CN203292634U - Device for preparing electrode of carbon nanometer tube with controllable length and for detecting electrical conductivity - Google Patents
Device for preparing electrode of carbon nanometer tube with controllable length and for detecting electrical conductivity Download PDFInfo
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- CN203292634U CN203292634U CN2013202756207U CN201320275620U CN203292634U CN 203292634 U CN203292634 U CN 203292634U CN 2013202756207 U CN2013202756207 U CN 2013202756207U CN 201320275620 U CN201320275620 U CN 201320275620U CN 203292634 U CN203292634 U CN 203292634U
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Abstract
The utility model relates to a device for preparing an electrode of a carbon nanometer tube with the controllable length and for detecting electrical conductivity, and belongs to the field of precise micro-electrochemistry machining. The device mainly comprises two sets of three-dimensional tender-moving control panels. A first loading platform (7) is used for clamping a test tungsten needle (12) in the process of preparing; a second loading platform (6) is composed of a carbon nanometer tube electrode preparing area (A) and an electrical conductivity detecting area (B), wherein the carbon nanometer tube electrode preparing area (A) is used for fixing conducting resin (14) which is adhered to an arrayed carbon nanometer tube, and the electrical conductivity detecting area (B) is used for fixing a probe (15). The carbon nanometer tube with a certain length is welded to a tungsten needle point to prepare the carbon nanometer tube electrode, on-line electrical conductivity is carried out, the number of clamping errors and the damage to the carbon nanometer tube electrode in the process of clamping are reduced, machining efficiency is effectively improved, and machining cost is reduced.
Description
Technical field
The utility model relates to a kind of length controllable carbon nanotube electrode preparation and electric conductivity checkout gear, belongs to precise fine electrochemistry manufacture field.
Background technology
Development along with science and technology and modern industry, the microminiaturization of functional structure has become the development trend of the various fields such as Aero-Space, biomedical engineering and precision instrument, physical dimension also reduces to micron accordingly, or even Nano grade, so nanofabrication technique becomes the focus of Chinese scholars research.Nanofabrication technique mainly contains at present: nano impression, FIB, the accurate LIGA of LIGA/, micro-electrochemical machining, femtosecond laser processing etc.Wherein, the micro-electrochemical machining process technology is from processing mechanism, and tool cathode is lossless, and the workpiece anode, with the ionic species ablation, therefore has the working ability of ion yardstick in process, be a kind of nanofabrication technique that development potentiality is arranged very much.German MPG adopted the ultrashort width pulse current technique of nanosecond in 2000, the metal 3 D complex die cavity of tens of micro-meter scales is processed in success, after further research, obtain new progress, process the approximately wide groove of 90nm, fully showed the processing potentiality of micro-electrochemical machining process technology in nanometer manufacturing field.
Because tool-electrode in electrochemical machining process does not contact with workpiece, 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, the micro-electrochemical machining process technology has been successfully applied to the fields such as precision instrument, biomedicine, national defense industry.But have the polytropy in dispersion corrosion, electric field and flow field, the factors such as processing locality make the precision of Electrolyzed Processing be subject to certain restrictions.Wherein, the shape of tool-electrode and yardstick have a significant impact precision and the crudy of micro-electrochemical machining processing, are the key factors that the micro-electrochemical machining process technology further develops to the nanoscale Electrolyzed Processing.The nanoscale electrode, as the instrument of nanometer Electrolyzed Processing, is the essential condition of carrying out the nanometer Electrolyzed Processing, and its characteristic size directly affects size and the precision of nanometer Electrolyzed Processing.
