CN103056463B - Manufacturing method for carbon nano tube tool electrode for micro electrochemical machining and multi-functional working tanks - Google Patents

Manufacturing method for carbon nano tube tool electrode for micro electrochemical machining and multi-functional working tanks Download PDF

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CN103056463B
CN103056463B CN201210544466.9A CN201210544466A CN103056463B CN 103056463 B CN103056463 B CN 103056463B CN 201210544466 A CN201210544466 A CN 201210544466A CN 103056463 B CN103056463 B CN 103056463B
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electrode
tool
cnt
pond
carbon nano
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CN103056463A (en
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朱荻
曾永彬
吴修娟
曲宁松
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention relates to manufacturing of a carbon nano tube tool electrode which is applicable to electrochemical machining and belongs to the field of electrochemical machining. The manufacturing method includes step 1, clamping an original tool electrode tungsten bar (13) on a Z shaft (5) which is a precision moving shaft and has nanometer resolution, step 2, placing multi-functional working tanks (8) on an X precision displacement stage (9) and a Y precision displacement stage (10), step 3, preparing a tungsten electrode on line by using electrochemical corrosion method in the multi-functional working tank (8) A, step 4, welding a carbon nano tube on the tungsten electrode by voltage method in the multi-functional working tank (8) B under a microscope (14) field of view, and step 5, utilizing a membrane micro electroforming method to electroforming a layer of metallic nickel on a position where the tungsten electrode and the carbon nano tube are connected in the multi-functional working tank (8) C. According to the manufacturing method for carbon nano tube tool electrode for micro electrochemical machining, the bonding strength of the tungsten electrode and the carbon nano tube and the electrical conductivity of the whole carbon nano tube tool electrode are increased, and nano electrochemical machining of the carbon nano tube tool electrode in electrolyte conditions is guaranteed.

Description

Micro-electrochemical machining processing carbon nano tube tool-electrode preparation method and multifunctional working groove
Technical field
The invention belongs to electrochemistry manufacture field, relate to micro-electrochemical machining processing carbon nano tube tool-electrode preparation method and multifunctional working groove.
Background technology
Along with scientific and technical development, in modern many new high-tech products, all comprising high-accuracy sub-micron or the structure of nano-scale, these fine structures often have vital effect.Micro-electrochemical machining processing is a kind of important processing method in fine manufacture field.Micro-electrochemical machining processing, refers within the scope of microfabrication, and the principle of utilizing metal that Anodic dissolving occurs in electrolyte is carried out the processing method of etching shaping to material.From processing mechanism, metallic atom work in-process on workpiece anode constantly loses electronics to be become ion and dissolves from workpiece, the minimizing process of its material is carried out with the form of ion, and the mode of this ion remaval makes Electrolyzed Processing have the ability of microfabrication.Therefore, controlled working condition, chooses suitable machined parameters, can realize with number of ions magnitude material is processed, and meets the demand of fine manufacturing technology.
Because tool-electrode in electrochemical machining process does not contact with workpiece, and it is wide to have rapidoprint scope, be not subject to the impact of the strength of materials, hardness, toughness, surface of the work is without machining stress, without distortion and heat affected area, without tool electrode loss, the advantages such as machined surface quality.Micro-electrochemical machining processing has been successfully applied to the fields such as medical treatment, electronics, space flight.But have the polytropy in dispersion corrosion, electric field and flow field, the factors such as processing locality are subject to certain restrictions the precision of Electrolyzed Processing.Wherein the shape and size of tool-electrode have a significant impact precision and the crudy of micro-electrochemical machining processing.High-precision micro-electrochemical machining processing needs high-precision tool-electrode.Reduce tool-electrode size, improve tool-electrode shape, can improve the precision of micro-electrochemical machining processing.
The micro electrode that micro-electrochemical machining processing is at present used is mainly to obtain by methods such as electrochemical etching, electrochemical deposition, the grinding of fine electric spark line electrode, laser cutting, ion etchings.By electrochemical method, electrode yardstick general control is in micron or sub-micrometer range, and it is shorter that nanoscale is difficult for the partial-length of acquisition and nanoscale.Ion etching is one of method accurate, the finest in special process method, and machined surface quality, and general mismachining tolerance can be controlled at several nanometers.The A.L.Trimmer of Virginia, USA university etc. use focused particle beam milling technology machining tool electrode, on the tungsten filament of original 100 micron diameters, mill out round building and 2x2 array columnar electrode, the seam of round building is wide in tens nanometers, and the preparation of each electrode has been used 1-3 hour.But this processing method need to have the ion beam of a set of complexity to produce equipment, expensive, also has the defects such as productivity ratio is low.
