CN109709353A - A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point - Google Patents
A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point Download PDFInfo
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- CN109709353A CN109709353A CN201910031214.8A CN201910031214A CN109709353A CN 109709353 A CN109709353 A CN 109709353A CN 201910031214 A CN201910031214 A CN 201910031214A CN 109709353 A CN109709353 A CN 109709353A
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Abstract
The present invention discloses the electrochemistry preparation facilities and preparation method of a kind of metal iridium needle point, including etching regulating device, control circuit and electrochemical cell, electrode is placed in electrolyte, the end of iridium wire to be prepared is placed in electrolyte by probe clamp, and the positive and negative anodes of pressure-variable alternating-current voltage source connect to form etched circuit with electrode and probe clamp respectively by control circuit；Etching regulating device adjusts the length dimension that the iridium wire to be prepared protrudes under the liquid level of electrolyte；Effective real-time current value and the connection or disconnection of etched circuit are controlled in control circuit acquisition etched circuit；The terminal that the present invention passes through control circuit control etching, etching voltage break time can be accurately controlled, it is easy to operate, the iridium needle point radius of curvature of preparation is small, it is reproducible, it is easy to get the optimum condition of iridium wire etching, the needle point of preparation is made to keep preferable pattern, and success rate with higher and preferable reproducibility.
Description
Technical field
The present invention relates to scanning probe preparation technical fields, and in particular to a kind of electrochemistry preparation facilities of metal iridium needle point
And preparation method.
Background technique
Iridium wire has high Young's modulus and chemical stability, has wider potential window in the solution, is adapted to
Probe as scanning probe microscopy；Iridium needle point, can be with other than the application in scanning probe microscopy field simultaneously
Using the fields such as lift-off technology on the scene and Tip-Enhanced Raman Spectroscopy technology, field is had a wide range of applications.
In scanning probe microscopy field, size, shape and the chemical component of probe tip directly affect scanning
The quality of probe microscope image, needle point tip is more sharp, shape is more symmetrical, and the quality and resolution ratio of image are higher.Laboratory
In more commonly used needle point preparation method have mechanical shearing method and electrochemical etching method, the needle point tip shape that mechanical shearing method obtains
Looks are asymmetric, come to the scanning probe microscopy needle point Wrapping belt in subsequent solution difficult；The equipment of electrochemical etching method is simple,
It is easy to operate, according to the alive property of institute, and direct current chemical etching method and AC electrochemical etching method can be divided into.However, iridium
Wire material is because of its chemical stability height, and required etching voltage is high, etch period is long, no matter is carved using direct current or AC electrochemical
The difficulty that erosion method prepares needle point is all larger, is especially difficult to control tip dimensions and shape.
The electrochemical etching method of existing probe tip preparation, generally use two-step method: first electricity consumption chemical etching method obtains song
The biggish needle point of rate radius, then fast moving in film etching liquid makes that needle point is more sharp, surface is more smooth.But existing side
Two steps in method need to use different electrolyte, and the instrument and equipment being related to is more, and making step is complicated.
In view of the above drawbacks, creator of the present invention obtains the present invention by prolonged research and practice finally.
Summary of the invention
To solve above-mentioned technological deficiency, the technical solution adopted by the present invention is, provides a kind of electrification of metal iridium needle point
Preparation facilities, including etching regulating device, control circuit and electrochemical cell are learned, the etching regulating device includes probe clamp；
The electrochemical cell includes electrode, iridium wire to be prepared and electrolyte；The electrode is placed in the electrolyte, the Probe clip
Tool clamps the iridium wire to be prepared and the end of the iridium wire to be prepared is placed in the electrolyte, pressure-variable alternating-current voltage source
Positive and negative anodes connect with the electrode and the probe clamp respectively by the control circuit and to form etched circuit；The etching
Regulating device controls the height of the probe clamp to adjust the length that the iridium wire to be prepared protrudes under the liquid level of electrolyte
Spend size；The control circuit acquires effective real-time current value in the etched circuit and controls the connection of the etched circuit
Or it disconnects.