Method for preparing nano electrode commonly used has electrochemical etching, focused ion milling and self-assembling technique etc. at present.The electrode needle point arc radius that electrochemical etching is prepared is generally in 10 ~ 100nm scope, and eletrode tip is cone-shaped and tapering is larger, if adopt this kind electrode to carry out Electrolyzed Processing, the structure side wall that processes has very large tapering; FIB milling technology processing nanometer tool-electrode is used in the cooperations such as the A.L.Trimmer of Virginia, USA university and R.Schuster, on the tungsten filament end face of original diameter 100 μ m the machining feature size at 100nm with interior planar shaping electrode, but the focused ion milling device is very expensive, prepares the electrode cost high; Self-assembling technique is the Main Means for preparing nanoscale structures,, because its assembling process is automatic, spontaneous, does not need expensive process equipment, develops quite ripely in the preparation research of flying-spot microscope probe.
CNT (carbon nanotube, CNT) since Japanese scientist S.Iijima in 1991 finds first, because of its unique structure and the good performances such as mechanics, electricity and chemistry, present wide application prospect in electrochemical field, the micro-structurals such as carbon nano tube sensor, ultracapacitor, fuel cell have become the focus of nanotechnology research.The tool-electrode preparation method that receives based on CNT mainly contains conductive adhesive method, carbon sedimentation, Chemical assembly method and voltage preparation method etc.Wherein, voltage preparation method technique is simple, and manufacturing cycle is short, and processing cost is low, and bond strength is better, is the important method of AFM or the preparation of STM probe.The R.Stevens of California, USA university etc. welds together the silicon probe of CNT and plating cobalt or nickel film by voltage method; The mode that the employing voltage methods such as the H.Nishijima of Osaka, Japan university combine with the carbon sedimentation is fixed on CNT on the silicon probe; The J.Tang of North Carolina, US university etc. improves the voltage preparation method, adopts bidirectional electrophoresis technique to prepare the CNT scan-probe.Due to the electric conductivity of the CNT difference with self structure, not only metallicity can be shown but also semiconductive can be shown, and the contact performance between CNT and metal electrode is being played the part of important effect in the CNT function element, directly affects performance, reliability and the applicability of device.Therefore, when preparing the CNT function element, the research of electrology characteristic is indispensable, and this respect has caused lot of domestic and foreign scholar's very big concern.The Germany Y.Woo of Ma Pu research institute etc. has studied metallicity is connected the electrical characteristics that CNT is connected with the metal Pd electrode respectively with semiconductive; The R.Martel of American I BM research institute etc. is deposited on CNT between metal Co or Ti electrode, studies its electrical characteristics as field-effect transistor; The C-V characteristic that metallic carbon nanotubes is connected with the Cr/Au electrode has been studied in hypo etc. by graduate school of the Chinese Academy of Sciences, and utilizes the method for AFM plating Pt probe spot welding to effectively reduce contact resistance between CNT and metal electrode.
At present, the voltage preparation method is subject to the impact of silicon electrode electric conductivity, still need to improve welding quality by other householder methods, and most ancillary methods needs expensive experimental facilities and harsher experimental situation.Tungsten has good electric conductivity and corrosion resistance, it is a kind of application electrode material very widely, as the tool-electrode of micro-nano processing, but by suitable method, CNT is welded on tungsten electrode the research for preparing tool-electrode and be applied to the nanometer Electrolyzed Processing also seldom., because the electric conductivity of tool-electrode is the necessary factor that carries out the experimental study of micro-nano Electrolyzed Processing, therefore need a kind of simple and easy to do method to detect the electric conductivity of carbon nanotube electrode.
The utility model content
The purpose of this utility model is for the problems referred to above, a kind of length controllable carbon nanotube electrode preparation and electric conductivity checkout gear are proposed, the CNT of certain-length is welded on tungsten tip and is prepared into carbon nanotube electrode, and carry out online electric conductivity and detect, reduced in clamping error and clamping process the damage to carbon nanotube electrode, effectively improve working (machining) efficiency, reduced processing cost.
