CN102107854B - Method for manufacturing multi-walled carbon nanotube electrode - Google Patents
Method for manufacturing multi-walled carbon nanotube electrode Download PDFInfo
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Abstract
The invention relates to a method for manufacturing a multi-walled carbon nanotube electrode with multilayer tube walls participating in electric conduction. The method comprises the following steps: dispersing a multi-walled carbon nanotube on a substrate with an insulating dielectric layer; manufacturing a metal electrode only in contact with the outer-layer tube wall of the multi-walled carbon nanotube by using electron beam lithography and other micro/nano processing technologies; perforating contact parts of the metal electrode and the multi-walled carbon nanotube by using a focused ion beam etching technology; then processing micropores by using a plasma etching method; and depositing metal by using focused ion beams to ensure that the multilayer tube walls of the multi-walled carbon nanotub are all in direct contact with the metal electrode. By utilizing the method provided by the invention, all the multilayer tube walls of the multi-walled carbon nanotube are ensured to participate in electric conduction, and the current bearing capacity of the multi-walled carbon nanotube can be improved; and the method is compatible with an integrated circuit manufacturing process and suitable for manufacturing micro/nano electronic devices by using the single multi-walled carbon nanotube.
Description
Technical field
The present invention relates to the preparation method of multi-walled carbon nanotube electrode, particularly relate to and the integrated circuit fabrication process compatibility, when utilizing multi-walled carbon nano-tubes to make the micro-nano electronic device, can improve the method for making its electrode of multi-walled carbon nano-tubes and metal electrode contact performance.
Background technology
CNT has excellent electricity, mechanics, calorifics and chemical characteristic, aspect a lot of potential application prospect is arranged.Helicity and the caliber arranged along with graphite annulus in the CNT tube wall change, and CNT can present metallicity or semiconductive.Metallic carbon nanotubes, especially multi-walled carbon nano-tubes owing to having very high current carrying capacity, are the ideal materials as following micro-nano electronic device and integrated circuit interconnection wire.Realize that the application of CNT in the micro-nano electronic device also has many problems to need to solve, for example, contact problems between CNT and the metal electrode, it will have a strong impact on the stable of device performance, and effectively controlling and improving CNT is the prerequisite of the reliable and stable nano electron device of manufacturing with the metal electrode contact performance.Report at present about utilizing synthetic single-root carbon nano-tube to make in the work of antetype device and its electrology characteristic of research, realize that the method that CNT contact with metal electrode mainly contains following two kinds: first method be the carbon nanotube dispersed that will synthesize to insulating substrate, be pressed on the CNT by micro-nano process technology making metal electrode; Second method is to utilize metallic nano detecting probe directly to contact CNT.Now specifically describe as follows to these the two kinds methods that realize that CNT contacts with metal electrode:
1. by micro-nano process technology metal electrode is pressed on the CNT: referring to file 1, " electricity of single-root carbon nano-tube is led " (Electrical conductivity of individual carbon nanotubes), be stated from " Nature " 1996, on the Vol.382:54-56; It is with carbon nanotube dispersed to the silicon chip with oxide layer, then utilize FIB induction and deposition tungsten electrode on CNT to form the electricity contact.The electricity contact that forms by this method, because the outer wall that only is multilayer carbon nanotube directly contacts with metal electrode, usually only have outer wall to participate in conduction, and inner layer tube wall does not almost have electric current to flow through, and does not give full play to the due powerful current carrying capacity of multi-walled carbon nano-tubes.
