CN103056463A - 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 PDFInfo
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- CN103056463A CN103056463A CN2012105444669A CN201210544466A CN103056463A CN 103056463 A CN103056463 A CN 103056463A CN 2012105444669 A CN2012105444669 A CN 2012105444669A CN 201210544466 A CN201210544466 A CN 201210544466A CN 103056463 A CN103056463 A CN 103056463A
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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
Technical field
The invention belongs to the electrochemistry manufacture field, relate to micro-electrochemical machining processing carbon nano tube tool-electrode preparation method and multifunctional working groove.
Background technology
Along with the development of science and technology, all comprising high-accuracy sub-micron or the structure of nano-scale in modern many new high-tech products, these fine structures often have vital effect.Micro-electrochemical machining processing is a kind of important processing method in the fine manufacturing field.Micro-electrochemical machining processing refers in the microfabrication scope, and the principle of utilizing metal that the Anodic dissolving occurs in electrolyte is carried out the processing method that etching is shaped to material.From processing mechanism, metallic atom work in-process on the 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, the controlled working condition is chosen suitable machined parameters, can realize with the number of ions magnitude material being processed, and satisfies the demand of fine manufacturing technology.
Because tool-electrode does not contact with workpiece in the electrochemical machining process, and it is wide to have the rapidoprint scope, be not subjected 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 processing factor such as locality so that the precision of Electrolyzed Processing be subject to certain restrictions.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 the tool-electrode size, improve the tool-electrode shape, can improve the precision of micro-electrochemical machining processing.
The micro electrode that at present micro-electrochemical machining processing is used mainly is 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 the 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, tungsten filament at original 100 micron diameters mills 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.Complicated ion beam produces equipment but this processing method need to have a cover, and is expensive, also has the defectives 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 CNT is used for Electrolyzed Processing as tool-electrode, the processing yardstick will reach Nano grade.So far, scientists has been carried out research extensively and profoundly to CNT performance and application, and CNT is bonded in plain scan probe formation CNT scan-probe.Method commonly used has: method, voltage preparation method etc. are picked up in conductive adhesive method, chemical vapour deposition technique, scanning.Wherein the voltage preparation method is more easily realized, at first the silicon probe with CNT and metal-coated membrane links to each other with two three-dimensional travelling carriages respectively, the positive pole of CNT one side joint additional power source, and negative pole links to each other with common probe.Very approaching between probe and CNT, about 1-10 micron apart from the time, between applies voltage, can see that under light microscope CNT is truncated, and produces with electric arc simultaneously, the CNT part that is truncated is adhered on the ordinary silicon probe.
The electrode that is used for Electrolyzed Processing not only requires to have good electric conductivity, but also will have the stability in liquid environment.Above-mentioned study general all is CNT is bonded in the silicon needle point or plated on the silicon needle point of layer metal, is usually used in the gaseous environment, is used for scanning probe microscopy, and the adhesion between CNT and the needle point is about 1.2-3.6 μ N.If be applied in the electrolyte environment, CNT is hydrophobic material, and very easily bending in entering the liquid environment process is perhaps owing to adhesion strength is lost not.Scientists provides feasibility to strengthen the bonding strength of CNT and probe for carbon nanotube probes carries out work in solution environmental by the ways such as deposition, plated film on carbon nanotube probes.The King of U.S. Ha Fu university etc., the carbon nanotube probes that uses in test is standby by the CVD legal system, and at SEM deposit carbide, to strengthen its adhesive strength.U.S. Canada nanometer technology center Stevens etc., in experiment by vacuum evaporation ethylenediamine film on the 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 to be carried out 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 kind of micro-electrochemical machining processing carbon nano tube tool-electrode preparation method is characterized in that comprising following process: step 1, in the tool-electrode preparation vessel, and use electrochemical etching method that original tool electrode tungsten bar is processed, 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 the 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 preparation vessel, CNT welding pond, moving through in the XY precision displacement table of film fine electroforming pond are realized.
Above-mentioned steps 1 detailed process can be as follows: above-mentioned tool-electrode prepares the first corrosion resistant plate that has in the pond with working hole; Electrolyte submergence the first corrosion resistant plate; Corrosion resistant plate links to each other with power cathode during work, and tool-electrode links to each other with positive source; The working hole that original tool electrode tungsten bar is passed on the first corrosion resistant plate immerses certain depth under the electrolysis liquid surface, begins to carry out electrochemical etching; Behind electrochemical etching after a while, electrode is upwards mentioned a segment distance, proceed electrochemical etching, upwards mention again a segment distance after a period of time, 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 the pond, is bonded with the multi-walled carbon nano-tubes of array on the second corrosion resistant plate with conducting resinl; Multi-walled carbon nano-tubes links to each other with positive source by the second corrosion resistant plate during work, and tool-electrode links to each other with power cathode; Amplify under the visual field at microscope, find an outstanding CNT up front, allow tungsten electrode near outstanding CNT, when the distance between CNT and the tungsten electrode is the 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 the tool-electrode arc discharge occuring, obtains the CNT tool-electrode.