CNT is elongated, diameter generally in several nanometers to tens nanometers, length is generally at micron order, aspect ratio is high; Elastic modelling quantity is very high; The lamellar structure of graphite is identical, has good electric conductivity.If for Electrolyzed Processing, processing yardstick will reach Nano grade using CNT as tool-electrode.So far, scientists has been carried out research extensively and profoundly to CNT performance and application, and CNT is bonded in to plain scan probe formation CNT scan-probe.Conventional method has: method, voltage preparation method etc. are picked up in conductive adhesive method, chemical vapour deposition technique, scanning.Wherein voltage preparation method is more easily realized, first the silicon probe of CNT and metal-coated membrane is connected with two three-dimensional travelling carriages respectively, and the positive pole of CNT one side joint additional power source, negative pole is connected with common probe.Very approaching between probe and CNT, during the distance of about 1-10 micron, between applies voltage, can see that CNT is truncated under light microscope, produces with electric arc simultaneously, and the CNT part being truncated is adhered on ordinary silicon probe.
For the electrode of Electrolyzed Processing, not only require to there is good electric conductivity, but also will there is the stability in liquid environment.Above-mentioned study general is all CNT is bonded in to silicon needle point or plated on the silicon needle point of layer metal, is usually used in gaseous environment, and for scanning probe microscopy, the adhesion between CNT and needle point is about 1.2-3.6 μ N.If be applied in electrolyte environment, CNT is hydrophobic material, very easily bending in entering liquid environment process, or because adhesion strength is lost not.Scientists to strengthen the bonding strength of CNT and probe, provides feasibility for carbon nanotube probes carries out work in solution environmental by ways such as deposition, plated films on carbon nanotube probes.The King of U.S. Ha Fu university etc., the carbon nanotube probes using is in test standby by CVD legal system, and under SEM deposit carbon compound, to strengthen its adhesive strength.U.S. Canada nanometer technology center Stevens etc., in experiment by toward vacuum evaporation ethylenediamine film on carbon nanotube probes, reduce the hydrophobicity of CNT, strengthen the adhesive strength of carbon nanotube probes, thereby can in liquid, be stable into picture, successfully utilize the carbon nanotube probes of plated film, in liquid, DNA molecular has been carried out to imaging.But no matter be sedimentation, or coating method all need expensive experimental facilities and harsh experimental situation.
Summary of the invention
The object of the invention is to, for the problems referred to above.Propose that a kind of method is simple, the better micro-electrochemical machining processing carbon nano tube of preparation quality tool-electrode preparation method and multifunctional working groove and multifunctional working groove thereof.
A micro-electrochemical machining processing carbon nano tube tool-electrode preparation method, is characterized in that comprising following process: step 1, at tool-electrode, prepare in pond, use electrochemical etching method to process original tool electrode tungsten bar, preparation more piece tip-like tungsten electrode; Step 2, in CNT welding pond, under microscopic fields of view, with voltage method, CNT is welded on tungsten electrode needle point; Step 3, in film fine electroforming pond, the position electroforming layer of metal nickel that adopts the method for film fine electroforming that tungsten electrode is connected with CNT; The accurate shifting axle Z axis that moves through of above-mentioned tool-electrode drives; Above-mentioned tool-electrode is prepared pond, CNT welding pond, moving through in XY precision displacement table of film fine electroforming pond realized.
Above-mentioned steps 1 detailed process can be as follows: above-mentioned tool-electrode is prepared and in pond, had the first corrosion resistant plate with working hole; Electrolyte submergence the first corrosion resistant plate; During work, corrosion resistant plate is connected with power cathode, and tool-electrode is connected with positive source; Original tool electrode tungsten bar is immersed to certain depth under electrolysis liquid surface through the working hole on the first corrosion resistant plate, start to carry out electrochemical etching; After electrochemical etching after a while, electrode is upwards mentioned to a segment distance, proceed electrochemical etching, after a period of time, upwards mention again a segment distance, proceed electrochemical etching, until etch required diameter.