The online preparation method of a kind of length controllable carbon nanotube electrode, it is characterized in that: the conducting resinl that step 1. will be stained with array carbon nano tube is fixed on the second objective table and is connected with dc power anode, will test tungsten pin clamping and be connected with dc power cathode on the first objective table; Under microscopical visual field, at first find in array carbon nano tube outstanding CNT, needle point and distance contacts at the default position of front end of outstanding CNT, apply the lasting 10-20s of 3-5V voltage, make CNT in this position generation local defect; Step 2. allows the needle point of testing the tungsten pin near outstanding CNT, keep 2-5 μ m gap, between adds 6-10V voltage, CNT is attracted by needle point and is stretching under the effect of electric field force, its axis direction is parallel with the needle point axis, then slowly increase voltage, when voltage adds between 15～55V, will produce the electric discharge phenomena of moment between needle point and CNT, CNT welds together with needle point under the moment of electric arc high temperature action, and at self fault location, be truncated, thereby obtain the carbon nanotube electrode of preset length; After the carbon nanotube electrode preparation of step 3. preset length is completed, the voltage of dc source is 10-20V, make preset length carbon nanotube electrode constantly approach foremost in array carbon nano tube outstanding CNT, the carbon nanotube electrode of preset length can be blocked a part by galvanic corrosion under the effect of electric field, thereby obtains the carbon nanotube electrode of appropriate length.
According to the online preparation method of above-mentioned length controllable carbon nanotube electrode, it is characterized in that: also comprise the online electric conductivity testing process of step 4., probe is fixed on the second objective table and is connected with dc power anode, the carbon nanotube electrode of prepared appropriate length is connected with dc power cathode on the first objective table, regulate the relative position of carbon nanotube electrode and probe, its top is docked with probe; Improve both contact performancies at the end coated conductive silver glue of probe, and by adding in advance 1-5V voltage, monitor the short circuit current signal of accurate microampere meter, guarantee the good contact of end, then adopt volt-ampere circuit method to detect online the electric conductivity of carbon nanotube electrode.
Realize the online preparation method's of above-mentioned length controllable carbon nanotube electrode device, it is characterized in that: this device mainly comprises the two three-dimensional fine motion consoles of cover, the three-dimensional fine motion console of first set is comprised of the first X-axis, the first Y-axis, the first Z axis and the first piezoelectric ceramics of being installed on the first Z axis, and the second three-dimensional fine motion console of cover is comprised of the second X-axis, the second Y-axis, the second Z axis and the second piezoelectric ceramics of being installed on the second Z axis; This device also comprises the first objective table of being installed on the first piezoelectric ceramics, is installed on the second objective table on the second piezoelectric ceramics, and vision-aided system;
Above-mentioned the first objective table for the preparation of the time clamping test tungsten pin;
Above-mentioned the second objective table by carbon nanotube electrode prepare regional A, electric conductivity surveyed area B forms;
Above-mentioned carbon nanotube electrode prepares regional A and is used for fixedly being stained with the conducting resinl of array carbon nano tube;
Above-mentioned electric conductivity surveyed area B is used for stationary probe.
The beneficial effects of the utility model are:
1, the utility model is made local defect by the homemade method of defect on outstanding CNT, to obtain the carbon nanotube electrode of preset length.Detailed process is that the tungsten pin is contacted with the predeterminated position of CNT, applies 3-5V voltage and continues 10-20s, utilizes the fuel factor of electric current in circuit to produce suitable local joule heat, makes CNT produce local defect at the position that contacts with the tungsten pin.
