CN104101738A - Preparation device and preparation method of nanometer probe controllable and large in length to diameter ratio - Google Patents
Preparation device and preparation method of nanometer probe controllable and large in length to diameter ratio Download PDFInfo
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- CN104101738A CN104101738A CN201410329359.3A CN201410329359A CN104101738A CN 104101738 A CN104101738 A CN 104101738A CN 201410329359 A CN201410329359 A CN 201410329359A CN 104101738 A CN104101738 A CN 104101738A
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Abstract
The invention provides a preparation device of a nanometer probe controllable and large in length to diameter ratio. The preparation device of the nanometer probe controllable and large in length to diameter ratio and a single chip microcomputer are cooperatively used to achieve accurate control of important parameters of corrosion voltage, probe immersion depth, probe lifting speed and the like during the corrosion process by arranging a corrosion voltage stabilizing circuit, a corrosion voltage shutdown circuit and a probe immersion judgment circuit, and the preparation device of the nanometer probe controllable and large in length to diameter ratio can be used to prepare the nanometer probe which is large in length to diameter ratio, controllable in length to diameter ratio, recyclable and low in cost, and resists abrasion. The invention further provides a preparation method of the nanometer probe controllable and large in length to diameter ratio. The preparation method of the nanometer probe controllable and large in length to diameter ratio is characterized by not stopping corrosion after a probe is immersed into liquid of the prescribed depth, but continuing to lift the probe so as to form the novel nanometer probe which is large in length to diameter ratio and with a long needle tip of smoothly varying curvature radiuses, and has the remarkable advantages of being difficult to abrade, recyclable, low in use cost and the like. The preparation device of the nanometer probe controllable and large in length to diameter ratio improves accuracy and quality of the nanometer probe by automatically controlling the parameters of the corrosion voltage, the probe immersion depth, the probe lifting speed and the like. The preparation method of the nanometer probe controllable and large in length to diameter ratio is simple and reliable to operate.
Description
Technical field
The preparation facilities and the preparation method that the present invention relates to a kind of nano-probe, particularly a kind of preparation facilities of controlled big L/D ratio nano-probe and preparation method, belong to field of nanometer technology.
Background technology
At present, Development of Nano-technology is rapid, and current scientific and technological research, social production, daily life are had an immense impact on.Nano-probe is widely used in nanosecond science and technology field, such as scanning tunnel microscope, Measurement of Semiconductors instrument, nano-manipulation arm etc.The conventional nano-probe preparation method of prior art comprises that ultravacuum ion field microscope, grinding, shearing, field cause (static) transmitting, galvanic corrosion etc.Wherein, electrochemical erosion method is prepared feature reproducible, cheap, simple in structure and is obtained increasing favor with it.
Application for a patent for invention: " a kind of preparation method of tungsten nano-probe and application thereof ", application publication number: CN102721832A, Shen Qing Publication day: 2012.10.10, a kind of preparation method of nano-probe is disclosed, utilize single-chip microcomputer step motor axial displacement system to realize automatically mentioning of tungsten filament in corrosion process, by controlling immersion depth, mention speed and time and can prepare tungsten nano-probe, the probe making is produced to the micro-control system of MM3A nanometer for Kleindiek Nanotechnik company, carbon nano-tube has been carried out to brand-new nano-grade displacement, location and control survey.
But the galvanic corrosion of foregoing invention Patent Application Publication is prepared nano-probe method and is had obvious defect or deficiency:
The one, preparation method adopts first probe is immersed after corrosive liquid, first mention afterwards and be still in corrosive liquid and corrode, thereby nano-probe length-diameter ratio very little (file points out that length-diameter ratio is 3.7) and the needle point of preparation are very short, this nano-probe in actual applications, especially during as nano-manipulation arm, probe very easily weares and teares, and discarded after wearing and tearing, cannot recycling, use cost is higher.
The 2nd, although above-mentioned application has also provided the restriction that corrosion voltage, probe are mentioned the preparation parameter such as speed, mention time, but do not disclose the quantitative relationship of the length-diameter ratio of above-mentioned parameter and probe, selected numerical range is only chosen by rule of thumb, thereby can not be by the adjusting of above-mentioned preparation parameter, realize control to nano-probe length-diameter ratio, that is to say that the length-diameter ratio right and wrong of nano-probe of preparation are controlled.
The 3rd, probe is still in the curvature of corroding nano-probe in corrosive liquid to be changed and can not keep mild, continuously, affects the smooth contour of probe.
The 4th, the comparison control circuit being made up of elements such as voltage comparators is set, although also can realize the automatic cut-out of corrosion voltage, the probe that further control break is simultaneously cut off after corrosion voltage is mentioned speed, is unfavorable for the form optimization of probe tip.
The 5th, although also provided the control parameter of probe immersion depth, but the shift length that single-chip microcomputer only can control step motor, accurately position probe arrives the position (being the starting point of depth calculation) of corrosion liquid level, thereby affect the precision of controlling immersion depth, further affect length-diameter ratio and the form of probe.
