CN103077888B - Method for preparing electrode on single nano wire - Google Patents
Method for preparing electrode on single nano wire Download PDFInfo
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- CN103077888B CN103077888B CN201310011661.XA CN201310011661A CN103077888B CN 103077888 B CN103077888 B CN 103077888B CN 201310011661 A CN201310011661 A CN 201310011661A CN 103077888 B CN103077888 B CN 103077888B
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Abstract
The invention discloses a method for preparing an electrode on a single nano wire. The method is used for preparing the electrode at a specific position on the nano wire so as to realize electrical contact and is implemented mainly by virtue of micro-nano manufacturing processes such as nano wire transfer, nano wire dispersion, electron beam photoengraving and nesting, and nano film deposition. The method is mainly characterized in that an Al film is used as a conductive layer for electron beam photoengraving, a protective layer of the nano wire, and a undercut layer for a stripping process; and by utilizing the method, the alignment precision of the electrode and the nano wire and the success rate of preparation can be obviously improved. The method can be used for preparing nano wire solar batteries, photoelectric detectors, light-emitting diodes, lasers, sensors and the like.
Description
Technical field
The present invention relates to the research frontier such as synthesis and preparative of nano optoelectronics, micro-nano sensing technology, microelectronics and micro-nano technology and monodimension nanometer material, being specifically related to a kind of method for preparing electrode on single nano wire.
Background technology
Nano wire is radial dimension is nanoscale, and the hard-core one-dimensional nano structure of length direction.As a kind of important nano material, although from being found to now only less than the vicennial time, due to the property that it shows in biochemistry, mechanics, electromagnetism and photoelectron, and get the attention in each field.Calendar year 2001, " Nature " magazine ran California, USA Berkeley University Yang Pei east group develops minimum in the world, based on the room temperature ultraviolet laser of ZnO nano-wire, shows good laser activity.The nano generator that professor Wang Zhonglin of " Science " magazine ran in 2006 georgia ,u.s.a Institute of Technology utilizes the piezoelectric effect of ZnO nano-wire to invent, some microvibrations of surrounding can be converted into electric energy, application that is microminiaturized for energy resource system and some passive nano devices provides desirable power-supply system.Within 2009, " Nature " impurity reports the nano wire processor of the Lieber professor group invention of the U.S., and this processor based on Ge/Si nano-wire fet, and achieves the function of adder, subtracter, multiplier, divider and the d type flip flop in integrated circuit.Nano-wire devices has the performance of so many excellence, but will realize nano wire electrical contact exists many difficult problems, and this not only constrains excavates the further research of its performance, also counteracts that development and the application of nano-wire devices.The current main method realizing nano wire electrical contact is the solder technology utilizing focused ion beam (FIB), based on the nanoimprinting technology of electron beam exposure, and uses AC dielectric to swim the technology arranged nano wire.Nanoimprinting technology based on electron beam exposure obtains to be paid close attention to widely; but nano wire is often randomly dispersed within substrate by this technique; there is no any fixation; so in follow-up technique; nano wire often can move or depart from for various reasons, and this makes the success rate using the method to prepare nano line electrode greatly reduce.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing electrode on single nano wire based on electron beam exposure technique.
For achieving the above object, present invention employs following technical scheme.
This method preparing electrode comprises the following steps: by nano wire dispersion on a dielectric base, then one deck nano level Al film cover layer as conductive layer and nano wire is covered on a dielectric base, then spin coating electron beam resist (PMMA on Al film, molecular weight 950k), photoetching development is carried out to the electron beam resist of spin coating in position according to nano wire in dielectric base, post bake obtains the photoetching agent pattern of electrode, then wet etching Al film forms undercutting window, then plated metal the metal be deposited on electron beam resist is peeled off, then erosion removal Al film.Al film is simultaneously as the conductive layer of electron beam lithography, and the protective layer of the undercutting layer of stripping technology and protection and fixing nano wire, what can significantly improve single nano line electrode is prepared into power.
Nano wire ultrasonic disperse is obtained suspension-turbid liquid in a solvent, suspension-turbid liquid is dropped in dielectric base, then the solvent in dielectric base is passed through baking evaporate to dryness, nano wire is disperseed on a dielectric base.Due to the effect of Van der Waals force, nano wire can be adsorbed onto in substrate, difficult drop-off.