2. utilize metallic nano detecting probe directly to contact CNT: referring to file 2 " the multichannel ballistic transport in the multi-walled carbon nano-tubes " (Multichannel Ballistic Transport in Multiwall Carbon Nanotubes), be stated from " Physical Review Letters " 2005, on the Vol.95:086601; It is by hot filament chemical vapour deposition method multi-walled carbon nano-tubes to be grown on the tungsten filament substrate, with the tungsten filament substrate as one of them electrode, observe at the SEM situ, handle one movably the tungsten nano-probe near the other end of multi-walled carbon nano-tubes, between tungsten nano-probe and CNT, apply a voltage and produce discharge, produce high temperature so that tungsten nano-probe and multi-walled carbon nano-tubes weld together in the contact site, thereby form good Ohmic contact.Measurement result shows that the electricity of this multi-walled carbon nano-tubes leads the G up to (460-490)
0, maximum current reaches 7.27mA, and almost every one deck tube wall of multi-walled carbon nano-tubes has all participated in electric transport process, and its current carrying capacity is greatly improved.But such method is only applicable to the electrology characteristic experimental study of nanotube, and is also incompatible with present integrated circuit fabrication process.
In a word, when utilizing at present synthetic single multi-walled carbon nano-tubes to make antetype device and its electrology characteristic of research, realize that the method that multi-walled carbon nano-tubes contacts with metal electrode is that outer CNT tube wall participates in conduction usually, fail to give full play to the due powerful current carrying capacity of multi-walled carbon nano-tubes, perhaps directly contact simultaneously with the multi-layer wall of CNT by metallic nano detecting probe and improve its current carrying capacity, but such method and integrated circuit fabrication process and incompatible.Although someone proposes to make first metal electrode and places the required metal catalyst particles of carbon nano-tube at electrode tip, and then carbon nano-tube is connected between the metal electrode, but not very good for the control of direction, size and the quantity of the CNT of growing.Therefore, a kind of method for making its electrode that can effectively embody the high current carrying capacity characteristic of multi-walled carbon nano-tubes of development is very important.
Summary of the invention:
The object of the invention is to: the existing shortcoming that only has outer wall to participate in conduction of method that overcomes existing making multi-walled carbon nano-tubes contact electrode, and provide a kind of multi-layer wall to participate in the preparation method of the multi-walled carbon nanotube electrode of conduction, the method can be manufactured the multi-walled carbon nanotube electrode that improves multi-walled carbon nano-tubes and metal electrode contact performance, the multi-layer wall of multi-walled carbon nano-tubes is all directly contacted with metal electrode, reach the purpose that improves the multi-walled carbon nano-tubes current carrying capacity.The method and integrated circuit fabrication process are compatible, are applicable to utilize single multi-walled carbon nano-tubes to make the micro-nano electronic device.
Technical scheme of the present invention is as follows:
The preparation method of multi-walled carbon nanotube electrode provided by the invention, its step is as follows:
1) selects to have the smooth substrate of insulating medium layer 1 as substrate;
2) multi-walled carbon nano-tubes is scattered on the substrate;
The substrate that 3) will be dispersed with multi-walled carbon nano-tubes is put into electron-beam exposure system, selectes a wherein single multi-walled carbon nano-tubes 2, and records the coordinate position of this single multi-walled carbon nano-tubes 2, then substrate is taken out from electron-beam exposure system; Having the substrate surface spin coating positive photoresist of these single many CNTs 2, utilize hot plate to toast; Again substrate is put into electron-beam exposure system, coordinate position according to the described single multi-walled carbon nano-tubes 2 that records before exposes and produces electrode pattern, and substrate is taken out from electron-beam exposure system, after development and photographic fixing, form electrode pattern in the photoresist layer on substrate;
4) adopt coating process having depositing metallic films on the substrate surface of electrode pattern, and put into acetone soln and carry out the solution-off lift-off processing, form the metal electrode 3 that is pressed on this single multi-walled carbon nano-tubes at substrate;
5) the described substrate of step 4) is put into focused ion beam system, in the position punching 4 that the described metal electrode 3 of substrate contacts with multi-walled carbon nano-tubes 2, hole depth penetrates described single multi-walled carbon nano-tubes;
6) then the described substrate of step 4) is put into plasma etching system, with plasma etching to improve the cross section quality of multi-walled carbon nano-tubes in the hole;
7) utilize FIB induction and deposition technology at the long-pending metal 5 of the inner hole deposition of the described substrate of step 4), make between described single multi-walled carbon nano-tubes 2 and the metal electrode 3 directly to contact by metal 5 formation, obtain multi-walled carbon nanotube electrode of the present invention.