Above-mentioned steps 2 detailed processes can be as follows: above-mentioned CNT welding has the second corrosion resistant plate in pond, is bonded with the multi-walled carbon nano-tubes of array on the second corrosion resistant plate with conducting resinl; During work, multi-walled carbon nano-tubes is connected with positive source by the second corrosion resistant plate, and tool-electrode is connected with power cathode; At microscope, amplify under visual field, find an outstanding CNT up front, allow tungsten electrode near outstanding CNT, when the distance between CNT and tungsten electrode is 1-10 micron, between applies 8 ~ 30V and exchanges or DC voltage, until CNT is attracted by electrode tip, adjustment precision micropositioner again, make the axis of CNT consistent with the direction of tool-electrode axis, then between applies 30 ~ 60V interchange or DC voltage, between CNT and tool-electrode, there is arc discharge, obtain CNT tool-electrode.
Above-mentioned steps 3 detailed processes can be as follows: a nickel ring suspends in above-mentioned film fine electroforming pond; The CNT tool-electrode having bondd, through nickel ring, is then drawn to electroforming solution and injected nickel ring with suction pipe, form the electroforming solution liquid film of thin layer; During work, CNT is connected with power cathode, and nickel ring is connected with power anode; Control the electroforming time, can be by the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT; The thickness of metallic nickel is by regulating current density and the time of electroforming to control, and current density is larger, and the time is longer, and the thickness of nickel dam is thicker.
Multifunctional working groove for described micro-electrochemical machining processing carbon nano tube tool-electrode preparation method, is characterized in that: this multifunctional working groove is prepared pond, CNT welding pond and film fine electroforming pond by tool-electrode and formed; Above-mentioned tool-electrode is prepared in pond and is had U-shaped base, is fixed wtih the first corrosion resistant plate with working hole on U-shaped base; Above-mentioned CNT welding has U-shaped base in pond, is fixed wtih the second corrosion resistant plate on U-shaped base, is bonded with the multi-walled carbon nano-tubes of array on the second corrosion resistant plate with conducting resinl; Above-mentioned film fine electroforming has L-type base in pond, and a nickel ring suspends on L-type base;
The present invention has the following advantages:
1. the method adopts and prepares online CNT tool-electrode, for the preparation of CNT tool-electrode, without through multiple clamping, reduces the damage to CNT tool-electrode in clamping error and clamping process.The welding of the preparation of general purpose tool electrode, CNT tool-electrode, and the post processing that it is carried out are generally all to carry out on different instrument and equipments.The multifunctional working groove that the present invention adopts, is divided into tri-work nests of A, B and C, and tool-electrode preparation, CNT welding and micro electroforming are reinforced and integrated, and without changing work nest, and makes on same precision machine tool.Adopt the method, not only reduced error and the number of times of clamping, but also improved efficiency prepared by CNT tool-electrode.
2. the position electroforming layer of metal nickel that adopts liquid-film method to be connected with CNT tungsten electrode.CNT is hydrophobic material, very easily bending in entering liquid environment process, or because adhesion strength is lost not.In existing research, increase in the method for CNT and probe adhesion strength, what use is deposit carbon compound, vacuum evaporation ethylenediamine film under SEM.These methods all need expensive equipment and harsh environment, and ethylenediamine or poisonous reagent, will pay special attention to safety in use.If adopt the method for general electroforming by CNT tool-electrode surface casting last layer metal, how the still carbon nanotube electrode that first will solve enters the problem of electroforming solution, and this has revert to initial point by problem again.What the present invention adopted is the method for liquid film micro electroforming, can address this problem, and first the CNT tool-electrode having bondd is passed to nickel ring, and then by suction pipe injection nickel ring for electroforming solution, can carry out electroforming test, and the method is simple and feasible.
3. the present invention adopts liquid film electrocasting to process CNT tool-electrode, has increased adhesion strength and electrical conductivity between electrode and CNT.By voltage method, CNT and electrode needle point are welded together, less and the adhesion of its pad contact area is about 1.2-3.6 μ N a little less than, by the local electroforming last layer metal in its welding, in a disguised form increase the contact area of CNT part with tool-electrode part, increased its electrical conductivity and adhesion strength.
