CN104101738B - The preparation facilities of a kind of controlled big L/D ratio nano-probe and preparation method - Google Patents
The preparation facilities of a kind of controlled big L/D ratio nano-probe and preparation method Download PDFInfo
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Abstract
The present invention provides the preparation facilities of a kind of controlled big L/D ratio nano-probe, by arranging corrosion mu balanced circuit, corrosion potentials cuts off circuit, probe submergence decision circuitry, coordinate with single-chip microcomputer and realize the corrosion potentials in corrosion process, probe submergence, probe are promoted the accurate of the important parameters such as speed and controlled, it is possible to prepare big L/D ratio, controlled draw ratio, wear-resistant, recyclable, the nano-probe of low cost.The present invention also provides for the preparation method of a kind of controlled big L/D ratio nano-probe, probe is used no longer to stop corrosion after immersing designated depth, but the most constantly mention probe, thus form needle point length, needle point radius of curvature smooth change, novel nano probe that draw ratio is big, there is the remarkable advantages such as recycling the most easy to wear, recyclable, use cost be low, and by corrosion potentials, probe submergence, mention that speed is isoparametric to be automatically controlled, improve the precision of nano-probe and quality, and preparation method operation is simple and reliable.
Description
Technical field
The present invention relates to preparation facilities and the preparation method of a kind of nano-probe, particularly to preparation facilities and the preparation method of a kind of controlled big L/D ratio nano-probe, belong to field of nanometer technology.
Background technology
At present, Development of Nano-technology is rapid, and has an immense impact on current Technological research, social production, daily life.Nano-probe is widely used in nanosecond science and technology field, such as PSTM, Measurement of Semiconductors instrument, nano-manipulation arm etc..The conventional nano-probe preparation method of prior art include ultravacuum ion field microscope, grind, shear, field causes (electrostatic) transmitting, electrochemical corrosion etc..Wherein, electrochemical erosion method is prepared reproducible, cheap, the feature of simple in construction with it and is obtained increasing favor.
Application for a patent for invention: " preparation method and applications of a kind of metal tungsten nano-probe ", application publication number: CN102721832A, Shen Qing Publication day: 2012.10.10, disclose the preparation method of a kind of nano-probe, the axial displacement system of single-chip microcomputer stepper motor is utilized to realize automatically mentioning of tungsten filament in corrosion process, by controlling immersion depth, mention speed and the time can prepare tungsten nano-probe, prepared probe is used for Kleindiek Nanotechnik company and produces the micro-steerable system of MM3A nanometer, CNT has been carried out brand-new nano-grade displacement, location and control are measured.
But, the electrochemical corrosion of foregoing invention patent application publication is prepared nano-probe method and be there is obvious defect or deficiency:
One is after probe is first immersed corrosive liquid by preparation method employing, first mention to be still in corrosive liquid afterwards and corrode, thus the nano-probe draw ratio the least (file points out that draw ratio is 3.7) of preparation and needle point are the shortest, this nano-probe is in actual applications, easily wear and tear especially as probe during nano-manipulation arm, and discarded after Mo Sun, it is impossible to recycling, use cost is higher.
Although two is that above-mentioned application give also corrosion potentials, the restriction of the preparation parameter such as speed, mention time mentioned by probe, but do not disclose the quantitative relationship of above-mentioned parameter and the draw ratio of probe, selected numerical range is chosen the most by rule of thumb, thus can not be by the regulation of above-mentioned preparation parameter, realize the control to nano-probe draw ratio, that is to say that the draw ratio of the nano-probe of preparation is non-controllable.
Three is that probe is still in corrosive liquid and corrodes the Curvature varying of nano-probe and can not keep mild, continuous, affects the smooth contour of probe.
Four is to arrange the comparison control circuit that is made up of elements such as voltage comparators, although also can realize automatically cutting off of corrosion potentials, but cannot mention speed by the probe after corrosion potentials is cut off in control break simultaneously further, is unfavorable for the form optimization of probe tip.
Although five is the control parameter that give also probe immersion depth, but single-chip microcomputer is only capable of controlling the shift length of motor, probe can not be accurately positioned and arrive the position (i.e. the starting point of depth calculation) of corrosion liquid level, thus impact controls the precision of immersion depth, affect draw ratio and the form of probe further.
Summary of the invention
Disadvantages described above or Improvement requirement for prior art, first technical purpose of the present invention aims to provide the preparation facilities of a kind of controlled big L/D ratio nano-probe, by arranging corrosion mu balanced circuit, corrosion potentials cuts off the control circuit such as circuit, probe submergence decision circuitry, coordinate with single-chip microcomputer and realize the corrosion potentials in corrosion process, probe submergence, probe are promoted the accurate of the important parameters such as speed and controlled, big L/D ratio, controlled draw ratio, wear-resistant, recyclable, the nano-probe of low cost can be prepared, meet the needs of the different nano-probe of preparation.