In technique scheme, the insulating medium layer 1 described in the step 1) comprises: silica, silicon nitride, aluminium oxide, hafnium oxide and other dielectric.Wherein silica can obtain by the thermal oxide silicon chip, also can obtain by sputtering sedimentation or chemical gaseous phase depositing process; Silicon nitride makes by chemical gaseous phase depositing process usually; Aluminium oxide and hafnium oxide can make by sputtering sedimentation or Atomic layer deposition method.Their thickness is generally the 10-500 nanometer, and concrete thickness is decided according to the actual needs of making device.
In technique scheme, step 2) material dissolves that normally will contain multi-walled carbon nano-tubes on the substrate that multi-walled carbon nano-tubes is scattered in described in is diluted in acetone, alcohol or other solvents, then with dropper with it on substrate, dry after multi-walled carbon nano-tubes namely distribute and become scattered about substrate surface.
In technique scheme, the single multi-walled carbon nano-tubes 2 that searching described in the step 3) is required also records its coordinate position and need to make two or three alignment marks at substrate in advance, in order to determine the sample coordinate system with this, when substrate is put into electron-beam exposure system again, define with these alignment marks equally and determine the sample coordinate system, so that twice sample coordinate system overlaps.
In technique scheme, the coating process described in the step 4) can adopt the metallic target sputtering method, comprises magnetron sputtering, DC glow sputter or ion beam sputtering etc., also can adopt the metal evaporation method, comprising: thermal evaporation, electron beam evaporation etc.; The kind of the metallic film of deposition is decided according to the actual needs that will make device, and the thickness of metallic film can not surpass the photoresist thickness of institute's spin coating, and normally the 1/3-1/2 of photoresist thickness is advisable.
In technique scheme, the drilling technology described in the step 5) can adopt the focused-ion-beam lithography method, also can adopt laser boring method, and the diameter that usually punches is advisable near the multi-walled carbon nano-tubes diameter.
In technique scheme, plasma etch process described in the step 6) can adopt reactive ion etching method, also can adopt other plasma sputtering method, etching gas can adopt oxygen, also can adopt argon gas, etch period is advisable can etch away several carbon atomic layers, is generally 20 seconds to 2 minutes.
In technique scheme, the FIB induction and deposition technology of utilizing in the described step 7) is to utilize the tungstenic organic matter as reacting gas at the long-pending tungsten of inner hole deposition, by this reacting gas is ejected in the hole, make the tungstenic organic substance decomposing with ion beam bombardment simultaneously, the tungsten atomic deposition is in the hole, the carbon oxygen atom that decomposes is taken away by vavuum pump, and the position of tungsten deposition and shape are determined by position and the pattern of ion beam bombardment scanning.
Described tungstenic organic matter is W (CO)
6
The invention has the advantages that:
1. the present invention utilizes the micro-nano process technology such as electron beam exposure after multi-walled carbon nano-tubes is made metal electrode, punch at the position that metal electrode contacts with multi-walled carbon nano-tubes by focused ion beam technology, then utilize method for etching plasma to process aperture, and use the focused ion beam deposition metal, the multi-layer wall of multi-walled carbon nano-tubes is all directly contacted with metal electrode, a kind of method for making its electrode that can improve multi-walled carbon nano-tubes and metal electrode contact performance is provided, thereby has improved the current carrying capacity of multi-walled carbon nano-tubes.
2. in whole technical process, employing all be conventional micro-nano process technology, so the method has good compatibility for integrated circuit fabrication process, be applicable to utilize single multi-walled carbon nano-tubes to make the micro-nano electronic device.