Described Al film adopts sputtering sedimentation to obtain, and thickness is 150-500 nanometer.As the undercutting layer use of the conductive layer of electron beam exposure, the protective layer of fixing nano wire and follow-up stripping technology.
Described post bake carries out on hot plate, and hot plate temperature is 100-110 DEG C, and the post bake time is 10-25 minute.Remove solvent residual in photoresist, increase the binding ability of glue-line and Al layer, in subsequent etching, play good shielding action, avoid uncontrollable undercutting to occur.
The tetramethylammonium hydroxide aqueous solution that the etching liquid that described wet etching Al film uses is 0.05-0.3mol/L, etch period is 60-300 second, and etching temperature is 17-25 DEG C.Utilize the isotropic etching feature of Al film, etch Al film undercut construction under PMMA photoetching agent pattern window, undercut construction can assure success the plated metal peeled off on electron beam resist.Etch period is determined according to etching liquid concentration and etching temperature, etching liquid concentration and etching temperature higher, etching speed is higher, but the more difficult control of etched shape.
The thickness of described plated metal is no more than 180 nanometers.As the electrode material of resulting devices.
The described method preparing electrode specifically comprises the following steps:
1) CdS nano wire ultrasonic disperse is obtained in a solvent the suspension-turbid liquid of nano wire;
2) be heated to 90 DEG C after dielectric base being cleaned up, then drip several suspension-turbid liquids on a dielectric base, after solvent evaporation removing, CdS nano wire is dispersed in substrate;
3) the Al film that sputtering sedimentation 200nm is thick in the dielectric base being dispersed with CdS nano wire;
4) electron beam resist (PMMA, polymethyl methacrylate) that spin coating 500nm is thick on Al film;
5) after step 4), under electron beam exposure apparatus, the CdS nano wire covered under Al film is positioned, then carry out photoetching development, post bake;
6) after step 5), use Tetramethylammonium hydroxide (TMAH) aqueous solution of 0.1mol/L to etch Al film 150 seconds, etching temperature is 23 DEG C, then repeatedly rinses with deionized water, use nitrogen to dry up after rinsing, toast 10 minutes in 100 DEG C on hot plate after drying up;
7) after step 6), the Pd of sputtering sedimentation thickness to be the Ti of 25nm and thickness be 150nm obtains electrode metal film successively, then the electrode metal film be deposited on electron beam resist is peeled off in acetone, leave required electrode pattern, then use described Tetramethylammonium hydroxide (TMAH) aqueous solution to etch and remove remaining Al film in dielectric base, obtain being prepared in the electrode on CdS nano wire;
8) after step 7), rush electrode with deionized water, dry up with nitrogen after flushing, then add heat abstraction moisture.
Beneficial effect of the present invention is embodied in:
The present invention is used on the ad-hoc location of one-dimensional nano structure, prepare electrode and carries out electrical contact, and mainly through transfer, the dispersion of nano wire, the micro-nano manufacturing process such as electron beam lithography alignment and Nanometer thin film deposition realizes; Main feature of the present invention uses Al film as the undercutting layer of the conductive layer of electron beam lithography, the protective layer of nano wire and stripping technology, uses the method for the invention can significantly improve the alignment precision of electrode and nano wire and be prepared into power; The method of the invention can be used for preparing single nanowire solar cells, photodetector, light-emitting diode, laser and sensor.
Accompanying drawing explanation
Fig. 1 is that the present invention uses Al as the schematic diagram of stripping technology undercutting layer;
Fig. 2 is bipolar electrode structure light microscopic figure prepared by the present invention;
Fig. 3 is flow chart of the present invention;
Fig. 4 is the structural representation of electrode prepared by the present invention;
Fig. 5 is the volt-ampere characteristics of figure of electrode prepared by the present invention;
In figure: 1 is metal deposition layer, 2 is PMMA electron beam resist, and 3 is Al film, and 4 is dielectric base, and 5 is undercutting window, and 6 is nano wire, and 7 is electrode.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
See Fig. 1-Fig. 4, specifically comprise the following steps:
1) by CdS nano wire ultrasonic disperse in isopropyl alcohol (IPA), ultrasonic power 60W, time are 2 minutes, form the suspension-turbid liquid of nano wire.Nano wire dispersion solvent for use is not limited to IPA, and only otherwise react with nano wire, and the solvent that can form stabilized nanoscale line suspension-turbid liquid all can.The nano wire mentioned in the present invention is not limited to certain material, as long as the nano wire that can be used for this technique all can.