Above-mentioned steps 3 detailed processes can be as follows: a nickel ring suspends in the said film micro electroforming pond; The CNT tool-electrode that bonding is good passes the nickel ring, then draws electroforming solution and injects the nickel ring with suction pipe, forms the electroforming solution liquid film of thin layer; CNT links to each other with power cathode during work, and the nickel ring links to each other with power anode; The control electroforming time, can be with the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT; The thickness of metallic nickel was controlled by current density and the time of regulating electroforming, and current density is larger, and the time is longer, and the thickness of nickel dam is thicker.
Be used for described micro-electrochemical machining processing carbon nano tube tool-electrode preparation method's multifunctional working groove, it is characterized in that: this multifunctional working groove prepares pond, CNT welding pond and film fine electroforming pond by tool-electrode and forms; Above-mentioned tool-electrode prepares and has U-shaped base in the pond, is fixed wtih the first corrosion resistant plate with working hole on the U-shaped base; Above-mentioned CNT welding has U-shaped base in the pond, is fixed wtih the second corrosion resistant plate on the U-shaped base, is bonded with the multi-walled carbon nano-tubes of array on the second corrosion resistant plate with conducting resinl; The said film micro electroforming has the L-type base in the pond, and a metal ring suspends on the L-type base;
The present invention has the following advantages:
1. the method adopts online preparation CNT tool-electrode, for the preparation of CNT tool-electrode, need not through multiple clamping, reduces in clamping error and the clamping process damage to the CNT tool-electrode.The welding of the preparation of general purpose tool electrode, CNT tool-electrode, and to its post processing of carrying out, all be to carry out at different instrument and equipments generally.The multifunctional working groove that the present invention adopts is divided into three work nests of A, B and C, tool-electrode preparation, CNT welding and micro electroforming is reinforced integrate, and need not to change work nest, and makes at same precision machine tool.Adopt the method, not only reduced error and the number of times of clamping, but also improved the efficient of CNT tool-electrode preparation.
2. the position electroforming layer of metal nickel that adopts liquid-film method that tungsten electrode is connected with CNT.CNT is hydrophobic material, and very easily bending in entering the liquid environment process is perhaps owing to adhesion strength is lost not.In existing research, increase in the method for CNT and probe adhesion strength, what use is at SEM deposit carbide, vacuum evaporation ethylenediamine film.These methods all need expensive equipment and harsh environment, and ethylenediamine or poisonous reagent will be paid special attention to safety in use.If adopt the method for general electroforming with CNT tool-electrode surface casting last layer metal, how the still carbon nanotube electrode that at first will solve enters the problem of electroforming solution, and this has revert to initial point with problem again.What the present invention adopted is the method for liquid film micro electroforming, can address this problem, and the good CNT tool-electrode that will bond first passes the nickel ring, and then electroforming solution is injected the nickel ring with suction pipe, can carry out the electroforming test, and the method is simple and feasible.
3. the present invention adopts the liquid film electrocasting that the CNT tool-electrode is processed, and has increased adhesion strength and electrical conductivity between electrode and the 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 the tool-electrode part, namely increased its electrical conductivity and adhesion strength.
Description of drawings
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 platform;
12. collet; 13. tool-electrode; 14.CCD; 15. metal ring; 16. array carbon nano tube; 17. electroforming solution; 18.L type base; 19. bolt; 20. wire; 21.U type base; 22. conducting resinl; 23. corrosion resistant plate; 24. corrosion resistant plate with holes; 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 places on the XY precision displacement table;
In multifunctional working groove A, use electrochemical etching to prepare more piece tip-like electrode.Be that the corrosion resistant plate with holes 24 of 1.8-2mm is fixed in the A pond on the U-shaped base 21 with thickness, bore dia is 4-5mm on the stainless steel, and corrosion resistant plate is linked to each other with power cathode 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 the electrolysis liquid surface with original tungsten electrode, begin to carry out electrochemical etching, behind electrochemical etching after a while, upwards mention a segment distance, proceed electrochemical etching, upwards mention again a segment distance after a period of time, proceed electrochemical etching, until stop processing after etching required diameter.