Second technical purpose of the present invention aims to provide the preparation method of a kind of controlled big L/D ratio nano-probe, use probe immerse, mention after the most static corrosion, but the most constantly mention probe after immersing, thus form needle point length, needle point radius of curvature smooth change, novel nano probe that draw ratio is big, there is the remarkable advantages such as recycling the most easy to wear, recyclable, use cost be low, and by corrosion potentials, probe submergence, mention that speed is isoparametric to be automatically controlled, improve the precision of nano-probe and quality, and preparation method operation is simple and reliable.
The present invention is that the technical scheme realizing technical purpose employing is:
nullA kind of preparation facilities of controlled big L/D ratio nano-probe，Described device includes mechanical displacement device、Control machine and control circuit，Described mechanical displacement device is fixed nano-probe and drives nano-probe to move up and down，Described control machine includes host computer and single-chip microcomputer，Described single-chip microcomputer is connected with mechanical displacement device and controls mechanical displacement device and moves，Described control circuit includes the corrosion potentials mu balanced circuit being connected with single-chip microcomputer、Corrosion potentials cuts off circuit and probe submergence decision circuitry，Described corrosion potentials cuts off the sampling resistor that circuit includes being sequentially connected in series、Voltage follower、Scaling circuit and voltage comparator，Described sampling resistor is connected with open circuit potential，For gathering open circuit potential current value and being converted into magnitude of voltage，Described voltage follower is used for following and is converted to judge voltage，Described scaling circuit is used for will determine that voltage signal amplifies，Described voltage comparator outfan is connected with the I/O port of single-chip microcomputer，Described voltage comparator is used for will determine that voltage compares with threshold voltage，When judging voltage less than threshold voltage，Voltage comparator outfan is become high level from low level，And level transitions signal is sent to single-chip microcomputer，Described corrosion potentials mu balanced circuit receives the corrosion potentials signal instruction that single-chip microcomputer sends，And according to instructing the default corrosion potentials of output and keeping corrosion potentials constant，Whether described probe submergence decision circuitry detection probe immerses corrosion liquid level，And probe is immersed signal transmission to single-chip microcomputer.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described corrosion potentials mu balanced circuit includes manostat and the digital varistor of series connection, the input of described digital varistor is connected with the outfan of single-chip microcomputer, described digital varistor receives the instruction that sends of single-chip microcomputer and changes self-resistance value, makes corrosion potentials that manostat output presets and keeps corrosion potentials constant.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described probe submergence decision circuitry includes audion, the base stage of described audion is connected with open circuit potential, colelctor electrode is connected with the input of single-chip microcomputer, and described audion turns on when probe immerses corrosive liquid and sends probe to single-chip microcomputer and immerses signal.
A kind of preparation facilities of controlled big L/D ratio nano-probe, described mechanical displacement device includes threephase asynchronous driver, threephase asynchronous, flexible coupling, bearing, ball-screw, fixing nut, flexible hinge, support, mobile working plate and probe clamp, the input of described threephase asynchronous driver connects single-chip microcomputer, outfan connects threephase asynchronous, the main shaft of described threephase asynchronous is connected by flexible coupling is fixing with the fixing end of ball-screw, described ball-screw is fixed on support by bearing, it is fixed with nut on described ball-screw, described mobile working plate is connected by flexible hinge and nut are fixing, linking probe fixture is fixed on described mobile working plate.
The preparation facilities of a kind of controlled big L/D ratio nano-probe, described bearing includes laying respectively at the upper end of ball-screw, the upper bearing (metal) of lower end and lower bearing, and described upper bearing (metal) is fixed bearing, and described lower bearing is swimming type bearing.
The preparation facilities of a kind of controlled big L/D ratio nano-probe, described probe clamp includes pricking with needle and mother row, and described pricking with needle is fixed on mobile working plate, and probe is arranged on row mother.
