 | 2019-12-13 | 南方科技大学 | Method and device for preparing metal probe based on electrochemical etching |
| CN110568226B (en) * | 2019-08-16 | 2022-05-03 | 南方科技大学 | Method and device for preparing metal probe based on electrochemical etching |
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