CN101628708A - Carbon nano-tube oriented alignment technology combining functional modification and bidirectional electrophoresis - Google Patents
Carbon nano-tube oriented alignment technology combining functional modification and bidirectional electrophoresis Download PDFInfo
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- CN101628708A CN101628708A CN200910194648A CN200910194648A CN101628708A CN 101628708 A CN101628708 A CN 101628708A CN 200910194648 A CN200910194648 A CN 200910194648A CN 200910194648 A CN200910194648 A CN 200910194648A CN 101628708 A CN101628708 A CN 101628708A
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Abstract
The invention relates to a carbon nano-tube oriented alignment technology combining functional modification and bidirectional electrophoresis in the manometer processing field. The carbon nano-tube oriented alignment technology comprises the following steps: the preparation of carbon nano-tube suspension liquid: firstly, carrying out the surface activating treatment of carbon nano-tubes; then, adopting ultrasonic dispersion treatment to disperse the carbon nano-tubes into organic solvent to prepare the carbon nano-tube suspension liquid; the preparation of a nanometer electronic device electrode pair: adopting a photoetching technology to process and manufacture the electrode pair on a surface insulation layer of a silicon chip; then, dipping the carbon nano-tube suspension liquid on the surfaces of the electrode pair so that a plurality of carbon nano-tubes are arranged between the electrode pair of a nanometer device; the preparation of a high-density carbon nano-tube film: adopting a high-frequency alternating field bidirectional electrophoresis method for alignment treatment between the electrode pair so that the carbon nano-tubes are mutually separated in parallel between the electrode pair; and then, using ultraviolet rays to radiate the surface of the silicon chip to finish oriented alignment treatment. The adjacent carbon nano-tubes treated by the method can achieve an average spacing of 200nm without entanglement.
Description
Technical field
What the present invention relates to is the technology in a kind of nanoprocessing field, specifically is the carbon nano-tube oriented alignment technology that a kind of functional modification and dielectrophoresis combine.
Background technology
At present, people just drop into a large amount of energy in the research of 1-dimention nano device, have obtained some important progress.But, it is essential the arrange surface of device of monodimension nanometer material in the face of the large-scale 1-dimention nano device of making.At present, employed alignment technology mainly contains following several in the nanometer electronic device preparation that monodimension nanometer material is constructed: 1.LB embrane method: the Lieber C.M. of Harvard University (Whang D.M., Jin s., WuY., Lieber C.M., Nano Lett., 2003,3 (9): 1255-1259) seminar's success is by the LB film method, use activating agent that it is spread over the surface of liquid on the surface of silicon nanowires, push sliding barrier, compressive surfaces rete zone is closely arranged the nano wire rule.Between this method gained nano wire spacing at 200nm to 2 μ m, though further the compressive surfaces rete can obtain littler spacing, but the following spacing of 200nm causes nano wire reunion each other easily, and for scale arrangement nano material, may need up to a hundred repetitive displacement operations, increase the technology cost, and caused inefficiency, greatly limited its industrialization promotion.2. flow method: the Dai H.J. of Stanford University (Wang D.W., Tu R., Zhang L., Dai H.J.Chem.Int.Ed., 2005,44,2-5) seminar for the monodimension nanometer material that obtains to align, works out a kind of man-to-man current oriented alignment method.On backing material,, obtain a series of metallic catalyst dot matrix by beamwriter lithography and lift-off technology.On this substrate, use the CVD method then, grow nanowire, each catalyst dot matrix correspondence grows a nano wire.Because an end of nano wire is used as the metallic particles of catalyst and is fixed on the substrate, at this time, as long as substrate is placed in the current, nano wire will be arranged along water (flow) direction under the souring of current.This method will make ultimate cost higher by means of advanced technologies such as beamwriter lithographies, and direct oriented growth monodimension nanometer material technology in substrate, because introduce impurity easily, has also limited it to a certain extent and has used and promote.3. spin-coating method: form mixed liquor in the direct ultrasonic dispersion organic solvent of CNT of IBM Corporation after with purifying, the CNT mixed liquor is spun on the silicon chip that is carved with the source-drain electrode pattern in advance, this method makes CNT distribute uncontrollable its orientation arbitrarily on silicon chip.The nano-device of making can't be obtained good performance.
Find by prior art documents, Chinese patent literature CN1693191A, put down in writing a kind of " process for preparing monocrystalline silicon nano line array of single axial arranging ", this technology adopts the auxiliary etch of catalysis at silicon chip surface deposition one deck Ag nano particle, uses the method for etching to produce silicon nanowires.Its weak point is: the diversified in specifications of the nano wire that this method makes causes, and the surface imperfection of the nano wire of formation is not suitable for making well behaved nano-device.