Summary of the invention
For above defect or the Improvement requirement of prior art, first technical purpose of the present invention aims to provide a kind of preparation facilities of controlled big L/D ratio nano-probe, by the control circuits such as corrosion mu balanced circuit, corrosion voltage cut-out circuit, probe submergence decision circuitry are set, coordinate the accurate control realizing important parameters such as the corrosion voltage in corrosion process, probe submergence, probe pulling speeies with single-chip microcomputer, can prepare big L/D ratio, controlled length-diameter ratio, the nano-probe that wear-resistant, recyclable, cost is low, meet the needs of the different nano-probes of preparation.
Second technical purpose of the present invention aims to provide a kind of preparation method of controlled big L/D ratio nano-probe, employing probe immerses, no longer static corrosion after mentioning, but constantly mention probe after immersing always, thereby it is long to form needle point, needle point radius-of-curvature smooth change, the novel nano probe that length-diameter ratio is large, have not easy to wear, recyclable recycling, the low remarkable advantage that waits of use cost, and pass through corrosion voltage, probe submergence, mention the isoparametric automatic control of speed, improve precision and the quality of nano-probe, and operation is simple and reliable for preparation method.
The present invention is that the technical scheme that realizes technical purpose employing is:
A kind of preparation facilities of controlled big L/D ratio nano-probe, described device comprises mechanical displacement device, controller and control circuit, the fixing nano-probe of described mechanical displacement device also drives nano-probe to move up and down, described controller comprises host computer and single-chip microcomputer, described single-chip microcomputer is connected with mechanical displacement device and controls mechanical displacement device and move, described control circuit comprises the corrosion voltage stabilizing circuit being connected with single-chip microcomputer, corrosion voltage cuts off circuit and probe submergence decision circuitry, described corrosion voltage cuts off circuit and comprises the sampling resistor of series connection successively, voltage follower, scale operation circuit and voltage comparator, described sampling resistor is connected with open circuit potential, be used for gathering open circuit potential current value and be converted into magnitude of voltage, described voltage follower is used for following and is converted to judgement voltage, described scale operation circuit amplifies for judging voltage signal, described voltage comparator output terminal is connected with the IO mouth of single-chip microcomputer, described voltage comparator is for comparing judgement voltage and threshold voltage, in the time judging voltage lower than threshold voltage, voltage comparator output terminal becomes high level from low level, and level transitions signal is sent to single-chip microcomputer, described corrosion voltage stabilizing circuit receives the corrosion voltage signal instruction that single-chip microcomputer sends, and export default corrosion voltage and keep corrosion voltage constant according to instruction, whether described probe submergence decision circuitry detector probe immerses corrosion liquid level, and probe is immersed to signal be sent to single-chip microcomputer.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described corrosion voltage stabilizing circuit comprises voltage stabilizer and the digital varistor of series connection, the input end of described digital varistor is connected with the output terminal of single-chip microcomputer, the instruction that described digital varistor reception single-chip microcomputer sends also changes self-resistance value, makes voltage stabilizer export default corrosion voltage and keeps corrosion voltage constant.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described probe submergence decision circuitry comprises triode, the base stage of described triode is connected with open circuit potential, collector is connected with the input end of single-chip microcomputer, and described triode immerses when corrosive liquid conducting and sends probe to single-chip microcomputer at probe and immerses signal.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described mechanical displacement device comprises threephase asynchronous driver, threephase asynchronous, flexible coupling, bearing, ball-screw, hold-down nut, flexible hinge, support, mobile working plate and probe clamp, the input end of described threephase asynchronous driver connects single-chip microcomputer, output terminal connects threephase asynchronous, the main shaft of described threephase asynchronous is fixedly connected with the stiff end of ball-screw by flexible coupling, described ball-screw is fixed on support by bearing, on described ball-screw, be fixed with nut, described mobile working plate is fixedly connected with nut by flexible hinge, on described mobile working plate, be fixedly connected with probe clamp.
A preparation facilities for controlled big L/D ratio nano-probe, described bearing comprises and lays respectively at the upper end of ball-screw, head bearing and the lower bearing of lower end, and described head bearing is fixed bearing, and described lower bearing is swimming type bearing.
A preparation facilities for controlled big L/D ratio nano-probe, described probe clamp comprises row's pin and mother row, and described row's pin is fixed on mobile working plate, and probe is arranged on row mother.
