CN104785871A - Probe manufacturing method and device - Google Patents

Probe manufacturing method and device Download PDF

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Publication number
CN104785871A
CN104785871A CN201510186082.8A CN201510186082A CN104785871A CN 104785871 A CN104785871 A CN 104785871A CN 201510186082 A CN201510186082 A CN 201510186082A CN 104785871 A CN104785871 A CN 104785871A
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wire
probe
solution
diameter
graphite electrode
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CN201510186082.8A
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CN104785871B (en
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张旻
易振东
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Shenzhen Graduate School Tsinghua University
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Shenzhen Graduate School Tsinghua University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23HWORKING OF METAL BY THE ACTION OF A HIGH CONCENTRATION OF ELECTRIC CURRENT ON A WORKPIECE USING AN ELECTRODE WHICH TAKES THE PLACE OF A TOOL; SUCH WORKING COMBINED WITH OTHER FORMS OF WORKING OF METAL
    • B23H3/00Electrochemical machining, i.e. removing metal by passing current between an electrode and a workpiece in the presence of an electrolyte

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Electrical Discharge Machining, Electrochemical Machining, And Combined Machining (AREA)

Abstract

The invention discloses a probe manufacturing method and device. The probe manufacturing method comprises the steps that 1, a metal wire is immersed into an electric corrosion solution, wherein the electric corrosion solution is contained in a container made from a graphite material or a cylindrical graphite electrode wounded with a metal wire is arranged in the electric corrosion solution, the graphite electrode is higher than liquid level, and the diameter of the graphite container or the cylindrical graphite electrode ranges from 20 mm to 75 mm; 2, voltage application between the metal wire and the container or between the metal wire and the cylindrical graphite electrode is implemented in the following mode: first sine alternating-current voltage ranging from 30 V to 45 V is firstly applied for application time to ensure that the corrosion speed of the portion, immersed under the liquid level, of the metal wire is 1/30-1/20 mm/s; then second sine alternating-current voltage ranging from 15 V to 25 V is applied for application time till corrosion reaction is completed; 3, the metal wire is lifted out of the liquid level to complete probe manufacture. A manufactured probe is cylinder-shaped, is at the sub-micron grade in size and has higher length-diameter ratio.