Accompanying drawing explanation
Fig. 1 is micro-electrochemical machining processing carbon nano tube tool-electrode preparation system figure;
Fig. 2 is CNT tool-electrode micro electroforming schematic diagram;
Fig. 3 is multifunctional working groove figure;
Its label name is called: 1. industrial computer; 2. data collecting card; 3. video frequency collection card; 4. motion control card; 5 motive spindle Z axis; 6. oscillograph; 7. power supply; 8. multifunctional working groove; 9. motive spindle Y-axis; 10. motive spindle X-axis; 11. vibration-isolating platforms;
12. collets; 13. tool-electrodes; 14.CCD; 15. nickel rings; 16. multi-walled carbon nano-tubes; 17. electroforming solution; 18.L type base; 19. bolts; 20. wires; 21.U type base; 22. conducting resinls; 23. second corrosion resistant plates; 24. first corrosion resistant plates; 25. electrolyte.
The specific embodiment
Original tool electrode tungsten bar 13 is held on the accurate shifting axle Z axis 5 with nanometer resolution; Multifunctional working groove 8 is placed in XY precision displacement table;
In multifunctional working groove A, use electrochemical etching to prepare more piece tip-like electrode.The first corrosion resistant plate 24 that is 1.8-2mm by thickness is fixed in A pond on U-shaped base 21, and on stainless steel, bore dia is 4-5mm, and is connected with power cathode corrosion resistant plate as negative electrode; Adopt the potassium hydroxide of 2mol/L as electrolyte, original tungsten electrode diameter is 300 μ m, and tungsten electrode connects positive source.Controlled motion main shaft Z axis 5 immerses certain depth under electrolysis liquid surface by original tungsten electrode, start to carry out electrochemical etching, after electrochemical etching after a while, upwards mention a segment distance, proceed electrochemical etching, after a period of time, upwards mention again a segment distance, proceed electrochemical etching, until stop processing after etching required diameter.
Prepare after electrode, moving movement major axis X axle 10 by multifunctional working groove B, move to electrode under.In B, the multi-walled carbon nano-tubes of array 16 use conducting resinls 22 are bonded on the second corrosion resistant plate 23 being fixed on base 21, CNT connects the positive pole of power supply by corrosion resistant plate, and now electrode connects power cathode.In microscope 14 multiplication factors, be under the visual field of 1000 times, find an outstanding CNT up front, and moving three dimension workbench, allow tungsten electrode near outstanding CNT.When the distance between CNT and tungsten electrode is very near, during about 1-10 micron, between applies 8 ~ 30V and exchanges or DC voltage, until CNT is attracted by electrode tip, adjustment precision micropositioner, makes the axis of CNT consistent with the direction of tool-electrode axis again, and then between applies 30 ~ 60V interchange or DC voltage, between CNT and tool-electrode, there is arc discharge, obtain CNT tool-electrode;
Obtain after CNT tool-electrode, moving movement major axis X axle 10 by multifunctional working groove C, move to tool-electrode under.Nickel ring 15 is fixed on L-type base 18, and one section of annulus is unsettled, and nickel ring 15 diameters are 4-5mm, is to form with the nickel wire bending that diameter is 200 μ m.The CNT tool-electrode now first just having bondd, through nickel ring, is then drawn electroforming solution and injects nickel ring with suction pipe, forms the electroforming solution liquid film of thin layer.CNT instrument connects power cathode, and nickel ring connects power anode, controls the electroforming time, can be by the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT.The thickness of metallic nickel can be by regulating current density and the time of electroforming to control.

Claims (7)

1. a micro-electrochemical machining processing carbon nano tube tool-electrode preparation method, is characterized in that comprising following process:
Step 1, at tool-electrode, prepare in pond (A), use electrochemical etching method to process original tool electrode tungsten bar (13), preparation more piece tip-like tungsten electrode;
Step 2, in CNT welding pond (B), under microscope (14) visual field, with voltage method, CNT is welded on tungsten electrode needle point;
Step 3, in film fine electroforming pond (C), the position electroforming layer of metal nickel that adopts the method for film fine electroforming that tungsten electrode is connected with CNT;
The accurate shifting axle Z axis (5) that moves through of above-mentioned tool-electrode drives; The XY precision displacement table (9,10) that moves through that above-mentioned tool-electrode is prepared pond (A), CNT welding pond (B), film fine electroforming pond (C) realizes.