2, the utility model will be tested the needle point of tungsten pin and outstanding CNT maintenance 2-5 μ m gap, thereby between adds 6-10V voltage and produces certain electric field force and CNT is attracted stretching, make its axis direction parallel with the needle point axis, can effectively control like this linearity of the rear carbon nanotube electrode of welding; Then adopting suitable voltage to produce arc discharge is welded on the CNT of preset length on tungsten tip and prepares carbon nanotube electrode, and adopt electro-erosion process to carry out brachymemma to the carbon nanotube electrode of preset length in circuit in position, thereby obtain the carbon nanotube electrode of appropriate length.During by the electro-erosion process shortening carbon nano-tube, when voltage is 10-20V, can effectively control the length of at every turn blocking in 100nm-1 μ m scope, voltage during less than 10V, can not produce electric arc effectively, and galvanic corrosion efficiency is lower; Voltage is during greater than 20V, and the length of each brachymemma is larger, easily causes galvanic corrosion excessive, makes the length of CNT too short.The said method canbe used on line the quick preparation of length-controllable carbon nanotube electrode, easy and simple to handle, feasible effectively.
When 3, the utility model prepared carbon nanotube electrode, the needle point arc radius of test tungsten pin in the 0-1000nm scope, when voltage meets certain condition respectively, can produce effective arc discharge.When producing effective arc discharge, the needle point size is less, the easier top that CNT is welded on needle point; The needle point size is larger, more is not easy to control the directionality of CNT welding, easily causes CNT to be welded on needle point top phenomenon on every side.The advantage of utilizing arc discharge to prepare carbon nanotube electrode is to control easy, and preparation efficiency is high, and welding quality is better.
4, device of the present utility model can carry out online electric conductivity and detects, and simple process, need not multiple clamping, has not only reduced in clamping error and clamping process the damage to carbon nanotube electrode, and has improved working (machining) efficiency, has reduced processing cost.
Description of drawings
Fig. 1 is the system diagram that the online preparation of length controllable carbon nanotube electrode and electric conductivity detect;
Fig. 2 is the experimental subjects regional distribution chart on objective table 6;
Fig. 3 is that the self-control of CNT defect and electrode welding prepare schematic diagram;
Fig. 4 is that electro-erosion process is controlled carbon nanotube electrode length schematic diagram
Fig. 5 is carbon nanotube electrode conducting performance test schematic diagram;
Its label title is respectively: 1. the second X-axis; 2. the second Y-axis; 3. the second Z axis; 4. motion control card; 5. the second piezoelectric ceramics; 6. the second objective table; 7. the first objective table; 8. the first piezoelectric ceramics; 9. the first Z axis; 10. the first Y-axis; 11. the first X-axis; 12. test tungsten pin; 13. microscopical object lens; 14. conducting resinl; 15. probe; 16. Unidirectional transparent protective glass; 17. industrial computer; 18. data collecting card; 19. dc source; 20. accurate microampere meter; 21. platform base; 22. array carbon nano tube; 23. outstanding CNT; 24. local defect; 25. electric arc; 26. the carbon nanotube electrode of preset length; 27. the carbon nanotube electrode of appropriate length; A. the carbon nanotube electrode preparation is regional; B. electric conductivity surveyed area.
The specific embodiment
In Fig. 1, the online preparation of length controllable carbon nanotube electrode and the system diagram that electric conductivity detects, mainly be comprised of kinetic control system, current signal monitoring system and vision-aided system etc.Dc source can be exported 0～61V continuous voltage, kinetic control system is comprised of the two three-dimensional fine motion consoles of cover and motion control card, the three-dimensional fine motion console of first set comprises the first X-axis 11, the first Y-axis 10, the first Z axis 9 and is installed on the first piezoelectric ceramics 8 on the first Z axis, the second three-dimensional fine motion console of cover comprises the second X-axis 1, the second Y-axis 2, the second Z axis 3 and is installed on the second piezoelectric ceramics 5 on the second Z axis, and motion control card 4 is controlled the movement locus of X/Y/Z.In the two three-dimensional fine motion consoles of cover, the displacement resolution of X-axis, Y-axis, Z axis are 100nm/step, and the displacement resolution of piezoelectric ceramics is 10nm/step, control minim gaps between needle points and CNT by controlling the two three-dimensional fine motion consoles of cover in test.The current signal monitoring system is comprised of accurate microampere meter 20 and data collecting card 18, is used for the short-circuit signal that the monitoring test needle point contacts with CNT, and gathers the current signal in process.Vision-aided system, can select microscopical object lens 13 to amplify the visual field of different multiples, and utilize digital camera head with the image data transmission in object lens to industrial computer, process of the test is carried out real-time monitored and IMAQ.