A method of preparing controlled big L/D ratio nano-probe, comprises the following steps:
1) probe is installed and probe is carried out to cleaning treatment;
2) speed is mentioned in default thick corrosion voltage, essence corrosion voltage, probe submergence, the probe submergence of host computer input, speed is mentioned in probe disengaging;
3) Single-chip Controlling mechanical displacement device forward and drive probe decline, when probe contact corrosion liquid moment, probe submergence decision circuitry detects that probe immerses corrosive liquid and sends probe immersion signal to single-chip microcomputer, the thick corrosion of Single-chip Controlling corrosion voltage stabilizing circuit output voltage, probe starts thick corrosion;
4) probe immerses after corrosive liquid, Single-chip Controlling mechanical displacement device continues to move down, until probe arrives default submergence, then Single-chip Controlling mechanical displacement device oppositely rises, and drives probe to mention speed according to default probe submergence and upwards mentions probe;
5) when probe starts to corrode, the sampling resistor that corrosion voltage cuts off circuit starts to gather the current signal of open circuit potential and is converted into magnitude of voltage, after following amplification, voltage follower obtains judging voltage, after amplifying, scale operation circuit exports voltage comparator to again, voltage comparator will judge that voltage and default threshold voltage compare, in the time judging voltage lower than threshold voltage, voltage comparator output terminal becomes high level from low level, single-chip microcomputer is cut disconnected corrosion voltage immediately after this signal intensity being detected, corrosion process stops, Single-chip Controlling mechanical displacement device is mentioned speed according to probe disengaging and is upwards mentioned probe simultaneously, until stop during to tat probe initial position,
6) single-chip microcomputer is again controlled mechanical displacement device forward and is driven probe to decline, when probe contact corrosion liquid moment, probe submergence decision circuitry detect probe immerse corrosive liquid and to and to single-chip microcomputer send probe immerse signal, Single-chip Controlling corrosion voltage stabilizing circuit is exported default essence corrosion voltage, and probe starts essence corrosion;
7) repeating step 4)-5), complete probe preparation.
Prepare a method for controlled big L/D ratio nano-probe, described host computer is provided with Parameters Computing System, and described Parameters Computing System can be mentioned the 3rd value of any two value calculative determinations in speed according to corrosion voltage, probe submergence and probe submergence.
A kind of method of preparing controlled big L/D ratio nano-probe, first the calculation procedure of described Parameters Computing System comprises determines etching time according to the proportional relation of corrosion voltage and corrosion speed, then determine probe submergence according to length-diameter ratio and probe diameter, then determine that according to etching time and probe submergence probe submergence mentions speed.
Prepare a method for controlled big L/D ratio nano-probe, described thick corrosion voltage is 5～12V direct current, and described essence corrosion voltage is 2～5V direct current.
Prepare a method for controlled big L/D ratio nano-probe, described probe submergence is 1～10cm, and it is 0.01～10mm/min that speed is mentioned in described probe submergence.
Prepare a method for controlled big L/D ratio nano-probe, described probe disengaging is mentioned speed and is greater than 100mm/min.
Prepare a method for controlled big L/D ratio nano-probe, the reaction time that described corrosion voltage cuts off circuit is less than 100 μ s.
Compared with prior art, the beneficial effect that the present invention has is:
1, probe immerses after corrosive liquid and just ceaselessly slowly mentions probe, no longer allows probe static corrosion in corrosive liquid, has thereby form the novel nano probe that longer needle point section, needle point radius-of-curvature smooth change and length-diameter ratio are large.The length-diameter ratio of the probe of prior art is generally no more than 10, probe length-diameter ratio in documents is 3.7, and the length-diameter ratio of probe prepared by the present invention can reach 40-400, and needle point section is level and smooth, needle point is long, level and smooth needle point is wear-resistant, and because diameter changes slowly, after most advanced wearing and tearing, still can continue to use, the more important thing is, even after larger length-diameter ratio makes points wear, can also reclaim and carry out essence corrosion, the probe that obtains small curvature radius re-uses, and has significantly reduced use cost.
2, require to determine the corrosion depth of probe according to the length-diameter ratio of probe, and further according to corrosion depth and mention speed, the closed loop relation of corrosion between voltage, definite speed, the corrosion voltage of mentioning of accurate Calculation, and by the accurate control of corroding voltage, mentioning speed, obtain having the nano-probe that needs length-diameter ratio, realize the exact controllability of probe length-diameter ratio.
3, by corrosion voltage stabilizing circuit is set, ensure that in corrosion process, corroding voltage keeps constant, experimental results show that the present invention prepares the corrosion change in voltage of nano-probe device in corrosion process slowly and difference range within 0.1V, corrosion voltage is very constant, thereby the probe constant curvature making, form standard.
4, corrosion voltage is set and cuts off circuit, single-chip microcomputer receiver voltage variable signal, judges and controls cut-out corrosion voltage, controls threephase asynchronous and accelerate to mention probe disengaging corrosive liquid in cutting off corrosion voltage, is conducive to form more excellent needle point form.
5, probe submergence decision circuitry is set, moment at probe at contact corrosion liquid, turn-on transistor triggering level change, single-chip microcomputer detects level variable signal, determine probe start position, control probe and be submerged to predetermined depth in corrosive liquid, thereby reach the object of accurate control probe submergence.
6, adopt corrosion voltage 5-12V direct current slightly to corrode, 2-5V direct current carries out essence corrosion, and corrosion voltage particularly essence corrosion voltage is lower, and probe is difficult for passivation while departing from corrosion liquid level, avoids radius-of-curvature not reach requirement.
7, it is higher that speed is mentioned in the disengaging that probe is shaped after disengaging corrosive liquid, is generally the probe maximal velocity obtaining by experiment, and probe tip is difficult for being passivated, and is conducive to obtain the probe compared with small curvature radius.
8, adopt the micro-displacement apparatus being made up of structures such as three-dimensional asynchronous machine, ball-screw, flexible coupling, connection bearings, connection is reliable, displacement is accurate, easy to use.
9, nano-probe preparation facilities provided by the invention, by the setting of host computer, single-chip microcomputer and automatic control circuit, has realized the Automatic Control of probe preparation process, easy to operate, control precisely, automaticity is high.