A kind of method preparing controlled big L/D ratio nano-probe, comprises the following steps:
1) probe is installed and is carried out probe processing；
2) host computer inputs the thick corrosion potentials preset, smart corrosion potentials, probe submergence, speed is mentioned in probe submergence, speed is mentioned in probe disengaging；
3) Single-chip Controlling mechanical displacement device rotates forward and drives probe to 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, Single-chip Controlling corrosion potentials mu balanced circuit exports thick corrosion potentials, and probe starts slightly to corrode；
4) after probe immerses corrosive liquid, Single-chip Controlling mechanical displacement device continues to move down, until probe arrives the submergence preset, then Single-chip Controlling mechanical displacement device reversely rises, and drives probe to mention speed according to default probe submergence and is lifted up probe；
5) when probe starts to corrode, corrosion potentials cuts off the sampling resistor of circuit to start gather the current signal of open circuit potential and be converted into magnitude of voltage, obtain judging voltage after amplification followed by voltage follower, export to voltage comparator after scaling circuit amplifies again, voltage comparator will determine that voltage compares with the threshold voltage preset, when judging voltage less than threshold voltage, voltage comparator outfan is become high level from low level, single-chip microcomputer detects that this signal intensity rear cutout is broken corrosion potentials immediately, corrosion process stops, Single-chip Controlling mechanical displacement device departs from according to probe and mentions speed and be lifted up probe simultaneously, until stopping to during tat probe initial position；
6) single-chip microcomputer again controls mechanical displacement device and rotates forward and drive probe to 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 smart corrosion potentials that the output of Single-chip Controlling corrosion potentials mu balanced circuit is preset, probe starts essence corrosion；
7) step 4 is repeated)-5), complete probe and prepare.
A kind of method preparing controlled big L/D ratio nano-probe, described host computer is provided with Parameters Computing System, and described Parameters Computing System can determine the 3rd value according to any two value calculating that corrosion potentials, probe submergence and probe submergence are mentioned in speed.
A kind of method preparing controlled big L/D ratio nano-probe, the calculation procedure of described Parameters Computing System includes first determining etching time according to the proportional relation of corrosion potentials and corrosion rate, then determine probe submergence according to draw ratio and probe diameter, determine that speed is mentioned in probe submergence further according to etching time and probe submergence.
A kind of method preparing controlled big L/D ratio nano-probe, described thick corrosion potentials is 5～12V unidirectional currents, and described essence corrosion potentials is 2～5V unidirectional currents.
A kind of method preparing 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.
A kind of method preparing controlled big L/D ratio nano-probe, described probe departs from mentions speed more than 100mm/min.
A kind of method preparing controlled big L/D ratio nano-probe, described corrosion potentials cuts off the response time of circuit less than 100 μ s.
Compared with prior art, the device have the advantages that into:
1, probe immerses after corrosive liquid and the most slowly mentions probe, no longer allows probe static corrosion in corrosive liquid, thus is formed and have the novel nano probe that longer needle point section, needle point radius of curvature smooth change and draw ratio is big.The draw ratio of the probe of prior art is usually no more than 10, probe draw ratio in documents is 3.7, and the draw ratio of probe prepared by the present invention can reach 40-400, and needle point section is smooth, needle point is long, smooth needle point is wear-resistant, and due to diameter change slowly, still can be continuing with after most advanced abrasion, the more important thing is, even if after bigger draw ratio makes points wear, can also reclaim and carry out essence corrosion, it is thus achieved that the probe of little radius of curvature re-uses, and significantly reduces use cost.
2, require to determine the corrosion depth of probe according to the draw ratio of probe, and further according to corrosion depth and the closed loop relation mentioned between speed, corrosion potentials, accurate calculating determines mentions speed, corrosion potentials, and pass through corrosion potentials, mention being precisely controlled of speed, obtain that there is the nano-probe needing draw ratio, it is achieved the exact controllability of probe draw ratio.
3, by arranging corrosion potentials mu balanced circuit, ensure that in corrosion process, corrosion potentials keeps constant, experiment proves the present invention to prepare the corrosion potentials change in corrosion process of the nano-probe device, and slowly and difference range is within 0.1V, corrosion potentials is the most constant, thus the probe constant curvature prepared, morphologic criteria.
4, corrosion potentials is set and cuts off circuit, single-chip microcomputer reception voltage change signal, it is judged that and control to cut off corrosion potentials, while cutting off corrosion potentials, control threephase asynchronous accelerate to mention probe disengaging corrosive liquid, advantageously form more excellent needle point form.
5, probe submergence decision circuitry is set, at probe in moment of 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 desired depth in corrosive liquid, thus reach accurately to control the purpose of probe submergence.
6, using corrosion potentials 5-12V unidirectional current slightly to corrode, 2-5V unidirectional current carries out essence corrosion, and corrosion potentials particularly essence corrosion potentials is relatively low, and probe is difficult to passivation when departing from corrosion liquid level, it is to avoid radius of curvature does not reaches requirement.
7, it is higher that speed is mentioned in the disengaging after probe shapes disengaging corrosive liquid, and the probe maximal velocity generally obtained by experiment, probe tip is difficult to be passivated, and is conducive to obtaining the probe of less radius of curvature.