Description

A kind of preparation method of probe and preparation facilities
[technical field]
The present invention relates to preparation method and the preparation facilities of probe, particularly relate to a kind of submicron order, the preparation method of probe of big L/D ratio and preparation facilities.
[background technology]
Fine probe is widely used in the fields such as scan-probe imaging, Multi-contact measurement, micro-nano manipulation and electrochemistry micro Process, and the size and dimension of needle point directly determines serviceability and the range of application of probe.For electrochemistry micro Process, the probe of current use mostly is micro fine cylindrical shape probe, by the relative motion of probe and workpiece, electrochemistry Milling Process goes out required part, and therefore the size and shape of probe directly determines the micro-machined machining accuracy of electrochemistry and the minimum process limit.
The micro fine cylindrical probe that current electrochemistry micro Process uses, is generally obtained by electrochemical etching method.The detail of electrochemical corrosion course is had nothing in common with each other, but cylindrical probe size obtained is at present all more than 3 microns, cannot be used in the electrochemistry micro Process of sub-micron or nanoscale structures.And the probe made by some electrochemical corrosive process, although needle point can be worked into nanoscale, probe pattern is conical, and major diameter is smaller, cannot be used for the occasion that the working depths such as electrochemistry micro Process are larger.
[summary of the invention]
Technical problem to be solved by this invention is: make up above-mentioned the deficiencies in the prior art, proposes a kind of preparation method and preparation facilities of probe, and the pattern of obtained probe is cylindric, and size at submicron order, and has larger draw ratio.
Technical problem of the present invention is solved by following technical scheme:
A preparation method for probe, comprises the following steps: 1) immersed by wire in galvano-cautery solution; Wherein, described galvano-cautery solution is contained in the container that graphite material makes, or is placed with in described galvano-cautery solution around described cylindric graphite electrode wiry, and described graphite electrode exceeds liquid level; Wherein, the diameter of the diameter of container made of described graphite material or the graphite electrode of described cylindrical shape is 20 ~ 75mm; 2) between described wire and described container, or apply voltage in the following manner between described wire and described cylindric graphite electrode: the first sinusoidal voltage first applying 30 ~ 45V, the corrosion rate of the part that application time is guaranteed under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then apply second sinusoidal voltage of 15 ~ 25V, application time is until corrosion reaction terminates; 3) the described wire lift after process is departed from liquid level, complete the preparation of probe.
A preparation facilities for probe, comprises electrolytic cell, displacement platform, alternating-current voltage source and control circuit; The container that the graphite material of described electrolytic cell to be diameter be 20 ~ 75mm is made, for loading galvano-cautery solution; Described displacement platform is used for fixing raw materials wire, and adjustablely makes described wire be dipped in described galvano-cautery solution; One output of described alternating-current voltage source connects described wire, and another output connects described container, and control signal receiving terminal connects described control circuit; Described control circuit first exports first sinusoidal voltage of 30 ~ 45V for controlling described alternating-current voltage source, the corrosion rate of the part that the duration guarantees under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then export second sinusoidal voltage of 15 ~ 25V, the duration is until corrosion reaction terminates.
A preparation facilities for probe, comprises electrolytic cell, cylindric graphite electrode, displacement platform, alternating-current voltage source and control circuit; Described electrolytic cell is for loading galvano-cautery solution; Described displacement platform is used for fixing raw materials wire, and adjustablely makes described wire be dipped in described galvano-cautery solution; The diameter of described cylindric graphite electrode is 20 ~ 75mm, is placed in described galvano-cautery solution, and arranges around described wire; One output of described alternating-current voltage source connects described wire, and another output connects described cylindric graphite electrode, and control signal receiving terminal connects described control circuit; Described control circuit first exports first sinusoidal voltage of 30 ~ 45V for controlling described alternating-current voltage source, the corrosion rate of the part that the duration guarantees under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then export second sinusoidal voltage of 15 ~ 25V, the duration is until corrosion reaction terminates.