Brief description of the drawings
Fig. 1 is the structural representation of the preparation facilities of controlled big L/D ratio nano-probe of the present invention.
Fig. 2 is the probe submergence decision circuitry of preparation facilities and the circuit diagram of corrosion voltage cut-out circuit of controlled big L/D ratio nano-probe of the present invention.
Fig. 3 is the circuit diagram of the corrosion voltage stabilizing circuit of controlled big L/D ratio nano-probe preparation facilities of the present invention.
Fig. 4 is controlled big L/D ratio nano-probe preparation method's of the present invention workflow diagram.
Fig. 5 is the structural representation of the nano-probe prepared of prior art.
Fig. 6 is the structural representation of the nano-probe prepared of the present invention.
In institute's drawings attached, identical Reference numeral is used for representing identical element or structure, wherein:
1-mechanical displacement device, 11-threephase asynchronous driver, 12-threephase asynchronous, 13-flexible coupling, 14-bearing, 15-ball-screw, 16-nut, 17-flexible hinge, 18-support, 19--mobile working plate, 20-probe clamp, 2-controller, 21-host computer, 22-single-chip microcomputer, 3-corrodes voltage stabilizing circuit, 31-voltage stabilizer, 32-digital varistor, 4-corrosion voltage cuts off circuit, 41-sampling resistor, 42-voltage follower, 43-scale operation circuit, 44-voltage comparator, 5-probe submergence circuit, 51-triode.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can combine mutually as long as do not form each other conflict.
Referring to Fig. 1, the preparation facilities of controlled big L/D ratio nano-probe provided by the invention, comprises mechanical displacement device 1, controller 2 and control circuit.Wherein, the fixing nano-probe of mechanical displacement device 1 also drives nano-probe to move up and down, and controller comprises host computer 21 and single-chip microcomputer 22, and single-chip microcomputer 22 is connected with mechanical displacement device 1 and controls mechanical displacement device and move.Control circuit comprises that the corrosion voltage stabilizing circuit 3, the corrosion voltage that are connected with single-chip microcomputer 22 cut off circuit 4 and probe submergence decision circuitry 5, wherein: the corrosion voltage signal instruction that corrosion voltage stabilizing circuit 3 sends for receiving single-chip microcomputer 22, and export default corrosion voltage and keep corrosion voltage constant according to instruction; Probe submergence decision circuitry 5 for detection of probe immerse, depart from corrosion liquid level, and by probe immerse signal, probe separating signal is sent to single-chip microcomputer 22.Corrosion voltage cuts off sampling resistor 41, voltage follower 42, scale operation circuit 43 and the voltage comparator 44 that circuit 4 comprises series connection successively.Wherein, sampling resistor 41 is for gathering open circuit potential current value and being converted into magnitude of voltage, voltage follower 42 is converted to judgement voltage for following, scale operation circuit 43 amplifies for judging voltage signal, voltage comparator 44 output terminals are connected with the IO mouth of single-chip microcomputer 22, voltage comparator 44 is for comparing judgement voltage and threshold voltage, in the time judging voltage lower than threshold voltage, voltage comparator 44 output terminals become high level from low level, and level transitions signal is sent to single-chip microcomputer 22.
When corrosion starts, corrosion voltage cut-out circuit 4 starts to gather the current signal of open circuit potential, obtains the voltage of open circuit potential electric current on sampling resistor, judges voltage.In the time that probe is near completion by disengaging liquid level, corrosion process, the resistance of whole open circuit potential sharply increases, cause corrosion current and judge that voltage also sharply reduces, judge that voltage is decreased to rapidly lower than threshold voltage, the output terminal of voltage comparator 44 becomes high level from low level, single-chip microcomputer 22 is cut disconnected corrosion voltage immediately after this signal intensity being detected, and corrosion process stops.Single-chip microcomputer 22 is controlled mechanical displacement device 1 and is accelerated upwards to mention probe disengaging corrosive liquid according to probe second cosmic velocity simultaneously.Cut off the setting of circuit 4 by corrosion, can accurately control stopping of corrosion process, and in stopping, mentioning fast probe, be conducive to form better probe tip form.
The preparation facilities of controlled big L/D ratio nano-probe provided by the invention, corrosion voltage stabilizing circuit 3 comprises voltage stabilizer 31 and the digital varistor 32 of series connection, the preferred switching mode integrated regulator of voltage stabilizer 31, the input end of digital varistor 32 is connected with the output terminal of single-chip microcomputer 22, digital varistor 32 receives the instruction that single-chip microcomputer 22 sends and changes self-resistance value, makes voltage stabilizer 31 export default corrosion voltage and keeps corrosion voltage constant.The corrosion magnitude of voltage that single-chip microcomputer 22 instructions obtain presetting from host computer 21 calculates the resistance of digital varistor 32.