8, using 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, the nano-probe preparation facilities that the present invention provides, by host computer, single-chip microcomputer and the setting of automatic control circuit, it is achieved that the Automatic Control of probe preparation process, easy to operate, control precisely, automaticity high.
Accompanying drawing explanation
Fig. 1 is the structural representation of the preparation facilities of the controlled big L/D ratio nano-probe of the present invention.
Fig. 2 is the workflow diagram of the controlled big L/D ratio nano-probe preparation method of the present invention.
Fig. 3 is probe submergence decision circuitry and the circuit diagram of corrosion potentials cut-out circuit of the preparation facilities of the controlled big L/D ratio nano-probe of the present invention.
Fig. 4 is the circuit diagram of the corrosion potentials mu balanced circuit of the controlled big L/D ratio nano-probe preparation facilities of the present invention.
Fig. 5 is the structural representation of nano-probe prepared by prior art.
Fig. 6 is the structural representation of nano-probe prepared by the present invention.
In all of the figs, identical reference 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-controls machine, 21-host computer, 22-single-chip microcomputer, 3-corrosion potentials mu balanced circuit, 31-manostat, 32-digital varistor, 4-corrosion potentials cuts off circuit, 41-sampling resistor, 42-voltage follower, 43-scaling circuit, 44-voltage comparator, 5-probe submergence circuit, 51-audion.
Detailed description of the invention
In order to make the purpose 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.As long as just can be mutually combined additionally, technical characteristic involved in each embodiment of invention described below does not constitutes conflict each other.
Seeing Fig. 1, the preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, including mechanical displacement device 1, control machine 2 and control circuit.Wherein, mechanical displacement device 1 is fixed nano-probe and drives nano-probe to move up and down, and control machine includes 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 moves.Control circuit includes that the corrosion potentials mu balanced circuit 3 being connected with single-chip microcomputer 22, corrosion potentials cut off circuit 4 and probe submergence decision circuitry 5, wherein: corrosion potentials mu balanced circuit 3 is for receiving the corrosion potentials signal instruction that single-chip microcomputer 22 sends, and exports, according to instruction, the corrosion potentials preset and keep corrosion potentials constant；Probe submergence decision circuitry 5 is used for detecting probe and immerses, departs from corrosion liquid level, and probe immerses signal, the transmission of probe separating signal to single-chip microcomputer 22.Corrosion potentials cuts off sampling resistor 41, voltage follower 42, scaling circuit 43 and the voltage comparator 44 that circuit 4 includes being sequentially connected in series.Wherein, sampling resistor 41 is used for gathering open circuit potential current value and being converted into magnitude of voltage, voltage follower 42 is used for following and is converted to judge voltage, scaling circuit 43 is used for will determine that voltage signal amplifies, voltage comparator 44 outfan is connected with the I/O port of single-chip microcomputer 22, voltage comparator 44 is used for will determine that voltage compares with threshold voltage, when judging voltage less than threshold voltage, voltage comparator 44 outfan is become high level from low level, and level transitions signal is sent to single-chip microcomputer 22.
When corrosion starts, corrosion potentials cuts off circuit 4 and starts to gather the current signal of open circuit potential, obtains open circuit potential electric current voltage on sampling resistor, i.e. judges voltage.When probe i.e. will be disengaged from liquid level, corrosion process be near completion time, the resistance of whole open circuit potential is increased dramatically, cause corrosion current and judge that voltage also strongly reduces, judge that voltage decreases below rapidly threshold voltage, the outfan of voltage comparator 44 is become high level from low level, single-chip microcomputer 22 detects that this signal intensity rear cutout is broken corrosion potentials immediately, and corrosion process stops.Simultaneously single-chip microcomputer 22 control mechanical displacement device 1 according to probe second cosmic velocity accelerate be lifted up probe depart from corrosive liquid.Cut off the setting of circuit 4 by corrosion, it is possible to the accurately stopping of control corrosion rate process, and quickly mention probe while stopping, advantageously forming more preferable probe tip form.
The preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, corrosion potentials mu balanced circuit 3 includes manostat 31 and the digital varistor 32 of series connection, the preferred switching mode integrated regulator of manostat 31, the input of digital varistor 32 is connected with the outfan of single-chip microcomputer 22, digital varistor 32 receives instruction that single-chip microcomputer 22 sends and changes self-resistance value, makes corrosion potentials that manostat 31 output presets and keeps corrosion potentials constant.Single-chip microcomputer 22 instructs the corrosion potentials value obtaining presetting from host computer 21 and calculates the resistance of digital varistor 32.
The preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, probe submergence decision circuitry 5 includes that audion 51, the base stage of audion 51 are connected with open circuit potential, and colelctor electrode is connected with the input of single-chip microcomputer 22.Audion 51 turns on when probe immerses corrosive liquid and sends probe to single-chip microcomputer 22 and immerses signal.During use, probe is in the moment of contact corrosion liquid, the base stage of audion 51 has electric current to pass through, audion 51 turns on, P2.2 mouth is transferred to low level state by original high level state, after single-chip microcomputer 22 detects the change of level, with probe position herein as basic point, controlling mechanical displacement device 1 makes probe move respective distance in corrosive liquid again, thus reaches accurately to control the purpose of probe submergence.
The preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, mechanical displacement device 1 includes threephase asynchronous driver 11, threephase asynchronous 12, flexible coupling 13, bearing 14, ball-screw 15, fixing nut 16, flexible hinge 17, support 18, mobile working plate 19 and probe clamp 20.Wherein, the input of threephase asynchronous driver 11 connects single-chip microcomputer 22, and outfan connects threephase asynchronous 12, and threephase asynchronous driver is for receiving the instruction that single-chip microcomputer 22 sends, and operates according to order-driven threephase asynchronous 12.The main shaft of threephase asynchronous 12 is connected by flexible coupling 13 is fixing with the fixing end of ball-screw 15, and ball-screw 15 is fixing on mount 18 by bearing 14.Being fixed with nut 16 on ball-screw 15, mobile working plate 19 is connected by flexible hinge 17 is fixing with nut 16, and mobile working plate 19 is fixed linking probe fixture 20.During use, under the instruction of single-chip microcomputer 22, threephase asynchronous driver 11 controls threephase asynchronous 12 and rotates, threephase asynchronous 12 drives ball-screw 15 to rotate by flexible coupling 13, the nut 16 being engaged with ball-screw 15 axially moves along a straight line along ball-screw, and drives mobile working plate 19, probe clamp 20 and probe the most for linear motion along ball-screw.
The preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, preferably the bearing 14 of mechanical displacement device is set to upper bearing (metal) and lower bearing, laying respectively at the top and bottom of ball-screw 15, being preferably set up upper bearing (metal) is fixed bearing, and lower bearing is swimming type bearing.
The preparation facilities of the controlled big L/D ratio nano-probe that the present invention provides, probe clamp 20 uses pricking with needle and row's parent structure, and pricking with needle is fixed on mobile working plate 19, and probe is arranged on row mother.Use pricking with needle row's parent structure that fixing probe is installed, not only can realize being conductively connected but also facilitating mounting or dismounting, and the active force that is subject in corrosion process due to probe is the least, this kind of connection is the most sufficiently tight stable, reliably realizes the round linear motion of probe in the vertical direction.
The preparation method of a kind of controlled big L/D ratio nano-probe that the present invention provides, comprises the following steps:
1) installing probe, be carried out probe processing, the preferred sonic oscillation of cleaning treatment cleans；
2) host computer 21 inputs the thick corrosion potentials preset, smart corrosion potentials, probe submergence, speed is mentioned in probe submergence, speed is mentioned in probe disengaging；
3) single-chip microcomputer 22 controls mechanical displacement device 1 and rotates forward and drive 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 control corrosion rate voltage stabilizing circuit 3 exports thick corrosion potentials, and probe starts slightly to corrode；
4) after probe immerses corrosive liquid, single-chip microcomputer 22 controls mechanical displacement device 1 and continues to move down, until probe arrives the submergence preset, then single-chip microcomputer 22 controls mechanical displacement device 1 and inverts, and drives probe to mention speed according to default probe submergence and is lifted up probe；
5) when probe starts to corrode, corrosion potentials cuts off the sampling resistor 41 of circuit 4 to start gather the current signal of open circuit potential and be converted into magnitude of voltage, obtain judging voltage after amplification followed by voltage follower 42, export to voltage comparator 44 after scaling circuit 43 amplifies again, voltage comparator 44 will determine that voltage compares with the threshold voltage preset, when judging voltage less than threshold voltage, voltage comparator outfan is become high level from low level, single-chip microcomputer 22 detects that this signal intensity rear cutout is broken corrosion potentials immediately, corrosion process stops, single-chip microcomputer 22 controls mechanical displacement device 1 and departs from according to probe and mention speed and be lifted up probe simultaneously, until stopping to during tat probe initial position, probe initial position is normally at above about the 5cm of liquid level；
6) single-chip microcomputer 22 again controls mechanical displacement device 1 and rotates forward and drive 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, the smart corrosion potentials that the output of single-chip microcomputer 22 control corrosion rate voltage stabilizing circuit 3 is preset, probe starts essence corrosion；
7) step 4 is repeated)-5), complete probe and prepare.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, the preferred scope of thick corrosion potentials is 5～12V unidirectional currents, and the essence preferred scope of corrosion potentials is 2～5V unidirectional currents.From electrochemical kinetics theory, corrosion potentials is the biggest, and corrosion rate is the highest, and the corrosion time used is the shortest, but when corrosion potentials is excessive, probe is easily passivated when departing from corrosion liquid level, and needle point radius of curvature does not reaches requirement.Therefore, the present invention uses the method for twice corrosion thick, smart, and corrosion potentials particularly essence corrosion potentials is less, and probe is difficult to passivation when departing from corrosion liquid level, makes probe tip radius of curvature reach requirement.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, can be according to the quantitative relationship between corrosion potentials, immersion depth and the corrosion rate of climb (i.e. speed is mentioned in probe submergence), determine and meet the relevant preparation parameter that probe draw ratio requires, it is achieved prepare the exact controllability of nano-probe draw ratio.