Preferably, the control circuit includes upper computer control module, relay module, signal acquisition module and leads to
Believe interface；The relay module and the signal acquisition module access the etched circuit, the relay module control
Make the connection and disconnection of the etched circuit；The signal acquisition module acquires effective electricity in real time in the etched circuit
Flow valuve；The relay module and the signal acquisition module pass through the communication interface and the PC control mould
Block connection.
Preferably, the etching regulating device further includes L-type support, manual slide unit, working plate；Equipped with the electrolyte
Container is arranged on the working plate, and the probe clamp is arranged in the L-type support, and the L-type support passes through the hand
Dynamic slide unit is arranged on the working plate, and the manual slide unit is provided with micrometer head, and the hand is adjusted by the micrometer head
Dynamic height and position of the slide unit on the working plate.
Preferably, a kind of electrochemistry preparation facilities using the metal iridium needle point carries out the preparation side of metal iridium needle point
Method, including step；
S1 configures the electrolyte；
S2 pours into the electrolyte in the container, and the probe clamp for being fixed with the iridium wire to be prepared is consolidated
Determine onto the manual slide unit, adjusts the micrometer head, the end of the iridium wire to be prepared is immersed to the liquid level of the electrolyte
Under；
S3, the positive and negative polarities of the pressure-variable alternating-current voltage source are respectively arranged with the connection with electrode holder and switch and lead
Line, by the electrode holder by the positive and negative polarities of the pressure-variable alternating-current voltage source respectively with the probe clamp and the electrode
Connection；
S4 opens the pressure-variable alternating-current voltage source, adjusts the voltage parameter of the etched circuit, starts the connection and leads
The switch on line, to carry out electrochemical etching until the end of the iridium wire to be prepared is formed initial iridium needle point；
S5 is processed by shot blasting the initial iridium needle point；
S6 after the polishing treatment, disconnects the switch；
S7 adjusts the micrometer head, and the iridium wire to be prepared is made to be fully removed the electrolyte；
S8 collects the iridium wire needle point of the iridium wire end to be prepared and is carried out with distilled water and alcohol to the iridium wire needle point
Cleaning.
Preferably, the alternating voltage virtual value of the initial etched circuit is set as 30V~40V in the step S4, when
When the diameter of the iridium wire to be prepared is reduced to a quarter of initial diameter, the alternating voltage virtual value of the etched circuit is set
It is set to 20V.
Preferably, when the voltage value of the etched circuit is fixed, with iridium wire end to be prepared described in the electrolyte
The progress of etching passes through the host computer along with the continuous diminution of iridium wire diameter to be prepared described under the liquid level of electrolyte
The etched circuit real-time current value of control module observation is gradually reduced, and is judged by the real-time current value described to be prepared
The diameter change of iridium wire.
Preferably, chopping current value is set in the upper computer control module, when the iridium wire to be prepared starts etching,
The real-time current value is compared by the upper computer control module with the chopping current value, when judging the real-time current
When value is lower than the chopping current value, the relay module on the etched circuit receives the upper computer control module
The cutting order of sending quickly cuts off the ac voltage signal that the pressure-variable alternating-current voltage source provides, thus by the electrification
Etching process is learned to stop and form the initial iridium needle point.
Preferably, the step S5 is to adjust the micrometer head, the iridium wire to be prepared is moved up until the initial iridium
Needle point largely removes the liquid level of the electrolyte, and the initial iridium needle point protrudes into the subsurface length dimension of the decomposed solution and sets
It is set to 0.1mm~0.2mm.
Preferably, restarting the control circuit, the alternating voltage of the etched circuit is set as 1V, to the decomposed solution
The interior initial iridium needle point continues fine polishing；Set pre-set current value, when the upper computer control module monitor it is described
When real-time current value is lower than the pre-set current value, the etched circuit is cut off by the relay module, to obtain iridium
Silk needle point.