The preparation facilities of controlled big L/D ratio nano-probe provided by the invention, probe submergence decision circuitry 5 comprises triode 51, and the base stage of triode 51 is connected with open circuit potential, and collector is connected with the input end of single-chip microcomputer 22.Triode 51 immerses when corrosive liquid conducting and sends probe to single-chip microcomputer 22 at probe and immerses signal.When use, probe is in the moment of contact corrosion liquid, the base stage of triode 51 has electric current to pass through, triode 51 conductings, P2.2 mouth transfers low level state to by original high level state, and single-chip microcomputer 22 detects after the variation of level, taking probe herein position as basic point, control mechanical displacement device 1 and make probe to mobile respective distance again in corrosive liquid, thereby reach the object of accurate control probe submergence.
The preparation facilities of controlled big L/D ratio nano-probe provided by the invention, mechanical displacement device 1 comprises threephase asynchronous driver 11, threephase asynchronous 12, flexible coupling 13, bearing 14, ball-screw 15, hold-down nut 16, flexible hinge 17, support 18, mobile working plate 19 and probe clamp 20.Wherein, the input end of threephase asynchronous driver 11 connects single-chip microcomputer 22, and output terminal connects threephase asynchronous 12, and threephase asynchronous driver is used for receiving the instruction that single-chip microcomputer 22 sends, and turns round according to order-driven threephase asynchronous 12.The main shaft of threephase asynchronous 12 is fixedly connected with the stiff end of ball-screw 15 by flexible coupling 13, and ball-screw 15 is fixed on support 18 by bearing 14.On ball-screw 15, be fixed with nut 16, mobile working plate 19 is fixedly connected with nut 16 by flexible hinge 17, is fixedly connected with probe clamp 20 on mobile working plate 19.When use, under the instruction of single-chip microcomputer 22, threephase asynchronous driver 11 is controlled threephase asynchronous 12 and is rotated, threephase asynchronous 12 drives ball-screw 15 to rotate by flexible coupling 13, along the axial rectilinear motion of ball-screw, and drive mobile working plate 19, probe clamp 20 and probe along the axial moving linearly of ball-screw with the nut 16 of ball-screw 15 interlocks.
The preparation facilities of controlled big L/D ratio nano-probe provided by the invention, preferably the bearing of mechanical displacement device 14 is made as to head bearing and lower bearing, lay respectively at the top and bottom of ball-screw 15, it is fixed bearing that head bearing is preferably set, and lower bearing is swimming type bearing.
The preparation facilities of controlled big L/D ratio nano-probe provided by the invention, probe clamp 20 row's of employing pins and row's parent structure, row's pin is fixed on mobile working plate 19, and probe is arranged on row mother.The row's of employing faller gill parent structure is installed stationary probe, not only can realize conduction connection but also facilitate mounting or dismounting, and the acting force being subject in corrosion process due to probe is very little, this kind of connection be enough firm stable also, reliably realize the round rectilinear motion of probe in the vertical direction.
The preparation method of a kind of controlled big L/D ratio nano-probe provided by the invention, comprises the following steps:
1) probe is installed, probe is carried out to cleaning treatment, the preferred sonic oscillation of cleaning treatment cleans;
2) speed is mentioned in default thick corrosion voltage, essence corrosion voltage, probe submergence, the probe submergence of host computer 21 inputs, speed is mentioned in probe disengaging;
3) single-chip microcomputer 22 is controlled mechanical displacement device 1 forward and is driven probe to decline, when probe contact corrosion liquid moment, probe submergence decision circuitry 5 detects that probe immerses corrosive liquid and sends probe immersion signal to single-chip microcomputer 22, single-chip microcomputer 22 is controlled the thick corrosion of corrosion voltage stabilizing circuit 3 output voltage, and probe starts thick corrosion;
4) when probe immerses after corrosive liquid, single-chip microcomputer 22 is controlled mechanical displacement device 1 and is continued to move down, until probe arrives default submergence, then single-chip microcomputer 22 is controlled mechanical displacement device 1 and is reversed, and drives probe to mention speed according to default probe submergence and upwards mentions probe;
5) when probe starts to corrode, the sampling resistor 41 that corrosion voltage cuts off circuit 4 starts to gather the current signal of open circuit potential and is converted into magnitude of voltage, after following amplification, voltage follower 42 obtains judging voltage, after amplifying, scale operation circuit 43 exports voltage comparator 44 to again, voltage comparator 44 will judge that voltage and default threshold voltage compare, in the time judging voltage lower than threshold voltage, voltage comparator output terminal becomes high level from low level, single-chip microcomputer 22 is cut disconnected corrosion voltage immediately after this signal intensity being detected, corrosion process stops, simultaneously single-chip microcomputer 22 is controlled mechanical displacement device 1 and is departed from and mention speed and upwards mention probe according to probe, until stop during to tat probe initial position, probe initial position is generally positioned at the above 5cm of liquid level left and right,
6) single-chip microcomputer 22 is again controlled mechanical displacement device 1 forward and is driven probe to decline, when probe contact corrosion liquid moment, probe submergence decision circuitry 5 detects that probe immerses corrosive liquid and sends probe immersion signal to single-chip microcomputer 22, single-chip microcomputer 22 is controlled corrosion voltage stabilizing circuit 3 and is exported default essence corrosion voltage, and probe starts essence corrosion;
7) repeating step 4)-5), complete probe preparation.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, slightly corroding voltage preferable range is 5～12V direct current, essence corrosion voltage preferable range is 2～5V direct current.From electrochemical kinetics theory, corrosion voltage is larger, and corrosion rate is higher, corrodes the time used shorter, but corrodes voltage when excessive, probe easy passivation in the time departing from corrosion liquid level, and needle point radius-of-curvature does not reach requirement.Therefore, that the present invention adopts is thick, the method for smart twice corrosion, and corrosion voltage particularly essence corrosion voltage is less, and probe is difficult for passivation while departing from corrosion liquid level, makes probe tip radius-of-curvature reach requirement.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, can be according to the quantitative relationship between corrosion voltage, immersion depth and corrosion ascending velocity (being that speed is mentioned in probe submergence), determine and meet the relevant preparation parameter that probe length-diameter ratio requires, realize the exact controllability of preparing nano-probe length-diameter ratio.