Description of drawings:
Fig. 1 a to Fig. 1 c is the making schematic flow sheet of multi-walled carbon nano-tubes contact electrode of the present invention:
Fig. 1 a is for being scattered in multi-walled carbon nano-tubes in the schematic diagram on the substrate;
Fig. 1 b utilizes micro-nano process technology to make the schematic diagram of metal electrode at single multi-walled carbon nano-tubes;
Fig. 1 c utilizes the focused-ion-beam lithography technology in the punching of position that metal electrode contacts with multi-walled carbon nano-tubes, and with the schematic diagram of plasma treatment;
Fig. 1 d is for utilizing FIB induction and deposition technology plated metal in the hole.
The specific embodiment
Further describe the present invention below by the drawings and specific embodiments.
With reference to Fig. 1, make the multi-walled carbon nano-tubes four electrode test devices of the present embodiment by method of the present invention, its step is as follows:
1) selects the SiO that thermal oxide is made that has of 500 nanometer thickness
2The silicon chip of film is as substrate;
2) with the multi-walled carbon nano-tubes dissolved dilution in spirit solvent, disperse through 1 hour ultrasonic vibration, the alcoholic solution that will contain multi-walled carbon nano-tubes with dropper afterwards drips on substrate, and substrate 50 ℃ of hot plates bakings 2 minutes, distributes multi-walled carbon nano-tubes and becomes scattered about substrate surface;
3) with step 2) the substrate that is dispersed with multi-walled carbon nano-tubes put into Raith 150 electron-beam exposure systems, at the multi-walled carbon nano-tubes of observing under the ESEM pattern on the substrate, a selected single multi-walled carbon nano-tubes also records its coordinate position, then substrate is taken out from electron-beam exposure system; Spin coating thickness is the positive photoresist PMMA of 100 nanometers on the substrate surface of this single multi-walled carbon nano-tubes having, and 180 ℃ of hot plate bakings 1 minute, again described substrate is put into Raith 150 electron-beam exposure systems, coordinate position according to this single multi-walled carbon nano-tubes that records before, four electrode patterns are produced in exposure, again substrate is taken out from Raith 150 electron-beam exposure systems, after development and photographic fixing, form four electrode patterns in the photoresist layer on being dispersed with the substrate of multi-walled carbon nano-tubes;
4) adopt the thermal evaporation film plating process on the substrate of step 3), at first to deposit the titanium film of 5 nanometer thickness, then deposit the golden film of 40 nanometer thickness, and described substrate is put into acetone soln carry out the solution-off lift-off processing, form the metal electrode 3 on the single multi-walled carbon nano-tubes that is pressed on described substrate;
5) the step 4) substrate is put into FEI DB235 focused ion beam system, be 30kV with accelerating potential, line is that the Ga ion pair substrate of 10pA bombards, and is bombarded punching at the position that the metal electrode 3 of substrate contacts with multi-walled carbon nano-tubes 2, and its hole depth penetrates multi-walled carbon nano-tubes 2;
6) the step 5) substrate is put into the reactive ion etching system it is carried out etching; The reaction cavity pressure of described reactive ion etching system is 0.7Pa, Dc bias 100V, power 200W, oxygen flow 20sccm, etch period 30 seconds;
7) then utilize FIB induction and deposition technology at the long-pending tungsten of described inner hole deposition, carry out ion-beam scanning in the position in hole, spray W (CO) by gas injection system
6In the hole, make its decomposition with high-octane ion beam bombardment simultaneously, the tungsten atomic deposition in the hole, is formed directly by tungsten between the multi-layer wall that makes this multi-walled carbon nano-tubes 2 and the metal electrode 3 and contacts, obtain multi-walled carbon nano-tubes four electrode test devices;
Before and after punching, measure respectively the electronic transport character of multi-walled carbon nano-tubes, the result show form new contact by the plated metal that punches again after, the electricity of multi-walled carbon nano-tubes is led and has been improved more than 10 times;
The present embodiment is made the metal measurement electrode of multi-walled carbon nano-tubes at the alumina insulation dielectric layer.