The beneficial effect that the present invention is compared with the prior art is:
The preparation method of probe of the present invention and preparation facilities, the container that graphite material conductive wire being placed in cylindric graphite electrode or cylindrical shape is made, immerse in electrochemical corrosion solution, adopt alternating current caustic solution, through the etch state of two step high-low voltage in corrosion process, and strict control voltage size and etching time, thus described conductive wire is corroded into big L/D ratio, the cylindrical probe of submicron-scale.After tested, the draw ratio of obtained probe is 20 ~ 50 (draw ratio of the probe below existing micron order is generally less than 10), and size is in 500nm ~ 1 μm.The present invention can realize the making of the cylindrical needle of submicron order big L/D ratio rapidly, easily, and process of preparing is simple, and cost is low, and can produce in batches.The size of cylindrical needle adopting the present invention to prepare only apply voltage with electrochemical corrosion and the time relevant, have nothing to do with equipment precision in process, relative to the relative displacement equally accurate needing in some preparation method existing strictly to control between two electrodes, the present invention can be convenient to control to prepare the cylindrical probe in high-aspect-ratio micro nano structure electrochemistry micro Process.
[accompanying drawing explanation]
Fig. 1 is the structural representation of the preparation facilities of the probe of the specific embodiment of the invention;
Fig. 2 is the scanning electron microscope (SEM) photograph of probe obtained in the embodiment 1 of the specific embodiment of the invention;
Fig. 3 is the scanning electron microscope (SEM) photograph of probe obtained in the embodiment 2 of the specific embodiment of the invention.
[detailed description of the invention]
Contrast accompanying drawing below in conjunction with detailed description of the invention the present invention is described in further details.
As shown in Figure 1, a kind of preparation facilities for the preparation of submicron order, large major diameter, cylindrical needle, comprising: electrolytic cell 5, displacement platform 1, adjustable ac source 3 and control circuit (not shown).
Wherein, electrolytic cell 5 is for splendid attire galvano-cautery solution 4.Galvano-cautery solution 4 can be the electrolytic solution configured by electrolytes such as calcium chloride, sodium chloride, NaOH, potassium hydroxide.The diameter that electrolytic cell 5 adopts graphite material to make is the container of 20 ~ 75mm, such as graphite crucible, preferably, selects high purity graphite crucible.The diameter of crystal vessel is 20 ~ 75mm, as lower than 20mm or higher than 75mm, cannot obtain satisfactory probe.In this embodiment, electrolytic cell 5 is as container containing, simultaneously as using electrode.
Displacement platform 1 is for fixing conductive wire 2, and preferred conductive wire 2 is placed in the center of electrolytic cell 5, perpendicular to electrolyte 4 liquid level.Conductive wire 2 can be the metal material such as tungsten, platinum, and preferably, conductive wire 2 diameter is 0.1 ~ 1mm.
Adjustable ac source 3, adjustable ac source 3, under the control of control circuit, applies sinusoidal voltage between conductive wire 2 and electrolytic cell 5, makes electrolyte 4 that conductive wire 2 is progressively corroded into big L/D ratio cylindrical probe.
Control circuit is divided into two stages for controlling whole electrochemical corrosion: the first stage, controls adjustable ac source 3 and exports sinusoidal voltage U1, and the virtual value of sinusoidal voltage U1, at 30 ~ 45V, continues processing a period of time T1; Second stage, control adjustable ac source 3 and export sinusoidal voltage U2, the virtual value of sinusoidal voltage U2 is at 15 ~ 25V, until corrosion reaction terminates.Wherein, each phase duration of adjustable ac source 3 and switched voltage are controlled automatically to complete by control circuit.The duration T 1 of U1 is determined according to the length of the part under wire immersed in liquid level, to guarantee that the corrosion rate of the part under described wire immersed in liquid level is for 1/20 ~ 1/30mm/s.Such as, the length of the part under wire immersed in liquid level is 3mm, then the duration T 1 of the first sinusoidal voltage is 60 ~ 90s.
By above-mentioned preparation facilities, conductive wire is placed in the container that graphite material is made, immerse in electrochemical corrosion solution, adopt alternating current caustic solution, through the etch state of two step high-low voltage in corrosion process, and strict control voltage size and etching time, make the first stage that electrochemistry+electric spark dual corrosion occur, only there is electrochemical corrosion in second stage, and around cylinder graphite material container guarantee that wire evenly completes in two stage corrosion, the most described conductive wire corrodes into big L/D ratio, the cylindrical probe of submicron-scale.