From electrochemical kinetics theory, in the situation that corrosive liquid concentration is certain, corrosion voltage is directly proportional to probe corrosion rate, so for the certain probe of diameter, needed etching time is also directly proportional to corrosion voltage, this direct ratio numerical relation can obtain by testing specifically, thereby can determine etching time according to corrosion voltage.Defined from length-diameter ratio, length-diameter ratio equals probe submergence divided by probe diameter, therefore can determine probe submergence by probe diameter and length-diameter ratio, then according to definite etching time, further speed is mentioned in definite probe submergence.The preparation method of controlled length-diameter ratio nano-probe provided by the invention, can adopt input corrosion voltage, corrosion depth and probe submergence to mention any two values in speed, by aforementioned another value of quantitative relationship calculative determination.Preferably, select to host computer 21 input corrosion voltage and corrosion depths, speed is mentioned in the submergence of calculative determination probe.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, mention the quantitative relationship between speed according to above-mentioned corrosion voltage, etching time, submergence and probe submergence, and definite corrosion voltage, probe diameter and length-diameter ratio, it is 1～10cm that probe submergence scope is preferably set, further according to etching time, can determine that probe submergence mentions speed preferable range 0.01～10mm/min.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, preferred pin arranges probe and departs from and mention speed and be greater than 100mm/min.The ascending velocity that probe is shaped after disengaging corrosive liquid is to depart from mentions speed, and it is faster that speed is mentioned in disengaging, and probe tip is more difficult for being passivated, and radius-of-curvature is just less.Probe departs from mentions the probe maximal velocity 100mm/min that speed preferably obtains by experiment.Probe departs from and mentions speed and also can be set voluntarily by user, and as without setting, controller default setting is probe maximal velocity.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, the reaction time that corrosion voltage cut-out circuit 4 is preferably set is less than 100 μ s.The reaction time of corrosion voltage cut-out circuit is shorter, and probe is more not easy passivation, and tip curvature radius is less, and the reaction time is mainly determined by the reaction time of voltage comparator 44, the reaction time of voltage stabilizer 31.
The preparation method of controlled big L/D ratio nano-probe provided by the invention, single-chip microcomputer 22 is also provided with timing software, described step 5) also comprise that, in the time that probe drops to default submergence, etching time timing starts, in the time that probe rises to disengaging corrosive liquid, etching time timing stops.Timing software is set on single-chip microcomputer 22, can in probe corrosion experiment, record the corrosion time used, to obtain corroding required time and the proportional relation that corrodes voltage, to determine etching time according to corrosion voltage in the time formally preparing nano-probe, and further the important parameters such as speed are mentioned in definite submergence.
Adopt the difference of the prepared nano-probe of nano-probe preparation facilities of the present invention and preparation method and the prepared probe of documents, referring to Fig. 5 and Fig. 6.Fig. 5 is the structural representation of the nano-probe prepared of prior art, probe has obvious needle point section (diameter of needle point Duan Yufei needle point section has larger gap), needle point segment length is very short, probe length-diameter ratio very little (instructions points out that the length-diameter ratio of probe is 3.7).Fig. 6 is the nano-probe that adopts preparation facilities of the present invention and preparation method to make, probe does not have obvious needle point section (diameter of needle point Duan Yufei needle point section does not have variation suddenly), it is mild, continuous that the curvature of needle point changes, thereby whole probe can be served as needle point section, the length-diameter ratio of probe can reach 40-400, far away higher than 3.7 of documents, and variation range is large.The probe of documents is because needle point is short, length-diameter ratio is little, and needle point is very easy to wearing and tearing, and can not re-use after tip wear.And probe tip of the present invention is long, length-diameter ratio is large, can reach 40-400, this probe is first not easy to wear in the time of nanometer manipulation, secondly after most advanced wearing and tearing because its diameter changes slowly, can continue to use, finally when may wear to can not use time, can reclaim the probe continuation use of carrying out essence corrosion and obtain minor radius, significantly reduce the use cost of probe.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the preparation facilities of a controlled big L/D ratio nano-probe, it is characterized in that: described device comprises mechanical displacement device (1), controller (2) and control circuit, the fixing nano-probe of described mechanical displacement device (1) also drives nano-probe to move up and down, described controller comprises host computer (21) and single-chip microcomputer (22), described single-chip microcomputer (22) is connected with mechanical displacement device (1) and controls mechanical displacement device (1) and move, described control circuit comprises the corrosion voltage stabilizing circuit (3) being connected with single-chip microcomputer (22), corrosion voltage cuts off circuit (4) and probe submergence decision circuitry (5),
Described corrosion voltage cuts off sampling resistor (41), voltage follower (42), scale operation circuit (43) and the voltage comparator (44) that circuit (4) comprises series connection successively, described sampling resistor (41) is connected with open circuit potential, be used for gathering open circuit potential current value and be converted into magnitude of voltage, described voltage follower (42) is converted to judgement voltage for following, and described scale operation circuit (43) amplifies for judging voltage signal; Described voltage comparator (44) output terminal is connected with the IO mouth of single-chip microcomputer (22), described voltage comparator (44) is for comparing judgement voltage and threshold voltage, in the time judging voltage lower than threshold voltage, voltage comparator (44) output terminal becomes high level from low level, and level transitions signal is sent to single-chip microcomputer (22);
Described corrosion voltage stabilizing circuit (3) receives the corrosion voltage signal instruction that single-chip microcomputer (22) sends, and exports default corrosion voltage and keep corrosion voltage constant according to instruction;
Described probe submergence decision circuitry (5) detector probe immerses corrosion liquid level, and probe is immersed to signal is sent to single-chip microcomputer (22).