To test tungsten pin 12 clampings on the first objective table 7, with the negative pole of dc source 19, be connected; The conducting resinl 14, the probe 15 that are stained with array carbon nano tube are separately fixed on the second objective table 6, with the positive pole of dc source 19, are connected.The connecting portion of objective table and piezoelectric ceramics need keep insulation.
Prepare in regional A, under the visual field of microscopical object lens 13, at first find CNT 23 outstanding in array carbon nano tube 22, regulating the first X-axis 11 and the first piezoelectric ceramics 8 contacts at the position of the front end preset length of outstanding CNT tungsten tip and distance, apply 3-5V voltage and continue 10-20s, make CNT produce local defect 24 at this position.
Then regulate the first X-axis 11 and allow the needle point of tungsten pin near outstanding CNT, keep 2-5 μ m gap, between adds 6-10V voltage, and CNT is attracted by needle point and be stretching under the effect of electric field force, and its axis direction is parallel with the needle point axis; Then slowly increase voltage, when voltage adds between 15～55V, will produce the electric discharge phenomena of moment between needle point and CNT, CNT welds together with needle point under the moment of electric arc 25 high temperature action, and at defect 24 places of self, being truncated, thereby the carbon nanotube electrode 26 of acquisition preset length.The needle point arc radius of test tungsten pin generally in the 0-1000nm scope, when voltage meets certain condition respectively, can produce effective arc discharge.The needle point arc radius of tungsten pin is in 0～300nm, and effectively discharge voltage is at 15-30V; In 300～700nm, effectively discharge voltage is in the 30-40V left and right; In 700～1000nm, effectively discharge voltage is at 40-50V.When producing effective arc discharge, the needle point size is less, the easier top that CNT is welded on needle point; The needle point size is larger, more is not easy to control the directionality of CNT welding, easily causes CNT to be welded on needle point top phenomenon on every side.While preparing the CNT tool-electrode, select the less tungsten pin of tip size as far as possible, must control suitable discharge voltage well, voltage is excessive not only can make most CNTs stick on needle point or sidewall, also easily cause the sintering of CNT, the character of CNT self is exerted an influence.
When the needle point arc radius of tungsten pin is about 100nm, the gap of needle point and CNT keeps 2 μ m, and attraction voltage is 8V, when discharge voltage is 25V, has successfully prepared carbon nanotube electrode; When the needle point arc radius of tungsten pin is about 300nm, the gap of needle point and CNT keeps 2 μ m, and attraction voltage is 8V, when discharge voltage is 35V, has successfully prepared carbon nanotube electrode.
After preparing carbon nanotube electrode, the voltage of dc source 19 is 5-20V, that regulates that the first X-axis 11 and the first piezoelectric ceramics 8 make carbon nanotube electrode constantly approaches outstanding CNT 23 foremost, CNT can be blocked a part by galvanic corrosion under the effect of electric arc 25, characteristic due to CNT self, CNT can form again at the position of blocking the hemispherical tip of complete rule, thereby obtains the carbon nanotube electrode 27 of appropriate length.
After obtaining the carbon nanotube electrode of appropriate length, regulate the first X-axis 11, the first Y-axis 10, the first Z axis 9 and the second X-axis 1, the second Y-axis 2, the second Z axis 3 enters in electric conductivity surveyed area B, probe 15 is fixed on the second objective table 6 and is connected with dc source 19 is anodal, carbon nanotube electrode is connected with dc source 19 negative poles, further control the relative position of the first X-axis 11, the first piezoelectric ceramics 8, the second piezoelectric ceramics 5 adjusting carbon nanotube electrodes and probe, its top is docked with probe.The needle point arc radius of probe is 1-3 μ m, can realize good focusing at same amplification visual field middle probe and tungsten pin, improve both contact performancies at the appropriate conductive silver glue of the end coated of probe, and by adding in advance 1-5V voltage, monitor the short circuit current signal of accurate microampere meter 20, guarantee the front end of carbon nanotube electrode and the good contact of probe tips, then adopt volt-ampere circuit method to detect online the electric conductivity of carbon nanotube electrode.