In above-mentioned embodiment, the container adopting graphite material to make both had played the effect of container containing, played again the effect to electrode.Alternative scheme is, common container selected by container, and then use diameter to be the effect that the graphite electrode of the cylindrical shape of 20 ~ 75mm directly plays to electrode, correspondingly, the alternating voltage of applying is then applied between wire and cylindric graphite electrode.By this replacement scheme, also big L/D ratio can be obtained, the cylindrical probe of submicron-scale.
Preferably, the diameter of the graphite electrode of the container that above-mentioned graphite material is made or cylindrical shape is 20 ~ 40mm, and when within the scope of this, relative to crystal vessel or the graphite electrode of other sizes, the pattern of obtained probe is better, peripheral evenly.
The parameter of probe prepared by this detailed description of the invention is described with exemplary embodiment below.
Embodiment 1
The present embodiment electrochemical corrosion platinum filament, prepare submicron order big L/D ratio cylindrical probe, specifically comprise the following steps:
1) first intercept long 10 ~ 15mm, diameter is the platinum filament of 0.3mm, with acetone and deionized water ultrasonic cleaning respectively, then dries up rear clamping on displacement platform 1 with nitrogen.
2) regulate displacement platform 1, platinum filament 2 be placed in the center of electrolytic cell 5 and immerse galvano-cautery liquid 4,3mm under the immersed in liquid level of platinum filament end.The galvano-cautery liquid 4 that the present embodiment carries out electrochemical corrosion platinum filament for mass fraction be the calcium chloride solution of 20%.Electrolytic cell 5 is circular graphitic crucible, and graphite crucible diameter is 40mm.
3) open adjustable ac source 3, between platinum filament 2 and electrolytic cell 5, apply sinusoidal voltage, electrochemical corrosion is carried out to platinum filament 2.Wherein, control AC power 3 by control circuit, make concrete electrochemical corrosion condition to be: control the sinusoidal voltage virtual value of adjustable ac source 3 for 35V, frequency is 50Hz, continue processing 60s; Then the sinusoidal voltage virtual value of adjustable ac source 3 is controlled to switch to 20V, until corrosion processing terminates.
4), after the platinum filament 2 taking-up washed with de-ionized water of having corroded being dried, the preparation of cylindrical probe is completed.
As shown in Figure 2, the microscopic appearance figure of the probe tip obtained for the present embodiment.As we know from the figure, the shape of probe is cylindric, and external corrosion is comparatively even.The size of probe obtained in this detailed description of the invention is 0.9 micron, and draw ratio is 20.
Embodiment 2: the difference of the present embodiment and embodiment 1 is: the length under wire immersed in liquid level, the parameters of electrochemical corrosions such as the virtual value of the mass fraction of electrolyte, the diameter of graphite crucible and sinusoidal voltage are different.
The present embodiment electrochemical corrosion platinum filament, prepare submicron order big L/D ratio cylindrical probe, specifically comprise the following steps:
1) first intercept long 10 ~ 15mm, diameter is the platinum filament of 0.3mm, with acetone and deionized water ultrasonic cleaning respectively, then dries up rear clamping on displacement platform 1 with nitrogen.
2) regulate displacement platform 1, platinum filament 2 be placed in the center of electrolytic cell 5 and immerse galvano-cautery liquid 4,3mm under the immersed in liquid level of platinum filament end.The galvano-cautery liquid 4 that the present embodiment carries out electrochemical corrosion platinum filament for mass fraction be the calcium chloride solution of 30%.Electrolytic cell 5 is circular graphitic crucible, and graphite crucible diameter is 25mm.
3) open adjustable ac source 3, between platinum filament 2 and electrolytic cell 5, apply sinusoidal voltage, electrochemical corrosion is carried out to platinum filament 2.Wherein, control AC power 3 by control circuit, make concrete electrochemical corrosion condition to be: control the sinusoidal voltage virtual value of adjustable ac source 3 for 30V, frequency is 50Hz, continue processing 90s; Then the sinusoidal voltage virtual value of adjustable ac source 3 is controlled to switch to 18V, until corrosion processing terminates.
4), after the platinum filament 2 taking-up washed with de-ionized water of having corroded being dried, the preparation of cylindrical probe is completed.
As shown in Figure 3, the microscopic appearance figure of the probe tip obtained for the present embodiment.As we know from the figure, the shape of probe is cylindric, and external corrosion is comparatively even.The size of probe obtained in this detailed description of the invention is 0.6 micron, and draw ratio is 24.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, make some substituting or obvious modification without departing from the inventive concept of the premise, and performance or purposes identical, all should be considered as belonging to protection scope of the present invention.