2. micro-electrochemical machining processing carbon nano tube tool-electrode preparation method according to claim 1, is characterized in that:
Above-mentioned steps 1 detailed process is as follows: above-mentioned tool-electrode is prepared and in pond (A), had the first corrosion resistant plate (24) with working hole; Electrolyte submergence the first corrosion resistant plate (24); Corrosion resistant plate during work (24) is connected with power cathode, and tool-electrode is connected with positive source; Original tool electrode tungsten bar (13) is immersed to certain depth under electrolysis liquid surface through the working hole on the first corrosion resistant plate (24), start to carry out electrochemical etching; After electrochemical etching after a while, electrode is upwards mentioned to a segment distance, proceed electrochemical etching, after a period of time, upwards mention again a segment distance, proceed electrochemical etching, until etch required diameter.
3. micro-electrochemical machining processing carbon nano tube tool-electrode preparation method according to claim 1, is characterized in that:
Above-mentioned steps 2 detailed processes are as follows: in above-mentioned CNT welding pond (B), have the second corrosion resistant plate (23), the upper multi-walled carbon nano-tubes (16) that is bonded with array with conducting resinl (22) of the second corrosion resistant plate (23), multi-walled carbon nano-tubes during work (16) is connected with positive source by the second corrosion resistant plate (23), and tool-electrode is connected with power cathode, at microscope (14), amplify under visual field, find an outstanding CNT up front, allow tungsten electrode near outstanding CNT, when the distance between CNT and tungsten electrode is 1-10 micron, between applies 8 ~ 30V and exchanges or DC voltage, until CNT is attracted by electrode tip, adjustment precision micropositioner again, make the axis of CNT consistent with the direction of tool-electrode axis, then between applies 30 ~ 60V interchange or DC voltage, between CNT and tool-electrode, there is arc discharge, obtain CNT tool-electrode.
4. micro-electrochemical machining processing carbon nano tube tool-electrode preparation method according to claim 1, is characterized in that:
Above-mentioned steps 3 detailed processes are as follows: a nickel ring (15) suspends in above-mentioned film fine electroforming pond (C); The CNT tool-electrode having bondd, through nickel ring, is then drawn to electroforming solution and injected nickel ring with suction pipe, form the electroforming solution liquid film of thin layer; During work, CNT is connected with power cathode, and nickel ring is connected with power anode; Control the electroforming time, can be by the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT; The thickness of metallic nickel is by regulating current density and the time of electroforming to control, and current density is larger, and the time is longer, and the thickness of nickel dam is thicker.
5. for micro-electrochemical machining processing carbon nano tube tool-electrode preparation method's claimed in claim 1 multifunctional working groove, it is characterized in that: this multifunctional working groove (8) is prepared pond (A), CNT welding pond (B) and film fine electroforming pond (C) by tool-electrode and formed;
Above-mentioned tool-electrode is prepared in pond (A) and is had U-shaped base (21), is fixed wtih the first corrosion resistant plate (24) with working hole on U-shaped base (21);
In above-mentioned CNT welding pond (B), there is U-shaped base (21), on U-shaped base (21), be fixed wtih the second corrosion resistant plate (23), the upper multi-walled carbon nano-tubes (16) that is bonded with array with conducting resinl (22) of the second corrosion resistant plate (23);
In above-mentioned film fine electroforming pond (C), have L-type base (18), a nickel ring (15) suspends on L-type base (18).
6. multifunctional working groove according to claim 5, is characterized in that: the first corrosion resistant plate (24) thickness that above-mentioned tool-electrode is prepared in pond (A) is 1.8-2mm, and described working hole diameter is 4-5mm.
7. multifunctional working groove according to claim 5, is characterized in that: nickel ring (15) diameter in above-mentioned film fine electroforming pond (C) is 4-5mm, and use diameter is that the nickel wire bending of 200 μ m forms.
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CN103252543B (en) * 2013-05-20 2015-05-20 南京航空航天大学 Method and device for electrochemical machining of ultra-thin workpiece
CN103252544B (en) * 2013-05-20 2015-05-20 南京航空航天大学 Method and device for manufacturing of carbon nanometer tube electrode with length controllable and detection of conductivity of carbon nanometer tube electrode
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CN104096932B (en) * 2014-07-09 2016-08-03 清华大学深圳研究生院 The preparation method of a kind of electrochemistry micro Process electrode and preparation facilities
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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

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JP2010058192A (en) * 2008-09-02 2010-03-18 Toshiba Corp Machining electrode, electrochemical machining device, method of electrochemical machining, and method of manufacturing structure
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