2. the preparation facilities of a kind of controlled big L/D ratio nano-probe according to claim 1, it is characterized in that: described corrosion voltage stabilizing circuit (3) comprises voltage stabilizer (31) and the digital varistor (32) of series connection, the input end of described digital varistor (32) is connected with the output terminal of single-chip microcomputer (22), the instruction that described digital varistor (32) reception single-chip microcomputer (22) sends also changes self-resistance value, makes voltage stabilizer (31) export default corrosion voltage and keeps corrosion voltage constant.
3. the preparation facilities of a kind of controlled big L/D ratio nano-probe according to claim 1, it is characterized in that: described probe submergence decision circuitry (5) comprises triode (51), the base stage of described triode (51) is connected with open circuit potential, collector is connected with the input end of single-chip microcomputer (22), and described triode (51) immerses when corrosive liquid conducting and sends probe to single-chip microcomputer (22) at probe and immerses signal.
4. the preparation facilities of a kind of controlled big L/D ratio nano-probe according to claim 1, it is characterized in that: described mechanical displacement device (1) comprises threephase asynchronous driver (11), threephase asynchronous (12), flexible coupling (13), bearing (14), ball-screw (15), hold-down nut (16), flexible hinge (17), support (18), mobile working plate (19) and probe clamp (20), the input end of described threephase asynchronous driver (11) connects single-chip microcomputer (22), output terminal connects threephase asynchronous (12), the main shaft of described threephase asynchronous (12) is fixedly connected with the stiff end of ball-screw (15) by flexible coupling (13), described ball-screw (15) is fixed on support (18) by bearing (14), on described ball-screw (15), be fixed with nut (16), described mobile working plate (19) is fixedly connected with nut (16) by flexible hinge (17), on described mobile working plate (19), be fixedly connected with probe clamp (20).
5. the preparation facilities of a kind of controlled big L/D ratio nano-probe according to claim 4, it is characterized in that: described bearing (14) comprises and lays respectively at the upper end of ball-screw (15), head bearing and the lower bearing of lower end, described head bearing is fixed bearing, and described lower bearing is swimming type bearing.
6. the preparation facilities of a kind of controlled big L/D ratio nano-probe according to claim 4, it is characterized in that: described probe clamp (20) comprises row's pin and mother row, it is upper that described row's pin is fixed on mobile working plate (19), and probe is arranged on row mother.
7. adopt nano-probe preparation facilities as claimed in claim 1 to prepare a method for controlled big L/D ratio nano-probe, it is characterized in that comprising the following steps:
1) probe is installed and probe is carried out to cleaning treatment;
2) speed is mentioned in default thick corrosion voltage, essence corrosion voltage, probe submergence, the probe submergence of host computer (21) input, speed is mentioned in probe disengaging;
3) single-chip microcomputer (22) is controlled mechanical displacement device 1 forward and is driven probe to decline, when probe contact corrosion liquid moment, probe submergence decision circuitry (5) detects that probe immerses corrosive liquid, and send probe immersion signal to single-chip microcomputer (22), single-chip microcomputer (22) is controlled the thick corrosion of corrosion voltage stabilizing circuit (3) output voltage, and probe starts thick corrosion;
4) probe immerses after corrosive liquid, single-chip microcomputer (22) is controlled mechanical displacement device 1 and is continued to move down, until probe arrives default submergence, then single-chip microcomputer (22) mechanical displacement device 1 oppositely rises, and drives probe to mention speed according to default probe submergence and upwards mentions probe;
5) when probe starts to corrode, the sampling resistor (41) that corrosion voltage cuts off circuit (4) starts to gather the current signal of open circuit potential and is converted into magnitude of voltage, after following amplification, voltage follower (42) obtains judging voltage, after amplifying, scale operation circuit (43) exports voltage comparator (44) to again, voltage comparator (44) will judge that voltage and default threshold voltage compare, in the time judging voltage lower than threshold voltage, voltage comparator output terminal becomes high level from low level, single-chip microcomputer (22) detects after this signal intensity disconnected corrosion voltage immediately, corrosion process stops, single-chip microcomputer (22) control mechanical displacement device (1) is mentioned speed according to probe disengaging and is upwards mentioned probe simultaneously, until stop during to tat probe initial position,
6) single-chip microcomputer (22) is again controlled mechanical displacement device 1 forward and is driven probe to decline, when probe contact corrosion liquid moment, probe submergence decision circuitry (5) detect probe immerse corrosive liquid and to and to single-chip microcomputer (22) send probe immerse signal, single-chip microcomputer (22) is controlled corrosion voltage stabilizing circuit (3) and is exported default essence corrosion voltage, and probe starts essence corrosion;
7) repeating step 4)-5), complete probe preparation.