From electrochemical kinetics theory, in the case of corrosive liquid concentration is certain, corrosion potentials is directly proportional to probe corrosion rate, so for the certain probe of diameter, required etching time is also directly proportional to corrosion potentials, this direct ratio numerical relation specifically can be obtained by testing, thus can determine etching time according to corrosion potentials.Being defined from draw ratio, draw ratio divided by probe diameter equal to probe submergence, therefore can be determined probe submergence by probe diameter and draw ratio, further according to the etching time determined, further determine that speed is mentioned in probe submergence.The preparation method of the controlled draw ratio nano-probe that the present invention provides, can use any two value that input corrosion potentials, corrosion depth and probe submergence are mentioned in speed, is calculated by aforementioned quantitative relationship and determines another value.Preferably, select to input corrosion potentials and corrosion depth to host computer 21, calculate and determine that speed is mentioned in probe submergence.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, the quantitative relationship between speed is mentioned according to above-mentioned corrosion potentials, etching time, submergence and probe submergence, and corrosion potentials, probe diameter and the draw ratio determined, being preferably set up probe submergence scope is 1～10cm, according further to etching time, it may be determined that the preferred scope of speed 0.01～10mm/min is mentioned in probe submergence.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, preferred pin arranges probe disengaging and mentions speed more than 100mm/min.The rate of climb after probe shaping disengaging corrosive liquid is disengaging and mentions speed, and it is the fastest that speed is mentioned in disengaging, and probe tip is more difficult to be passivated, and radius of curvature is the least.Probe departs from and mentions probe maximal velocity 100mm/min that speed is preferably obtained by experiment.Speed is mentioned in probe disengaging also can be by user's sets itself, and such as without setting, controlling machine default setting is probe maximal velocity.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, is preferably set up corrosion potentials and cuts off the response time of circuit 4 less than 100 μ s.The response time that corrosion potentials cuts off circuit is the shortest, and probe is less susceptible to passivation, and tip curvature radius is the least, and the response time is mainly determined by the response time of the response time of voltage comparator 44, manostat 31.
The preparation method of the controlled big L/D ratio nano-probe that the present invention provides, single-chip microcomputer 22 is additionally provided with timing software, described step 5) also include that, when probe drops to the submergence preset, etching time timing starts, when probe rises to depart from corrosive liquid, etching time timing stops.Timing software is set on single-chip microcomputer 22, the corrosion time used can be recorded in probe corrosion experiment, to obtain the proportional relation corroding required time with corrosion potentials, to determine etching time when formally preparing nano-probe according to corrosion potentials, and further determine that the important parameters such as speed are mentioned in submergence.
Use the difference of probe prepared by the nano-probe preparation facilities of the present invention and the nano-probe prepared by preparation method and documents, see Fig. 5 and Fig. 6.Fig. 5 is the structural representation of nano-probe prepared by prior art, probe has obvious needle point section (diameter of needle point Duan Yufei needle point section has bigger gap), needle point segment length is the shortest, probe draw ratio the least (description points out that the draw ratio of probe is 3.7).Fig. 6 is the nano-probe that the preparation facilities using the present invention prepares with preparation method, probe does not has obvious needle point section (diameter of needle point Duan Yufei needle point section does not has change suddenly), the Curvature varying of needle point is mild, continuously, thus whole probe can serve as needle point section, the draw ratio of probe is up to 40-400, it is significantly larger than the 3.7 of documents, and excursion is big.The probe of documents is owing to needle point is short, draw ratio is little, and needle point is very easy to abrasion, and i.e. can not re-use after tip wear.And the probe tip of the present invention is long, draw ratio is big, up to 40-400, this probe is the most easy to wear when nanometer manipulation, secondly after most advanced abrasion due to the change of its diameter slowly, can be continuing with, finally when may wear to unusable, can reclaim and carry out essence corrosion and obtain the probe of minor radius and be continuing with, significantly reduce the use cost of probe.