Preferably, restarting the control circuit, the alternating voltage of the etched circuit is set as 1V, to the decomposed solution
The interior initial iridium needle point continues fine polishing；Default polishing time is set, when the upper computer control module monitors institute
It states after the polishing treatment time reaches the default polishing time, the etched circuit is cut off by the relay module, thus
Obtain iridium wire needle point.
The beneficial effects of the present invention are the ends that: the present invention passes through control circuit control etching compared with the prior art
Point can be accurately controlled etching voltage break time, and easy to operate, the iridium needle point radius of curvature of preparation is small, reproducible, hold
The optimum condition for easily obtaining iridium wire etching makes the needle point of preparation keep preferable pattern, and success rate with higher and preferably
Reproducibility.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the electrochemistry preparation facilities of metal iridium needle point of the present invention；
Fig. 2 is the process schematic of step s4 in the preparation method of metal iridium needle point of the present invention；
Fig. 3 is the process schematic of step S5 in the preparation method of metal iridium needle point of the present invention；
Fig. 4 is the scanning electron microscope master drawing of the iridium wire needle point obtained.
Digital representation in figure:
1-L type bracket；The manual slide unit of 2-；3- working plate；4- probe clamp；5- control circuit；6- pressure-variable alternating voltage
Source；7- upper computer control module；8- relay module；9- signal acquisition module；10- communication interface；11- electrode；12- is waited for
Prepare iridium wire；13- container；14- electrolyte.
Specific embodiment
Below in conjunction with attached drawing, the forgoing and additional technical features and advantages are described in more detail.
Embodiment one
As shown in FIG. 1, FIG. 1 is the structural schematic diagrams of the electrochemistry preparation facilities of metal iridium needle point of the present invention.It is described
The electrochemistry preparation facilities of metal iridium needle point includes etching regulating device, control circuit and electrochemical cell, and the etching adjusts dress
It sets including L-type support 1, manual slide unit 2, working plate 3 and probe clamp 4；The control circuit 5 includes pressure-variable alternating-current voltage source
6, upper computer control module 7, relay module 8, signal acquisition module 9 and communication interface 10；The electrochemical cell includes
Electrode 11, iridium wire to be prepared 12, container 13 and electrolyte 14.
The electrolyte 14 is arranged in the container 13, and the electrode 11 is placed in the electrolyte 14, the spy
Needle fixture 4 clamps the iridium wire to be prepared 12 and is placed in the electrolyte 14, the positive and negative anodes of the pressure-variable alternating-current voltage source 6
It is connect respectively with the electrode 11 and the probe clamp 4 by the control circuit 5, to form etched circuit.
The container 13 equipped with the electrolyte 14 is arranged on the working plate 3, and the probe clamp 4 is arranged in institute
It states in L-type support 1, the L-type support 1 is arranged on the working plate 3 by the manual slide unit 2, and the manual slide unit 2 is set
It is equipped with micrometer head, height and position of the manual slide unit 2 on the working plate 3 is adjusted by the micrometer head, to adjust
It saves the iridium wire to be prepared 12 and protrudes into the subsurface length dimension of the electrolyte 14.
The relay module 8 and the signal acquisition module 9 access the etched circuit, the relay module
The connection and disconnection of the 8 control etched circuits；The signal acquisition module 9 acquires effective real in the etched circuit
When current value；The relay module 8 and the signal acquisition module 9 by the communication interface 10 with it is described upper
Machine control module 7 connects.
Specifically, the pressure-variable alternating-current voltage source 6 generates alternating voltage and loads in the electrode 11 and the probe
On fixture 4, to generate 0 to 300mA or so etching electric current in the electrochemical cell.Using the high-precision AC signal
Acquisition module 9 acquires effective real-time current value in the etched circuit, and passes through the communication interface 10 and the host computer
Control module 7 carries out data communication, and the upper computer control module 7 is according to the real-time current value real-time display of acquisition
Current waveform in etched circuit.
Preferably, chopping current value is arranged in the upper computer control module 7, when the signal acquisition module 9
When real-time current value in the collected etched circuit meets condition, the relay in the control circuit 5 is set
Device module 8 receives cutting order, quickly cuts off the ac voltage signal that the pressure-variable alternating-current voltage source 6 provides.