8. the preparation method of a kind of controlled big L/D ratio nano-probe according to claim 7, it is characterized in that: described host computer (21) is provided with Parameters Computing System, described Parameters Computing System can be mentioned the 3rd value of any two value calculative determinations in speed according to corrosion voltage, probe submergence and probe submergence.
9. the preparation method of a kind of controlled big L/D ratio nano-probe according to claim 8, it is characterized in that: first the calculation procedure of described Parameters Computing System comprises determines etching time according to the proportional relation of corrosion voltage and corrosion speed, then determine probe submergence according to length-diameter ratio and probe diameter, then determine that according to etching time and probe submergence probe submergence mentions speed.
10. the preparation method of a kind of controlled big L/D ratio nano-probe according to claim 7, is characterized in that: described thick corrosion voltage is 5～12V direct current, and described essence corrosion voltage is 2～5V direct current.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785871A (en) * | 2015-04-17 | 2015-07-22 | 清华大学深圳研究生院 | Probe manufacturing method and device |
| CN105239148A (en) * | 2015-11-17 | 2016-01-13 | 襄阳宏伟航空器有限责任公司 | Probe machining equipment |
| 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 |
| 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 |
| CN109844545A (en) * | 2016-08-12 | 2019-06-04 | 提普泰克有限责任公司 | Scan probe and electron microscope probe and its manufacture |
| CN110514877A (en) * | 2019-08-30 | 2019-11-29 | 西安交通大学 | A kind of assemble method of big L/D ratio probe |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000065712A (en) * | 1998-08-20 | 2000-03-03 | Japan Science & Technology Corp | Method for manufacturing silver probe of scanning tunnel microscope |
| US20020063066A1 (en) * | 2000-11-28 | 2002-05-30 | Ahn Hyo Sok | Wire etching device and method |
| US20060075626A1 (en) * | 2004-10-09 | 2006-04-13 | Academia Sinica | Single-atom tip and preparation method thereof |
| CN101118789A (en) * | 2007-07-31 | 2008-02-06 | 厦门大学 | Method for manufacturing platinum-iridium needlepoint and device thereof |
| CN102721832A (en) * | 2012-06-25 | 2012-10-10 | 天津大学 | Preparation method and application of metal tungsten nano-probe |
| CN204028107U (en) * | 2014-07-10 | 2014-12-17 | 华中科技大学 | A kind of preparation facilities of controlled big L/D ratio nano-probe |
-
2014
- 2014-07-10 CN CN201410329359.3A patent/CN104101738B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000065712A (en) * | 1998-08-20 | 2000-03-03 | Japan Science & Technology Corp | Method for manufacturing silver probe of scanning tunnel microscope |
| US20020063066A1 (en) * | 2000-11-28 | 2002-05-30 | Ahn Hyo Sok | Wire etching device and method |
| US20060075626A1 (en) * | 2004-10-09 | 2006-04-13 | Academia Sinica | Single-atom tip and preparation method thereof |
| CN101118789A (en) * | 2007-07-31 | 2008-02-06 | 厦门大学 | Method for manufacturing platinum-iridium needlepoint and device thereof |
| CN102721832A (en) * | 2012-06-25 | 2012-10-10 | 天津大学 | Preparation method and application of metal tungsten nano-probe |
| CN204028107U (en) * | 2014-07-10 | 2014-12-17 | 华中科技大学 | A kind of preparation facilities of controlled big L/D ratio nano-probe |
Non-Patent Citations (2)
| Title |
|---|
| 杨永斌等: "制备扫描近场光学显微镜光纤探针的自动化腐蚀方法", 《光子学报》 * |
| 王玉光: "PSTM光纤探针腐蚀***的研制", 《信息工程大学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104785871A (en) * | 2015-04-17 | 2015-07-22 | 清华大学深圳研究生院 | Probe manufacturing method and device |
| CN105239148A (en) * | 2015-11-17 | 2016-01-13 | 襄阳宏伟航空器有限责任公司 | Probe machining equipment |
| 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 |
| CN109844545A (en) * | 2016-08-12 | 2019-06-04 | 提普泰克有限责任公司 | Scan probe and electron microscope probe and its manufacture |
| 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 |
| CN110514877A (en) * | 2019-08-30 | 2019-11-29 | 西安交通大学 | A kind of assemble method of big L/D ratio probe |
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|---|---|
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