2) dielectric base is cleaned: dielectric base adopts the glass substrate being coated with 300nm thick silicon nitride film, by dielectric base according to each ultrasonic cleaning of the order of acetone, ethanol, deionized water 10 minutes, uses N after cleaning
2dry up, and toast 20 minutes on 80 DEG C of hot plates, remove surperficial steam.
3) 90 DEG C are heated to after dielectric base being cleaned up, then the suspension-turbid liquid prepared is dripped upper several on a dielectric base, dripping several concentration according to configured suspension-turbid liquid (500/ml) in specific implementation process and testing needs and determines, and the present invention uses 0.2ml/cm
2, after IPA evaporation is clean, hot plate temperature is promoted to 100 DEG C, and toasts 30min, remove remaining IPA, CdS nano wire is disperseed on a dielectric base.Described dielectric base is not limited to the substrate of glass being coated with silicon nitride, as long as can requirement on devices be met, and the substrate that can be used for this technique all can, as being coated with the silicon chip etc. of certain thickness silicon nitride or silicon dioxide.
4) Al and even glue is sputtered: the metal A l film that magnetically controlled DC sputtering 200nm is thick in the dielectric base being dispersed with CdS nano wire, then the PMMA electron beam resist of thick, the 950k molecular weight of spin coating 500nm on Al film.In actual mechanical process, Al film thickness is determined according to the needs of thickness of electrode, and Al film should thicker than electrode film thickness about at least 1/4.And the thickness of PMMA electron beam resist should not be less than 100nm, avoid, in nano wire position fixing process, being exposed.
5) electron beam lithography: first search out the nano wire needing to prepare electrode under SEM pattern, then SEM is adjusted to as far as possible high multiplication factor, and position, then expose, exposure dose is 120 μ C/cm
2.Use MIBK(methylisobutylketone): IPA=1:3(volume ratio) developing liquid developing 1-2min, IPA fixing 30s, N
2dry up.Then dry 20 minutes on 110 DEG C of hot plates or in 110 DEG C of thermostatic drying chambers.Electron beam exposure parameter in this step and follow-up development post-drying parameter are determined according to the equipment of reality and photoresist.
6) Al is corroded: because most nano wire can react with acid etching liquid, therefore the present invention adopts Tetramethylammonium hydroxide (TMAH) aqueous solution of 0.1mol/L to carry out wet etching Al, etching temperature 23 DEG C, the etching Al film time is 150 seconds, then repeatedly rinse with deionized water, use nitrogen to dry up after rinsing, toast 10 minutes in 100 DEG C on hot plate after drying up; Because etching is in isotropism, so undercutting to a certain degree can be formed, " convex " shape photoetching window can be formed like this, significantly simplify follow-up metal lift-off material.Employing etching liquid concentration is the TMAH aqueous solution of 0.1mol/L, just in order to avoid etching liquid and nano wire react.Only require that etching liquid does not react with nano wire during actual etching, can Al be etched simultaneously, and good undercutting undercut construction can be formed.
7) sputtering electrode, stripping and removal Al: successively sputter 25nm Ti and 150nm Pd, peel off in acetone afterwards, obtain required electrode pattern.Then use the etching liquid of previous step to be got rid of by Al remaining in dielectric base, just obtain final required nano line electrode pattern.The kind of sputter material should be determined as required, but this sputtering electrode material require by final etching remove Al etching liquid destroy.
8) after step 7), rush electrode pattern with deionized water, dry up with nitrogen after flushing, then add heat abstraction moisture.
Fig. 5 gives the I-V performance plot of device prepared by above-mentioned steps, uses Keithley 4200SCS characteristic of semiconductor analyzer to measure, and when being added in that on two electrodes, bias voltage reaches 6V, reach 100nA by the electric current of device, device conducts is good.
Claims (7)
1. one kind for preparing the method for electrode on single nano wire, it is characterized in that: this method preparing electrode comprises the following steps: by nano wire dispersion on a dielectric base, then one deck nano level Al film cover layer as conductive layer and nano wire is covered on a dielectric base, then spin coating electron beam resist on Al film, photoetching development is carried out to the electron beam resist of spin coating in position according to nano wire in dielectric base, post bake obtains the photoetching agent pattern of electrode, then wet etching Al film forms undercutting window, then plated metal the metal be deposited on electron beam resist is peeled off, leave required electrode pattern, then erosion removal Al film, obtain the electrode be prepared on nano wire.