Claims (10)

1. a preparation method for probe, is characterized in that: comprise the following steps: 1) immersed by wire in galvano-cautery solution; Wherein, described galvano-cautery solution is contained in the container that graphite material makes, or is placed with in described galvano-cautery solution around described cylindric graphite electrode wiry, and described graphite electrode exceeds liquid level; Wherein, the diameter of the diameter of container made of described graphite material or the graphite electrode of described cylindrical shape is 20 ~ 75mm; 2) between described wire and described container, or apply voltage in the following manner between described wire and described cylindric graphite electrode: the first sinusoidal voltage first applying 30 ~ 45V, the corrosion rate of the part that application time is guaranteed under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then apply second sinusoidal voltage of 15 ~ 25V, application time is until corrosion reaction terminates; 3) the described wire lift after process is departed from liquid level, complete the preparation of probe.
2. the preparation method of probe according to claim 1, is characterized in that: described step 1) in, the diameter of the diameter of the container that described graphite material is made or the graphite electrode of described cylindrical shape is 20 ~ 40mm.
3. the preparation method of probe according to claim 1, is characterized in that: described step 1) in, the length of the part under described wire immersed in liquid level is 3mm; Described step 2) in, the application time of described first sinusoidal voltage is 60 ~ 90s.
4. the preparation method of probe according to claim 1, is characterized in that: described step 1) in, described diameter wiry is 0.1 ~ 1mm.
5. the preparation method of probe according to claim 1, is characterized in that: described step 1) in, described wire is tungsten material or alloy platinum material.
6. the preparation method of probe according to claim 1, is characterized in that: described step 1) in, described galvano-cautery solution is the electrolytic solution configured by calcium chloride, sodium chloride, NaOH, potassium hydroxide.
7. a preparation facilities for probe, is characterized in that: comprise electrolytic cell, displacement platform, alternating-current voltage source and control circuit;
The container that the graphite material of described electrolytic cell to be diameter be 20 ~ 75mm is made, for loading galvano-cautery solution;
Described displacement platform is used for fixing raw materials wire, and adjustablely makes described wire be dipped in described galvano-cautery solution;
One output of described alternating-current voltage source connects described wire, and another output connects described container, and control signal receiving terminal connects described control circuit;
Described control circuit first exports first sinusoidal voltage of 30 ~ 45V for controlling described alternating-current voltage source, the corrosion rate of the part that the duration guarantees under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then export second sinusoidal voltage of 15 ~ 25V, the duration is until corrosion reaction terminates.
8. the preparation facilities of probe according to claim 7, is characterized in that: the diameter of the container that described graphite material is made is 20 ~ 40mm.
9. a preparation facilities for probe, is characterized in that: comprise electrolytic cell, cylindric graphite electrode, displacement platform, alternating-current voltage source and control circuit;
Described electrolytic cell is for loading galvano-cautery solution;
Described displacement platform is used for fixing raw materials wire, and adjustablely makes described wire be dipped in described galvano-cautery solution;
The diameter of described cylindric graphite electrode is 20 ~ 75mm, is placed in described galvano-cautery solution, and arranges around described wire;
One output of described alternating-current voltage source connects described wire, and another output connects described cylindric graphite electrode, and control signal receiving terminal connects described control circuit;
Described control circuit first exports first sinusoidal voltage of 30 ~ 45V for controlling described alternating-current voltage source, the corrosion rate of the part that the duration guarantees under described wire immersed in liquid level is 1/30 ~ 1/20mm/s; Then export second sinusoidal voltage of 15 ~ 25V, the duration is until corrosion reaction terminates.
10. the preparation facilities of probe according to claim 7, is characterized in that: the diameter of described cylindric graphite electrode is 20 ~ 40mm.
CN201510186082.8A 2015-04-17 2015-04-17 A kind of preparation method of probe and preparation facilitiess Expired - Fee Related CN104785871B (en)

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Cited By (5)

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CN106771377A (en) * 2017-03-14 2017-05-31 贵州大学 The draw bail and probe rod fixing means of a kind of vertical fixed probe rod
CN109709353A (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 the electrochemistry preparation facilities and preparation method of metal iridium needle point
CN109909569A (en) * 2019-04-23 2019-06-21 中南大学 A kind of processing method and device of high-precision micropore
CN113073376A (en) * 2021-03-03 2021-07-06 上海伟测半导体科技股份有限公司 Application of corrosion powder in shaping platinum probe and shaping method of platinum probe
CN116543982A (en) * 2023-03-23 2023-08-04 清华大学 Microelectrode preparation method and microelectrode

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Publication number Priority date Publication date Assignee Title
CN106771377A (en) * 2017-03-14 2017-05-31 贵州大学 The draw bail and probe rod fixing means of a kind of vertical fixed probe rod
CN109709353A (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 the electrochemistry preparation facilities and preparation method of metal iridium needle point
CN109909569A (en) * 2019-04-23 2019-06-21 中南大学 A kind of processing method and device of high-precision micropore
CN113073376A (en) * 2021-03-03 2021-07-06 上海伟测半导体科技股份有限公司 Application of corrosion powder in shaping platinum probe and shaping method of platinum probe
CN113073376B (en) * 2021-03-03 2022-04-12 上海伟测半导体科技股份有限公司 Application of corrosion powder in shaping platinum probe and shaping method of platinum probe
CN116543982A (en) * 2023-03-23 2023-08-04 清华大学 Microelectrode preparation method and microelectrode
CN116543982B (en) * 2023-03-23 2024-01-30 清华大学 Microelectrode preparation method and microelectrode

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