The technical scheme is that preparing iridium wire needle point using AC electrochemical etching method, pass through the control circuit 5
The terminal for controlling etching can be accurately controlled etching voltage break time, easy to operate, the iridium needle point radius of curvature of preparation
It is small, it is reproducible, it is easy to get the optimum condition of iridium wire etching, so that the needle point of preparation is kept preferable pattern, and have higher
Success rate and preferable reproducibility.
Embodiment two
The preparation method of metal iridium needle point of the present invention, specifically includes step；
S1 configures the electrolyte 14；
S2 pours into the electrolyte 14 in the container 13, will be fixed with the probe of the iridium wire to be prepared 12
Fixture 4 is fixed on the manual slide unit 2, adjusts the micrometer head, and the electricity is immersed in the end of the iridium wire 12 to be prepared
Under the liquid level for solving liquid 14；
S3, the positive and negative polarities of the pressure-variable alternating-current voltage source 6 are respectively arranged with the connection with electrode holder and switch and lead
Line, by the electrode holder by the positive and negative polarities of the pressure-variable alternating-current voltage source 6 respectively with the probe clamp 4 and the electricity
Pole 11 connects；
S4 opens the pressure-variable alternating-current voltage source 6, adjusts the voltage parameter of the etched circuit, starts the connection
The switch on conducting wire, to carry out electrochemical etching until the end of the iridium wire 12 to be prepared is formed initial iridium needle
Point；
S5 is processed by shot blasting the initial iridium needle point；
S6 after the polishing treatment, disconnects the switch；
S7 adjusts the micrometer head, and the iridium wire to be prepared 12 is made to be fully removed the electrolyte 14；
S8, collect the iridium wire needle point of 12 end of iridium wire to be prepared and with distilled water and alcohol to the iridium wire needle point into
Row cleaning.
In step sl, specifically, a certain amount of CaCl that will be weighed in the balance2Powder pours into beaker, then with measuring cup amount
A certain amount of deionized water is taken, by CaCl2Powder and deionized water mixed configuration are saturated CaCl2Solution, the saturation CaCl2It is molten
Liquid is the electrolyte 14.
As shown in Fig. 2, Fig. 2 is the process schematic of step S4 in the preparation method of metal iridium needle point of the present invention；Institute
It states in step S4, when the voltage value of the etched circuit is fixed, with 12 end of iridium wire to be prepared described in the electrolyte 14
The progress of portion's etching, the upper computer control module 7 acquire the electricity of the etched circuit by the signal acquisition module 9
Stream signal simultaneously shows effective real-time current value, not along with 12 diameter of iridium wire to be prepared described under 14 liquid level of electrolyte
It is disconnected to reduce, it is gradually reduced by the real-time current value that the upper computer control module 7 can observe the etched circuit；It is logical
Cross the diameter change that the real-time current value judges the iridium wire to be prepared.
Preferably, the alternating voltage virtual value of the initial etched circuit may be configured as between 30V~40V, when it is described to
Prepare iridium wire 12 diameter reduce be about original diameter a quarter when, the etched circuit alternating voltage virtual value setting more
It is changed to 20V.The original diameter, that is, iridium wire 12 to be prepared initial diameter, it is described specially before being put into the electrolyte 14
The diameter of iridium wire 12 to be prepared.
Chopping current value is set in the upper computer control module 7, it is described when the iridium wire 12 to be prepared starts etching
The real-time current value is compared by upper computer control module 7 with the chopping current value, when judging the real-time current value
When lower than the chopping current value, the relay module 8 on the etched circuit receives the upper computer control module 7
The cutting order of sending quickly cuts off the ac voltage signal that the pressure-variable alternating-current voltage source 6 provides, thus by the electrification
Etching process is learned to stop being formed and the initial iridium needle point.
