CN101226879B - Method for preparation of nanometer clearance electrode - Google Patents
Method for preparation of nanometer clearance electrode Download PDFInfo
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- CN101226879B CN101226879B CN2007100628326A CN200710062832A CN101226879B CN 101226879 B CN101226879 B CN 101226879B CN 2007100628326 A CN2007100628326 A CN 2007100628326A CN 200710062832 A CN200710062832 A CN 200710062832A CN 101226879 B CN101226879 B CN 101226879B
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Abstract
A process for preparing nanometer-spaced electrodes comprises steps of preparing electrode pairs with larger gaps on nano materials which can not be destructed by electron beams, adsorbing raw material molecules induced and deposited by the electron beams on the surface of the electrode pairs, focusing the electron beams on gap areas of the electrode pairs and stopping irradiation by the electron beams to prepare and obtain the nanometer-spaced electrodes, when the gaps of the electrodes achieve the required width. Compared with the traditional process, the gaps of the electrodes can be observed in-situ in the process of preparation of the invention, thereby accurately controlling the gaps of the nanometer-spaced electrodes. Simultaneously, the invention has the advantages of convenient operation, simplicity and feasibility and high success rate, which is favorable for increasing preparing efficiency of the nanometer-spaced electrodes. The prepared nanometer-spaced electrodes have quite wide gap range from 2 nanometers to 100 nanometers, which is extremely significant for the control and application of nano and molecular devices.
Description
Technical field
The present invention relates to a kind of preparation method of nano-electrode, relate to a kind of e-beam induced deposition legal system particularly and be equipped with nano-gap electrode.
Background technology
Molecular electronic device is as electronic device of future generation, and the nearly more than ten years are the focus of scientific circles' research all the time.Obtained a series of major progresses recent years, but some problem is not solved effectively all the time, hampers further developing of molecular electronics.Wherein the preparation of nano-gap electrode is exactly a difficult problem of being badly in need of solution.To prepare the molecule clearance electrode exactly because realize the first step of molecular electronics, make electrode the gap just with the consistent size that will be connected molecule.How a lot of researchers solve this difficult problem in research, have had some to compare successful method at present and have prepared the nano-electrode of this control gap, such as disconnected connection (break junction method, Reed M.A.; Zhou C.; Muller C.J.Science 1997,127,193), electrochemical deposition method (electrochemicaldeposition method, Qing Q.; Chen F.; Li P.G.; Tang W. H.; Liu Z.F.Angew.Chem.Int.Ed.2005,44,7771), nano wire template (nanowire lithography, Qin L.; Park S.; Huang L; Mirkin C.A.Science 2005,309,113) or the like.Yet these methods still do not solve this difficult problem fully.Can't in the process of preparation nano-electrode, realize the real-time observation of original position at present, therefore accurately control electrode with gap width remain and be difficult to realize.
E-beam induced deposition method (EBID) is a kind ofly to make molecule in the scanning area take place decompose and go out at its scanning area surface deposition the method for nanostructure by high density electron beam.This method is used through the micro-nano manufacture field of being everlasting, and is used for the nano-pattern of the various structures of processing and preparing.This method also is used to connect and handle nano material (Wang M. simultaneously; Wang J.; Chen Q.; Peng L-M.Adv.Funct.Mater.2005,15,1825).All carry out in scanning electron microscopy or transmission electron microscope under a lot of situations of e-beam induced deposition, therefore can observe it in the e-beam induced deposition process in situ carries out situation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-gap electrode.
For achieving the above object, nano-gap electrode preparation method provided by the invention, its concrete steps are as follows:
A) preparation has the electrode pair in gap greatly on the nano material that not destroyed by electron beam;
B) at the raw molecule of the surface adsorption e-beam induced deposition of electrode pair;
C) electron beam is focused on the gap area of electrode pair;
D) when electrode gap reaches required width, stop the electron beam irradiation, prepare nano-gap electrode.
Described preparation method, wherein, step a adopts photoetching technique, electron beam lithography, electric current ablation technology, disconnected knot technology, electrochemical deposition technique, nano wire mould plate technique or focused ion beam ablation technology to prepare electrode pair.
Described preparation method, wherein, the nano material that not destroyed by electron beam is metal, inorganic semiconductor material or conductivity organic material.
Described preparation method, wherein, the nano material that not destroyed by electron beam is gold, silver, copper, iron, aluminium, silicon, germanium, poly-enedioxy thiophene or carbon nano-tube.
Described preparation method, wherein, the electron beam energy of step c is 0.1 to 1000 kiloelectron-volt.
Described preparation method, wherein, the electron beam density of step c is 105 to 1010 amperes every square metre.
Described preparation method, wherein, the electrode gap of steps d is 2 to 100 nanometers.
The present invention has following feature and advantage:
1) the present invention has realized the in-situ observation in the nano-gap electrode preparation process first, thereby makes that the control of electrode gap is effective more and accurate.
2) the present invention compares with traditional method, and is easy to operate, simple and feasible, and the success rate height helps improving the preparation efficiency of nano-gap electrode.