Those skilled in the art is easy to understand; the foregoing is only presently preferred embodiments of the present invention; not in order to limit the present invention, all any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, should be included within the scope of the present invention.
Claims (13)
1. the preparation facilities of a controlled big L/D ratio nano-probe, it is characterised in that: described device includes mechanical displacement device
(1), controlling machine (2) and control circuit, the fixing nano-probe of described mechanical displacement device (1) also drives on nano-probe
Lower movement, described control machine includes that host computer (21) and single-chip microcomputer (22), described single-chip microcomputer (22) fill with mechanical displacement
Putting (1) to be connected and to control mechanical displacement device (1) mobile, described control circuit includes being connected with single-chip microcomputer (22)
Corrosion potentials mu balanced circuit (3), corrosion potentials cut off circuit (4) and probe submergence decision circuitry (5)；
Described corrosion potentials cut-out circuit (4) includes the sampling resistor (41) being sequentially connected in series, voltage follower (42), compares
Example computing circuit (43) and voltage comparator (44), described sampling resistor (41) is connected with open circuit potential, is used for gathering
Open circuit potential current value is also converted into magnitude of voltage, and described voltage follower (42) is used for following and is converted to judge voltage,
Described scaling circuit (43) is used for will determine that voltage signal amplifies；Described voltage comparator (44) outfan and monolithic
The I/O port of machine (22) is connected, and described voltage comparator (44) is used for will determine that voltage compares with threshold voltage, when sentencing
Power-off is forced down when threshold voltage, and voltage comparator (44) outfan is become high level from low level, and level transitions is believed
Number it is sent to single-chip microcomputer (22)；
Described corrosion potentials mu balanced circuit (3) receives the corrosion potentials signal instruction that single-chip microcomputer (22) sends, and according to instruction
Export the corrosion potentials preset and keep corrosion potentials constant；
Described probe submergence decision circuitry (5) detection probe immerses corrosion liquid level, and probe immerses signal transmission to single-chip microcomputer
(22)。
The preparation facilities of a kind of controlled big L/D ratio nano-probe the most according to claim 1, it is characterised in that: described
Corrosion potentials mu balanced circuit (3) includes manostat (31) and digital varistor (32), the described digital varistor (32) of series connection
Input be connected with the outfan of single-chip microcomputer (22), described digital varistor (32) receives single-chip microcomputer (22) and sends
Instruct and change self-resistance value, making manostat (31) export the corrosion potentials preset and keep corrosion potentials constant.
The preparation facilities of a kind of controlled big L/D ratio nano-probe the most according to claim 1, it is characterised in that: described
Probe submergence decision circuitry (5) includes that audion (51), the base stage of described audion (51) are connected with open circuit potential,
Colelctor electrode is connected with the input of single-chip microcomputer (22), and described audion (51) turns on and to list when probe immerses corrosive liquid
Sheet machine (22) sends probe and immerses signal.
The preparation facilities of a kind of controlled big L/D ratio nano-probe the most according to claim 1, it is characterised in that: described
Mechanical displacement device (1) includes threephase asynchronous driver (11), threephase asynchronous (12), flexible shaft coupling
Device (13), bearing (14), ball-screw (15), fixing nut (16), flexible hinge (17), support (18),
Mobile working plate (19) and probe clamp (20), the input of described threephase asynchronous driver (11) connects single
Sheet machine (22), outfan connects threephase asynchronous (12), and the main shaft of described threephase asynchronous (12) passes through
Flexible coupling (13) is fixing with the fixing end of ball-screw (15) to be connected, and described ball-screw (15) passes through bearing (14)
It is fixed on support (18), described ball-screw (15) is fixed with nut (16), described mobile working plate (19)
It is connected by flexible hinge (17) and nut (16) are fixing, the upper fixing linking probe fixture of described mobile working plate (19)
(20)。
The preparation facilities of a kind of controlled big L/D ratio nano-probe the most according to claim 4, it is characterised in that: described
Bearing (14) includes laying respectively at the upper end of ball-screw (15), the upper bearing (metal) of lower end and lower bearing, and described upper bearing (metal) is
Fixed bearing, described lower bearing is swimming type bearing.
The preparation facilities of a kind of controlled big L/D ratio nano-probe the most according to claim 4, it is characterised in that: described
Probe clamp (20) includes pricking with needle and mother row, and described pricking with needle is fixed on mobile working plate (19), and probe is arranged on mother row
On.