With reference to figure 1, the preparation method of the present embodiment carries out according to the technological process of Fig. 1, is described in detail as follows:
1) silicon chip is put into the Savannah-100 atomic layer deposition system that Cambridge NanoTech Inc produces, at the alumina insulation dielectric layer of silicon chip growth 50 nanometer thickness, bottom silicon can be used as gate electrode when device is measured;
2) with the multi-walled carbon nano-tubes dissolved dilution in spirit solvent, disperse through 1 hour ultrasonic vibration, the alcoholic solution that will contain multi-walled carbon nano-tubes with dropper drips on the silicon substrate with alumina insulation dielectric layer, toasted silicon substrates 1 minute at 50 ℃ hot plates, multi-walled carbon nano-tubes is scattered on the alumina insulation dielectric layer of substrate;
The substrate that 3) will be dispersed with multi-walled carbon nano-tubes is put into Raith 150 electron-beam exposure systems, by the multi-walled carbon nano-tubes on the scanning electron microscopic observation substrate, a selected single multi-walled carbon nano-tubes also records its coordinate position, then substrate is taken out from Raith 150 electron-beam exposure systems; At the positive photoresist PMMA with spin coating 100 nanometer thickness on the substrate surface of this single multi-walled carbon nano-tubes, and 180 ℃ of hot plate bakings 1 minute; Again substrate is put into Raith 150 electron-beam exposure systems, according to the coordinate position that records before this single multi-walled carbon nano-tubes, electrode pattern is produced in exposure, substrate is taken out from Raith 150 electron-beam exposure systems, after development and photographic fixing, form electrode pattern in the photoresist layer on substrate;
4) adopt the thermal evaporation film plating process to have the titanium film that at first deposits 5 nanometer thickness on the surface of electrode pattern at substrate, and then deposit the golden film of 50 nanometer thickness, substrate is put into acetone soln carry out the solution-off lift-off processing, metal membrane-coating solution-off on the photoresist strips down, and stays the metal electrode 3 that is pressed on the described single multi-walled carbon nano-tubes 2;
5) substrate is put into FEI DB235 focused ion beam system, utilize accelerating potential to be 30kV, line is the focusing Ga Ions Bombardment of 10pA, in the position punching that metal electrode contacts with multi-walled carbon nano-tubes, hole depth penetrates multi-walled carbon nano-tubes, then utilizes the Ar ion sputtering to process aperture 1 minute; At last, in the hole, utilize FIB induction and deposition metal platinum, form directly by metal platinum between the multi-layer wall 2 of described this single multi-walled carbon nano-tubes and the metal electrode 3 and contact, just made the metal measurement electrode of making multi-walled carbon nano-tubes at the alumina insulation dielectric layer of the present embodiment.