2. a kind of method for preparing electrode on single nano wire according to claim 1, it is characterized in that: nano wire ultrasonic disperse is obtained suspension-turbid liquid in a solvent, suspension-turbid liquid is dropped in dielectric base, then the solvent in dielectric base is passed through baking evaporate to dryness, nano wire is disperseed on a dielectric base.
3. a kind of method for preparing electrode on single nano wire according to claim 1, is characterized in that: described Al film adopts sputtering sedimentation to obtain, and thickness is 150-500 nanometer.
4. a kind of method for preparing electrode on single nano wire according to claim 1, it is characterized in that: described post bake carries out on hot plate, hot plate temperature is 100-110 DEG C, and the post bake time is 10-25 minute.
5. a kind of method for preparing electrode on single nano wire according to claim 1, it is characterized in that: the tetramethylammonium hydroxide aqueous solution that the etching liquid that described wet etching Al film uses is 0.05-0.3mol/L, etch period is 60-300 second, and etching temperature is 17-25 DEG C.
6. a kind of method for preparing electrode on single nano wire according to claim 1, is characterized in that: the thickness of described plated metal is no more than 180 nanometers.
7. a kind of method for preparing electrode on single nano wire according to claim 1, is characterized in that: the described method preparing electrode specifically comprises the following steps:
1) CdS nano wire ultrasonic disperse is obtained in a solvent the suspension-turbid liquid of nano wire;
2) be heated to 90 DEG C after dielectric base being cleaned up, then drip several suspension-turbid liquids on a dielectric base, after solvent evaporation removing, CdS nano wire is dispersed in substrate;
3) the Al film that sputtering sedimentation 200nm is thick in the dielectric base being dispersed with CdS nano wire;
4) electron beam resist that spin coating 500nm is thick on Al film;
5) through step 4) after, under electron beam exposure apparatus, the CdS nano wire covered under Al film is positioned, then carry out photoetching development, post bake;
6) through step 5) after, the tetramethylammonium hydroxide aqueous solution etching Al film of use 0.1mol/L 150 seconds, etching temperature is 23 DEG C, then uses deionized water rinsing, uses nitrogen to dry up, toast 10 minutes after drying up on hot plate in 100 DEG C after rinsing;
7) through step 6) after, the Pd of sputtering sedimentation thickness to be the Ti of 25nm and thickness be 150nm obtains electrode metal film successively, then the electrode metal film be deposited on electron beam resist is peeled off in acetone, then use described tetramethylammonium hydroxide aqueous solution to etch and remove remaining Al film in dielectric base, obtain being prepared in the electrode on CdS nano wire.
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| DE102015015452A1 (en) * | 2015-12-02 | 2017-06-08 | Forschungszentrum Jülich GmbH | Process for planarizing nanostructures |
| CN106299123B (en) * | 2016-10-11 | 2019-03-15 | 北京科技大学 | A method of being patterned with machine electrode PEDOT:PSS |
| CN111584707B (en) * | 2020-04-10 | 2023-02-03 | 中国科学院上海微系统与信息技术研究所 | Double-layer adhesive stripping method for nanowire structure of SNSPD (single-wire quantum device) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1979768A (en) * | 2005-12-08 | 2007-06-13 | 中国科学院微电子研究所 | Method for preparing metal nano electrode by adopting positive electronic resist |
| CN101552207A (en) * | 2008-04-02 | 2009-10-07 | 中国科学院微电子研究所 | Method for preparing ZnO top gate nanowire field effect transistor |
| CN101924202A (en) * | 2010-09-08 | 2010-12-22 | 武汉理工大学 | Single nanowire electrochemical device and assembly and in-situ characterization method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1979768A (en) * | 2005-12-08 | 2007-06-13 | 中国科学院微电子研究所 | Method for preparing metal nano electrode by adopting positive electronic resist |
| CN101552207A (en) * | 2008-04-02 | 2009-10-07 | 中国科学院微电子研究所 | Method for preparing ZnO top gate nanowire field effect transistor |
| CN101924202A (en) * | 2010-09-08 | 2010-12-22 | 武汉理工大学 | Single nanowire electrochemical device and assembly and in-situ characterization method thereof |
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