Claims (1)
1. a length controllable carbon nanotube electrode prepares and the electric conductivity checkout gear, it is characterized in that:
This device mainly comprises the two three-dimensional fine motion consoles of cover, the three-dimensional fine motion console of first set is comprised of the first X-axis (11), the first Y-axis (10), the first Z axis (9) and the first piezoelectric ceramics (8) of being installed on the first Z axis (9), and second overlaps three-dimensional fine motion console is comprised of the second X-axis (1), the second Y-axis (2), the second Z axis (3) and the second piezoelectric ceramics (5) of being installed on the second Z axis (3); This device also comprises the first objective table (7) of being installed on the first piezoelectric ceramics (8), is installed on the second objective table (6) on the second piezoelectric ceramics (5), and vision-aided system;
Above-mentioned the first objective table (7) for the preparation of the time clamping test tungsten pin (12);
Above-mentioned the second objective table (6) is comprised of carbon nanotube electrode preparation zone (A), electric conductivity surveyed area (B);
Above-mentioned carbon nanotube electrode preparation zone (A) is used for fixedly being stained with the conducting resinl (14) of array carbon nano tube;
Above-mentioned electric conductivity surveyed area (B) is used for stationary probe (15).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013202756207U CN203292634U (en) | 2013-05-20 | 2013-05-20 | Device for preparing electrode of carbon nanometer tube with controllable length and for detecting electrical conductivity |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013202756207U CN203292634U (en) | 2013-05-20 | 2013-05-20 | Device for preparing electrode of carbon nanometer tube with controllable length and for detecting electrical conductivity |
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| CN2013202756207U Withdrawn - After Issue CN203292634U (en) | 2013-05-20 | 2013-05-20 | Device for preparing electrode of carbon nanometer tube with controllable length and for detecting electrical conductivity |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103252544A (en) * | 2013-05-20 | 2013-08-21 | 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 |
| CN105731369A (en) * | 2016-02-26 | 2016-07-06 | 东南大学 | Device and method for bonding indium tin oxide (ITO) nanowires at room temperature |
| CN114571014A (en) * | 2020-11-30 | 2022-06-03 | 六和机械股份有限公司 | HCU electrochemical deburring system and processing method thereof |
-
2013
- 2013-05-20 CN CN2013202756207U patent/CN203292634U/en not_active Withdrawn - After Issue
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103252544A (en) * | 2013-05-20 | 2013-08-21 | 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 |
| 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 |
| CN105731369A (en) * | 2016-02-26 | 2016-07-06 | 东南大学 | Device and method for bonding indium tin oxide (ITO) nanowires at room temperature |
| CN105731369B (en) * | 2016-02-26 | 2017-05-31 | 东南大学 | A kind of apparatus and method of room-temperature bonding ITO nano wires |
| CN114571014A (en) * | 2020-11-30 | 2022-06-03 | 六和机械股份有限公司 | HCU electrochemical deburring system and processing method thereof |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Meng Lingchao Inventor after: Zeng Yongbin Inventor after: Qu Ningsong Inventor before: Meng Lingchao Inventor before: Zeng Yongbin Inventor before: Qu Ningsong Inventor before: Zhu Di |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: MENG LINGCHAO CENG YONGBIN QU NINGSONG ZHU DI TO: MENG LINGCHAO CENG YONGBIN QU NINGSONG |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20131120 Effective date of abandoning: 20150520 |
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| RGAV | Abandon patent right to avoid regrant |