Claims (9)
1. a multi-layer wall participates in the preparation method of the multi-walled carbon nanotube electrode of conduction, and it may further comprise the steps:
1) selects to have the smooth substrate of insulating medium layer (1) as substrate;
2) multi-walled carbon nano-tubes is scattered on the substrate;
The substrate that 3) will be dispersed with multi-walled carbon nano-tubes is put into electron-beam exposure system, and then a selected wherein single multi-walled carbon nano-tubes (2), and the coordinate position of this single multi-walled carbon nano-tubes (2) of record take out substrate from electron-beam exposure system; Having the substrate surface spin coating positive photoresist of this single multi-walled carbon nano-tubes (2), utilize hot plate to toast; Again substrate is put into electron-beam exposure system, coordinate position according to the described single multi-walled carbon nano-tubes (2) that records before, expose and produce electrode pattern, substrate is taken out from electron-beam exposure system, after development and photographic fixing, form electrode pattern in the photoresist layer on substrate;
4) adopt coating process having depositing metallic films on the substrate surface of electrode pattern, and put into acetone soln and carry out the solution-off lift-off processing, form the metal electrode (3) that is pressed on this single multi-walled carbon nano-tubes at substrate;
5) the described substrate of step 4) is put into focused ion beam system, in the position punching (4) that the described metal electrode (3) of substrate contacts with multi-walled carbon nano-tubes (2), hole depth penetrates described single multi-walled carbon nano-tubes;
6) substrate that then step 5) is obtained is put into plasma etching system, with plasma etching to improve the cross section quality of multi-walled carbon nano-tubes in the hole;
7) utilize the long-pending metal (5) of inner hole deposition of the substrate that FIB induction and deposition technology obtains in step 6), make between described single multi-walled carbon nano-tubes (2) and the metal electrode (3) to form by metal (5) directly to contact, obtain multi-walled carbon nanotube electrode.
2. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, the material of the insulating medium layer described in the described step 1) (1) is silica, silicon nitride, aluminium oxide or hafnium oxide, and its thickness is the 10-500 nanometer.
3. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, multi-walled carbon nano-tubes is scattered on the substrate described step 2) be with the multi-walled carbon nano-tubes dissolved dilution in organic solution, then with dropper with it on substrate, dry after multi-walled carbon nano-tubes namely distribute and become scattered about substrate surface.
4. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 3, it is characterized in that, described organic solution is acetone or alcohol.
5. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, the coating process described in the described step 4) is metallic target sputtering method or metal evaporation method; Described metallic target sputtering method is magnetron sputtering, DC glow sputter or ion beam sputtering; Described metal evaporation method is thermal evaporation or electron beam evaporation; The thickness of the metal film that deposits is the 1/3-1/2 of described positive photoresist thickness.
6. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, the focused-ion-beam lithography punching is adopted in punching in the described step 5), or adopts laser boring; The aperture equals the diameter of described single multi-walled carbon nano-tubes.
7. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, oxygen or argon gas are adopted in described step 6) plasma etching or ion sputtering, and etch period is 20 seconds to 2 minutes.
8. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 1, it is characterized in that, the FIB induction and deposition technology of utilizing in the described step 7) is to utilize the tungstenic organic matter as reacting gas at the long-pending tungsten of inner hole deposition, by this reacting gas is ejected in the hole, make the tungstenic organic substance decomposing with ion beam bombardment simultaneously, the tungsten atomic deposition is in the hole, the carbon oxygen atom that decomposes is taken away by vavuum pump, and the position of tungsten deposition and shape are determined by position and the pattern of ion beam bombardment scanning.
9. participate in the preparation method of the multi-walled carbon nanotube electrode of conduction by multi-layer wall claimed in claim 8, it is characterized in that, described tungstenic organic matter is W (CO)
6
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| CN102412016B (en) * | 2011-07-09 | 2013-05-01 | 电子科技大学 | Method for preparing ordered micron/nano structure array of conducting polymer |
| CN104627957B (en) * | 2015-02-12 | 2016-05-11 | 武汉理工大学 | A kind of manufacture craft of RESEARCH OF PYROCARBON micro-structural electrode and electrical property characterizing method thereof |
| US10847757B2 (en) | 2017-05-04 | 2020-11-24 | Carbon Nanotube Technologies, Llc | Carbon enabled vertical organic light emitting transistors |
| KR102511414B1 (en) * | 2017-05-08 | 2023-03-16 | 아톰 에이치투오, 엘엘씨 | Manufacturing of carbon nanotube thin film transistor backplanes and display integration thereof |
| CN109557160A (en) * | 2018-12-29 | 2019-04-02 | 温州大学 | The method that self assembly has the preparation of the carbon nanotube of nanometer gold bar and carries out biomolecule detection using it |
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