Fig. 3 is the process schematic of step S5 in the preparation method of metal iridium needle point of the present invention；Step S5 specifically,
The micrometer head is adjusted, the iridium wire 12 to be prepared is moved up until the initial iridium needle point largely removes the electrolyte 14
Liquid level；Preferably, retaining the part initial iridium needle point under the decomposed solution liquid level, the initial iridium needle point protrudes into described
The subsurface length dimension L of decomposed solution is about set as 0.1mm~0.2mm.
Restart the control circuit 5, the alternating voltage of the etched circuit is set as 1V, to the institute in the decomposed solution
It states initial iridium needle point and continues fine polishing；Pre-set current value and default polishing time are set, when the upper computer control module 7 is supervised
When measuring the real-time current value lower than the pre-set current value or the polishing treatment time reaches the default polishing time
Afterwards, the etched circuit is cut off by the relay module 8, to obtain sharp iridium wire needle point.The pre-set current value
With the default polishing time best practices value can be obtained by repeating experiment several times.As shown in figure 4, Fig. 4 is the described of acquisition
The scanning electron microscope master drawing of iridium wire needle point.
The present invention have preparation method is simple and convenient to operate, preparation cost is cheap, high yield rate, high repeatability and other advantages,
The iridium wire needle point of the minimum 5nm of front end radius of curvature can be made, can be applied to scanning probe microscopy and field emission electron
Source.
The foregoing is merely presently preferred embodiments of the present invention, is merely illustrative for the purpose of the present invention, and not restrictive
's.Those skilled in the art understand that in the spirit and scope defined by the claims in the present invention many changes can be carried out to it,
It modifies or even equivalent, but falls in protection scope of the present invention.
Claims (10)
1. a kind of electrochemistry preparation facilities of metal iridium needle point, which is characterized in that including etching regulating device, control circuit and electricity
Chemical bath, the etching regulating device includes probe clamp；The electrochemical cell includes electrode, iridium wire to be prepared and electrolyte；
The electrode is placed in the electrolyte, and the probe clamp clamps the iridium wire to be prepared for the end of the iridium wire to be prepared
Portion is placed in the electrolyte, the positive and negative anodes of pressure-variable alternating-current voltage source by the control circuit respectively with the electrode and
The probe clamp connects to form etched circuit；The etching regulating device controls the height of the probe clamp to adjust institute
State the length dimension that iridium wire to be prepared protrudes under the liquid level of electrolyte；The control circuit acquires in the etched circuit effectively
Real-time current value and control the connection or disconnection of the etched circuit.
2. the electrochemistry preparation facilities of metal iridium needle point as described in claim 1, which is characterized in that the control circuit includes
Upper computer control module, relay module, signal acquisition module and communication interface；The relay module is exchanged with described
Signal acquisition module accesses the etched circuit, and the relay module controls the connection and disconnection of the etched circuit；It is described
Signal acquisition module acquires effective real-time current value in the etched circuit；The relay module exchanges letter with described
Number acquisition module is connect by the communication interface with the upper computer control module.
3. the electrochemistry preparation facilities of metal iridium needle point as described in claim 1, which is characterized in that the etching regulating device
It further include L-type support, manual slide unit, working plate；Container equipped with the electrolyte is arranged on the working plate, the probe
Fixture is arranged in the L-type support, and the L-type support is arranged on the working plate by the manual slide unit, the hand
Dynamic slide unit is provided with micrometer head, and height and position of the manual slide unit on the working plate is adjusted by the micrometer head.