7. a preparation method for controlled big L/D ratio nano-probe, uses nano-probe as claimed in claim 1 preparation dress
Put preparation, it is characterised in that comprise the following steps:
1) probe is installed and is carried out probe processing；
2) the thick corrosion potentials that host computer (21) input is preset, smart corrosion potentials, probe submergence, probe submergence are mentioned
Speed, probe depart from and mention speed；
3) single-chip microcomputer (22) control mechanical displacement device (1) rotates forward and drives probe to decline, when probe contact corrosion liquid wink
Between, 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) control corrosion rate voltage stabilizing circuit (3) exports thick corrosion potentials, and probe starts slightly to corrode；
4), after probe immerses corrosive liquid, single-chip microcomputer (22) controls mechanical displacement device (1) and continues to move down, until probe arrives
Reaching default submergence, then single-chip microcomputer (22) control mechanical displacement device (1) reversely rises, and drives probe according in advance
If probe submergence mention speed and be lifted up probe；
5), when probe starts to corrode, corrosion potentials cuts off the sampling resistor (41) of circuit (4) to start to gather open circuit potential
Current signal is also converted into magnitude of voltage, obtains judging voltage after amplification followed by voltage follower (42), then through than
Example computing circuit (43) exports to voltage comparator (44) after amplifying, and voltage comparator (44) will determine that voltage and presets
Threshold voltage compare, when judging voltage less than threshold voltage, voltage comparator outfan is become high electricity from low level
Flat, single-chip microcomputer (22) breaks after this signal intensity being detected corrosion potentials immediately, and corrosion process stops, single-chip microcomputer (22) simultaneously
Control mechanical displacement device (1) is mentioned speed according to probe disengaging and is lifted up probe, until it reaches stop during probe initial position
Only；
6) single-chip microcomputer (22) again controls mechanical displacement device (1) and rotates forward and drive probe to decline, when probe contact corrosion
Liquid moment, probe submergence decision circuitry (5) detects that probe immerses corrosive liquid and sends probe immersion letter to single-chip microcomputer (22)
Number, the smart corrosion potentials that single-chip microcomputer (22) control corrosion rate voltage stabilizing circuit (3) output is preset, probe starts essence corrosion；
7) step 4 is repeated)-5), complete probe and prepare.
The preparation method of a kind of controlled big L/D ratio nano-probe the most according to claim 7, it is characterised in that: described
Host computer (21) is provided with Parameters Computing System, and described Parameters Computing System can be according to corrosion potentials, probe submergence and spy
Any two value calculating that pin submergence is mentioned in speed determines the 3rd value.
The preparation method of a kind of controlled big L/D ratio nano-probe the most according to claim 8, it is characterised in that: described
The calculation procedure of Parameters Computing System includes first determining etching time according to the proportional relation of corrosion potentials and corrosion rate, so
Determine probe submergence according to draw ratio and probe diameter afterwards, determine that probe soaks further according to etching time and probe submergence
Do not mention speed.
The preparation method of a kind of controlled big L/D ratio nano-probe the most according to claim 7, it is characterised in that: institute
Stating thick corrosion potentials is 5～12V unidirectional currents, and described essence corrosion potentials is 2～5V unidirectional currents.
The preparation method of 11. a kind of controlled big L/D ratio nano-probes according to claim 7, it is characterised in that: institute
Stating probe submergence is 1～10cm, and it is 0.01～10mm/min that speed is mentioned in described probe submergence.
The preparation method of 12. a kind of controlled big L/D ratio nano-probes according to claim 7, it is characterised in that: institute
State probe disengaging and mention speed more than 100mm/min.
The preparation method of 13. a kind of controlled big L/D ratio nano-probes according to claim 7, it is characterised in that: institute
State corrosion potentials and cut off the response time of circuit (4) less than 100 μ s.
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| CN104785871B (en) * | 2015-04-17 | 2017-03-15 | 清华大学深圳研究生院 | A kind of preparation method of probe and preparation facilitiess |
| 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 |
| US10060948B2 (en) * | 2016-08-12 | 2018-08-28 | Tiptek, LLC | Scanning probe and electron microscope probes and their manufacture |
| CN108196093B (en) * | 2017-12-26 | 2021-01-12 | 北京阳光凯特科贸有限公司 | Auxiliary device for preparing metal nano probe |
| CN109706515B (en) * | 2019-01-11 | 2020-02-28 | 中国电子科技集团公司第三十八研究所 | Preparation device and preparation method of tungsten filament needle tip with controllable length-diameter 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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