3) interstice coverage of the nano-gap electrode of the present invention's preparation is very big, can be 2 nanometer to 100 nanometers, and this preparation and application for nanometer and molecular device has very important meaning.
Description of drawings
Fig. 1 is for being distributed in the electron scanning micrograph of carbon nano-tube between two titanium electrodes among the present invention.
Fig. 2 among the present invention at the electric current back (a) of ablating, 2 minutes (b) of electron beam irradiation, 4 minutes (c) of electron beam irradiation, the electron scanning micrograph of the carbon nanotube electrode of electron beam irradiation 6 minutes (d).
Fig. 3 is that the electrode of 2 nanometers is before the dna molecular assembling and the i-v curve after assembling for the gap for preparing among the present invention.
Fig. 4 for e-beam induced deposition among the present invention before the back electron scanning micrograph of the carbon nanotube electrode of (b) of (a) and deposition.
Embodiment
The method that the present invention prepares nano-gap electrode is to shine previously prepared electrode by electron beam in scanning electron microscopy, the material of depositing electrically conductive makes electrode gap reduce on electrode, pass through the observation electrode spacing of scanning electron microscopy original position simultaneously, when reaching required electrode spacing, stop the electron beam irradiation, thus the nano-gap electrode of preparation controllably with a certain gap width.
Preparation method of the present invention based on principle be: in scanning electron microscopy, shine previously prepared electrode with highdensity electron beam, the secondary electron of electron beam and generation thereof will make the molecule that is adsorbed on electrode surface that complicated chemical reaction takes place, be deposited on the surface of electrode after the decomposition, thereby make electrode broaden, the spacing of electrode diminishes gradually.
Specifically, the preparation method of nano-gap electrode provided by the invention utilizes the e-beam induced deposition technology, and its step is as follows:
A) has the electrode pair in big gap with at present general electrode preparation method (as: photoetching technique, electron beam lithography, electric current ablation technology, disconnected knot technology, electrochemical deposition technique, nano wire mould plate technique or focused ion beam ablation technology etc.) preparation.
B) at the raw molecule of the surface adsorption e-beam induced deposition of electrode.
C) in scanning electron microscopy, (electron beam energy is 0.1 to 1000 kiloelectron-volt, and electron beam density is 10 with electron beam
5To 10
10Every square metre of ampere) focuses on the electrode gap zone, the situation that while home position observation e-beam induced deposition and electrode gap reduce.
D) when electrode gap reaches required width (2 to 100 nanometer), stop the electron beam irradiation.Thereby nano-gap electrode prepares successfully.
The present invention is described in detail below in conjunction with accompanying drawing:
The first step, by photoetching technique, electron beam lithography, electric current ablation technology, disconnected knot technology, electrochemical deposition technique, nano wire mould plate technique, or the preparation of method such as focused ion beam ablation technology has the electrode pair in big gap, and its electrode gap is 5 to 1000 nanometers.
Second step was placed on electrode in the steam of e-beam induced deposition raw molecule of electrode, or the method by evaporation, made the raw molecule of electrode surface absorption one deck e-beam induced deposition.
The 3rd step was positioned over electrode in the scanning electron microscopy, and (energy is 0.1 to 1000 kiloelectron-volt, and density is 10 with electron beam
5To 10
10Every square metre of ampere) focus on the electrode gap zone, the electron beam-induced raw molecule decomposes, and at the coating layer of electrode surface deposition one deck conduction, thereby makes electrode gap narrow down gradually.
The 4th step, situation about reducing by scanning electron microscopy home position observation electrode gap.When electrode gap reaches required width, stop the electron beam irradiation immediately.Thereby nano-gap electrode prepares successfully.Its electrode gap is 2～100 nanometers.
Embodiment 1
The example that is prepared as with the CNT (carbon nano-tube) electrode
The first step is dispersed in carbon nano-tube in the ethanolic solution.Be on 2 microns the titanium electrode, then with drips of solution by the distribution situation of sem observation carbon nano-tube on the titanium electrode in spacing.(Fig. 1)
Second step added a bigger voltage at the titanium electrode two ends that are connected with carbon nano-tube, and carbon nano-tube is blown, and (Fig. 2 a) thereby form nano level gap in the centre.
The 3rd step placed the steam of toluene molecule with carbon nanotube electrode, placed 1 day, made the surface of toluene Molecular Adsorption at carbon nanotube electrode.
The 4th step was positioned over carbon nanotube electrode in the scanning electron microscopy, and (energy is 15 kiloelectron-volts, and density is 10 with electron beam
7Every square metre of ampere) focus on the carbon nanotube electrode gap area, electron beam-induced toluene molecular breakdown at the carbon coating layer of carbon nano tube surface depositing electrically conductive, thereby makes electrode gap narrow down gradually.Its process such as Fig. 2 a to Fig. 2 d.