4. a kind of preparation side of the electrochemistry preparation facilities using metal iridium needle point as claimed in any one of claims 1-3
Method, which is characterized in that including step；
S1 configures the electrolyte；
S2 pours into the electrolyte in the container, and the probe clamp for being fixed with the iridium wire to be prepared is fixed to
On the manual slide unit, the micrometer head is adjusted, the end of the iridium wire to be prepared is immersed under the liquid level of the electrolyte；
S3, the positive and negative polarities of the pressure-variable alternating-current voltage source are respectively arranged with the connecting wire with electrode holder and switch, lead to
The electrode holder is crossed to connect the positive and negative polarities of the pressure-variable alternating-current voltage source with the probe clamp and the electrode respectively；
S4 opens the pressure-variable alternating-current voltage source, adjusts the voltage parameter of the etched circuit, starts in the connecting wire
The switch, to carry out electrochemical etching until the end of the iridium wire to be prepared formed initial iridium needle point；
S5 is processed by shot blasting the initial iridium needle point；
S6 after the polishing treatment, disconnects the switch；
S7 adjusts the micrometer head, and the iridium wire to be prepared is made to be fully removed the electrolyte；
S8 collects the iridium wire needle point of the iridium wire end to be prepared and is carried out clearly with distilled water and alcohol to the iridium wire needle point
It washes.
5. preparation method as claimed in claim 3, which is characterized in that in the step S4, the friendship of the initial etched circuit
Stream voltage effective value is set as 30V~40V, when the diameter of the iridium wire to be prepared is reduced to a quarter of initial diameter,
The alternating voltage virtual value of the etched circuit is set as 20V.
6. preparation method as claimed in claim 5, which is characterized in that when the voltage value of the etched circuit is fixed, with institute
The progress of the iridium wire end etching to be prepared in electrolyte is stated, it is straight along with iridium wire to be prepared described under the liquid level of electrolyte
The continuous diminution of diameter is gradually reduced by the etched circuit real-time current value that the upper computer control module is observed, is passed through
The real-time current value judges the diameter change of the iridium wire to be prepared.
7. preparation method as claimed in claim 5, which is characterized in that chopping current is arranged in the upper computer control module
Value, when the iridium wire to be prepared starts etching, the upper computer control module is by the real-time current value and the chopping current
Value is compared, the relay when judging the real-time current value lower than the chopping current value, on the etched circuit
Device module receives the cutting order that the upper computer control module issues, and quickly cuts off the pressure-variable alternating-current voltage source and provides
Ac voltage signal, so that the electrochemical etching process be stopped and form the initial iridium needle point.
8. preparation method as claimed in claim 3, which is characterized in that the step S5 is to adjust the micrometer head, will be described
Iridium wire to be prepared moves up until the initial iridium needle point largely removes the liquid level of the electrolyte, and the initial iridium needle point protrudes into
The subsurface length dimension of decomposed solution is set as 0.1mm~0.2mm.
9. preparation method as claimed in claim 8, which is characterized in that restart the control circuit, the etched circuit
Alternating voltage is set as 1V, continues fine polishing to the initial iridium needle point in the decomposed solution；Pre-set current value is set, when
When the upper computer control module monitors the real-time current value lower than the pre-set current value, pass through the relay module
The etched circuit is cut off, to obtain iridium wire needle point.
10. preparation method as claimed in claim 8, which is characterized in that restart the control circuit, the etched circuit
Alternating voltage is set as 1V, continues fine polishing to the initial iridium needle point in the decomposed solution；Default polishing time is set,
After the upper computer control module monitors that the polishing treatment time reaches the default polishing time, pass through the relay
Device module cuts off the etched circuit, to obtain iridium wire needle point.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910031214.8A CN109709353A (en) | 2019-01-11 | 2019-01-11 | A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point |
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| CN201910031214.8A CN109709353A (en) | 2019-01-11 | 2019-01-11 | A kind of the electrochemistry preparation facilities and preparation method of metal iridium needle point |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110333371A (en) * | 2019-06-21 | 2019-10-15 | 武汉科技大学 | A kind of gold nano-probe preparation facilities and preparation method thereof |
| CN111190032A (en) * | 2020-01-08 | 2020-05-22 | 中国科学院力学研究所 | Atomic force probe preparation device and method and atomic force probe |
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| CN110333371A (en) * | 2019-06-21 | 2019-10-15 | 武汉科技大学 | A kind of gold nano-probe preparation facilities and preparation method thereof |
| CN111190032A (en) * | 2020-01-08 | 2020-05-22 | 中国科学院力学研究所 | Atomic force probe preparation device and method and atomic force probe |
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