After preparing electrode, moving movement major axis X axle 10 will multifunctional working groove B move to electrode under.In B, the multi-walled carbon nano-tubes 16 usefulness conducting resinls 22 of array are bonded on the corrosion resistant plate 23 that is fixed on the base 21, CNT connects the positive pole of power supply by corrosion resistant plate, and this moment, electrode connect power cathode.Be under 1000 times the visual field, to find an outstanding CNT up front in microscope 14 multiplication factors, and the moving three dimension workbench, allow tungsten electrode near outstanding CNT.When the distance between CNT and the 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, the 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 the tool-electrode arc discharge occuring, obtains the CNT tool-electrode;
After obtaining the CNT tool-electrode, moving movement major axis X axle 10 will multifunctional working groove C move to tool-electrode under.Metal ring 15 is fixed on the L-type base 18, and one section of annulus is unsettled, and metal ring 15 diameters are 4-5mm, is to be that the nickel wire bending of 200 μ m forms with diameter.The CNT tool-electrode that this moment, just bonding was good first passes the nickel ring, then draws electroforming solution and injects the nickel ring with suction pipe, forms the electroforming solution liquid film of thin layer.The CNT instrument connects power cathode, and the nickel ring connects power anode, the control electroforming time, and can be with the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT.The thickness of metallic nickel can be controlled by current density and the time of regulating electroforming.
Claims (6)
1. micro-electrochemical machining processing carbon nano tube tool-electrode preparation method is characterized in that comprising following process:
Step 1, in tool-electrode preparation vessel (A), use electrochemical etching method that original tool electrode tungsten bar (13) is processed, 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 the 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; Above-mentioned tool-electrode preparation vessel (A), CNT welding pond (B), moving through in XY precision displacement table (9,10) of film fine electroforming pond (C) are realized.
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 prepares the first corrosion resistant plate (24) that has in the pond (A) with working hole; Electrolyte submergence the first corrosion resistant plate (24); Corrosion resistant plate during work (24) links to each other with power cathode, and tool-electrode links to each other with positive source; The working hole that original tool electrode tungsten bar (13) is passed on the first corrosion resistant plate (24) immerses certain depth under the electrolysis liquid surface, begins to carry out electrochemical etching; Behind electrochemical etching after a while, electrode is upwards mentioned a segment distance, proceed electrochemical etching, upwards mention again a segment distance after a period of time, 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: have the second corrosion resistant plate (23) in the above-mentioned CNT welding pond (B), 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) links to each other with positive source by the second corrosion resistant plate (23), and tool-electrode links to each other with power cathode; Amplify under the visual field at microscope (14), find an outstanding CNT up front, allow tungsten electrode near outstanding CNT, when the distance between CNT and the tungsten electrode is the 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 the tool-electrode arc discharge occuring, obtains the 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 the said film micro electroforming pond (C); The CNT tool-electrode that bonding is good passes the nickel ring, then draws electroforming solution and injects the nickel ring with suction pipe, forms the electroforming solution liquid film of thin layer; CNT links to each other with power cathode during work, and the nickel ring links to each other with power anode; The control electroforming time, can be with the part electroforming layer of metal nickel of the bonding of tungsten electrode and CNT; The thickness of metallic nickel was controlled by current density and the time of regulating electroforming, and current density is larger, and the time is longer, and the thickness of nickel dam is thicker.
5. be used 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) prepares pond (A), CNT welding pond (B) and film fine electroforming pond (C) by tool-electrode and forms;
Above-mentioned tool-electrode prepares and has U-shaped base (21) in the pond (A), is fixed wtih the first corrosion resistant plate (24) with working hole on the U-shaped base (21);
Have U-shaped base (21) in the above-mentioned CNT welding pond (B), be fixed wtih the second corrosion resistant plate (23) on the U-shaped base (21), the upper multi-walled carbon nano-tubes (16) that is bonded with array with conducting resinl (22) of the second corrosion resistant plate (23);
Have L-type base (18) in the said film micro electroforming pond (C), a metal ring (15) suspends on the L-type base (18);
Multifunctional working groove according to claim 5 is characterized in that: the first corrosion resistant plate (24) thickness that above-mentioned tool-electrode prepares in the pond (A) is 1.8-2mm, and described working hole diameter is 4-5mm.
6. multifunctional working groove according to claim 5, it is characterized in that: metal ring (15) diameter in the said film micro electroforming pond (C) is 4-5mm, using diameter is that the nickel wire bending of 200 μ m forms.
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