The 5th step, situation about reducing by scanning electron microscopy home position observation electrode gap.When electrode gap reaches 2 nanometers, stop the electron beam irradiation immediately.Thereby nano-gap electrode prepares successfully.The nano-electrode two ends are connected circuit, and its current-voltage curve is as Fig. 3 (shown in the curved portion), and electrode is conducting not, illustrates that electrode does not have short circuit.When behind assembled dna molecule on the electrode, its current-voltage curve is as Fig. 3 (shown in the straight line portion), and electrode conduction illustrates that this electrode can be used to prepare molecular device.
Press the preparation method among the embodiment 1, difference is: the 3rd step, carbon nanotube electrode is placed the steam of ethanol, and placed 2 days.In the 4th step, electron beam density is 2 * 10
6Every square metre of ampere.In the 5th step, when electrode gap reaches 5 nanometers, stop the electron beam irradiation immediately.Having prepared electrode gap is the carbon nanotube electrode of 5 nanometers.As Fig. 4.
Embodiment 3
The first step has the gold electrode that the gap is 120 nanometers by the electron beam lithography preparation.
Second step is with the naphthalene molecule of gold electrode surfaces evaporation one deck 0.1 nanometer insulation.
The 3rd step was positioned over gold electrode in the scanning electron microscopy, and (energy is 30 kiloelectron-volts, and density is 10 with electron beam
8Every square metre of ampere) focus on the electrode gap zone, electron beam-induced naphthalene molecular breakdown at the coating layer of electrode surface deposition one deck conduction, thereby makes electrode gap narrow down gradually.
The 4th step, situation about reducing by scanning electron microscopy home position observation electrode gap.When electrode gap reaches 80 nanometers, stop the electron beam irradiation immediately.Thereby the gap is the nano-gap electrode of 80 nanometers to prepare successfully.
The foregoing description is that example is illustrated with carbon nanomaterial and gold electrode, and its effect is just with helping to understand technical scheme of the present invention, rather than is used to limit claim scope of the present invention.In fact, those skilled in the art can understand and realize the technical scheme that the present invention proposes.
Claims (7)
1. nano-gap electrode preparation method, its concrete steps are as follows:
A) preparation has the electrode pair in gap greatly on the nano material that not destroyed by electron beam;
B) at the raw molecule of the surface adsorption e-beam induced deposition of electrode pair, this raw molecule is toluene, naphthalene or ethanol;
C) electron beam is focused on the gap area of electrode pair;
D) when electrode gap reaches required width, stop the electron beam irradiation, prepare nano-gap electrode.
2. preparation method as claimed in claim 1, wherein, step a adopts photoetching technique, electron beam lithography, electric current ablation technology, disconnected knot technology, electrochemical deposition technique, nano wire mould plate technique or focused ion beam ablation technology to prepare electrode pair.
3. preparation method as claimed in claim 1, wherein, the nano material that not destroyed by electron beam is metal, inorganic semiconductor material or conductivity organic material.
4. as claim 1 or 3 described preparation methods, wherein, be not subjected in the nano material of electron beam destruction, metal is gold, silver, copper, iron, aluminium or germanium; Inorganic semiconductor material is a silicon; The conductivity organic material is poly-enedioxy thiophene or carbon nano-tube.
5. preparation method as claimed in claim 1, wherein, the electron beam energy of step c is 0.1 to 1000 kiloelectron-volt.
6. preparation method as claimed in claim 1, wherein, the electron beam density of step c is 10
5To 10
10Every square metre of ampere.
7. preparation method as claimed in claim 1, wherein, the electrode gap of steps d is 2 to 100 nanometers.
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| CN102180440A (en) * | 2011-04-06 | 2011-09-14 | 北京大学 | Preparation method of nano-gap electrode in micro-nano electromechanical device |
| CN102891083B (en) * | 2011-07-22 | 2016-10-19 | 中国人民解放军国防科学技术大学 | A kind of method preparing single electron transistor at room temperature |
| CN102914395B (en) * | 2012-11-06 | 2015-04-08 | 苏州新锐博纳米科技有限公司 | Nano stress sensor based on metal nano gap and preparation method thereof |
| CN105474398B (en) * | 2013-09-06 | 2018-11-13 | 国立研究开发法人科学技术振兴机构 | Electrode to, its production method, device substrate and device |
| CN107910371B (en) * | 2017-09-21 | 2021-02-12 | 中国电子科技集团公司第五十五研究所 | Method for improving direct-write charge accumulation of electron beam on surface of GaN HEMT |
| CN109909493A (en) * | 2019-02-25 | 2019-06-21 | 华中科技大学 | A kind of method that electron beam irradiation improves metal material stability |
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| US6864481B2 (en) * | 2001-12-04 | 2005-03-08 | Sii Nanotechnology Inc. | Probe for scanning probe microscope |
| US7082683B2 (en) * | 2003-04-24 | 2006-08-01 | Korea Institute Of Machinery & Materials | Method for attaching rod-shaped nano structure to probe holder |
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| US6864481B2 (en) * | 2001-12-04 | 2005-03-08 | Sii Nanotechnology Inc. | Probe for scanning probe microscope |
| US7082683B2 (en) * | 2003-04-24 | 2006-08-01 | Korea Institute Of Machinery & Materials | Method for attaching rod-shaped nano structure to probe holder |
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