Summary of the invention
The present invention is directed to the prior art above shortcomings, the carbon nano-tube oriented alignment technology that provides a kind of functional modification and dielectrophoresis to combine, the alternating electric field dielectrophoresis that carries out after the pre-modification is arranged and avoided in the past shortcoming entangled to each other between the CNT of directional technology assembling back, effectively improved the effect of arranging, made CNT be separated from each other, directionally be arranged in and form highdensity carbon nano pipe array between the source-drain electrode of nano-device.After utilizing this technology that two kinds of carbon nano-tube solution that are dissolved in chloroform and isopropyl alcohol are arranged, the average headway of adjacent carbons nanotube can reach 200nm and 150nm respectively and not tangle.
The present invention is achieved by the following technical solutions, the present invention uses the CNT of modifying in advance through octadecylamine, use ultrasonic technique that the CNT of this pre-modification is distributed to and be prepared into carbon nano tube suspension in the organic solvent, this hanging drop is applied the high-frequency ac electric field to the electrode of nano-device will obtain highdensity carbon nano pipe array.
The present invention includes following steps:
The first step, preparation of carbon nano-tube suspension liquid: at first CNT is carried out surface activation process, adopt ultrasonic dispersion treatment that CNT is distributed to then and make carbon nano tube suspension in the organic solvent.
Described CNT is meant semiconductive carbon nano tube or metallic carbon nanotubes.
Described surface activation process is meant and places mix acid liquor to reflux 30 minutes under 50-140 ℃ of environment CNT, produces the carboxyl with activity in carbon nano tube surface, makes things convenient for carbon nano tube surface grafting octadecylamine.
Described mix acid liquor is meant: mass percent is that 98% aqueous sulfuric acid mixes the mix acid liquor that obtains with the aqueous solution of nitric acid of mass percent 68% with 3: 1 volume ratio.
Described function of surface molecular chemistry is modified and is meant, with the CNT after the surface activation process and octadecylamine, N, N '-dicyclohexylcarbodiimide is 1: 100: 30 the ratio environment that mixes to be placed on 60 ℃-110 ℃ reaction 24h down with mass ratio, make octadecylamine in the carbon nano tube surface grafting, like this on the CNT band certain net charge can be in electric field electrophoresis, clean CNT then to remove unnecessary octadecylamine.
Described ultrasonic dispersion treatment is meant CNT placed organic solvent, and is to disperse 10s-2min under the ultrasonic wave of 10-60KHz in frequency, forms the carbon nano tube suspension of stable dispersion.
Described organic solvent is meant chloroform or isopropyl alcohol.
The preparation of second step, nano electron device electrode pair: adopt photoetching technique processing and fabricating on the insulating barrier of silicon chip surface to go out electrode pair, then carbon nano tube suspension is dropped in the electrode pair surface, many CNTs are placed between the electrode of nano-device.
Described photoetching technique is meant and adopts Au, Ag, Mg, Fe, Al, Ti, Ni, W or Cu to make electrode pair on insulating barrier.
Described insulating barrier is meant a kind of in silica, aluminium oxide, silicon nitride, calcirm-fluoride, epoxy resin or the polyimides.
Described electrode pair is two parallel poles to structure, finger-like symmetry electrode to structure, interdigital electrode to a kind of in the structure of structure or annular comparative electrode, wherein: the spacing of two electrodes is 5nm-50 μ m in the described electrode pair, and the partly overlapping relatively width of two electrodes is 50nm-3mm in this electrode pair.
The preparation of film of the 3rd step, high-density carbon nano-tube: adopt the processing of arranging of high frequency alternating electric field at electrode pair, it is separated from each other and is parallel to each other between the electrode pair, with ultraviolet ray silicon chip surface is carried out radiation treatment then, finish oriented alignment and handle.
The frequency of described high frequency alternating electric field is 1k-100MHz, and the P-to-P voltage of this high frequency alternating electric field is the alternating voltage of 1-50V/ μ m.
Described arrange to handle be meant: it is 5s-5min that sedimentation time is set, temperature be 0 ℃-60 ℃ to the manipulation of arranging of the CNT between the electrode pair.
Described radiation treatment is meant: employing power is 10-300W, and wavelength is that the ultraviolet ray of 175nm-365nm is shone the side that silicon chip surface has electrode pair, and irradiation time is 5 minutes.
Operation principle of the present invention is:
CNT is carried out surface activation process, and this chemical treatment can produce in carbon nano tube surface has active carboxyl, makes things convenient for carbon nano tube surface grafting octadecylamine.CNT is carried out the function of surface molecular chemistry to be modified, make its finishing octadecylamine organic molecule, this processing can separating carbon nano-tube, avoids it to tangle mutually, simultaneously even carbon nanotube is scattered in organic solvent or the water, thereby forms the suspension of stable existence.The silicon chip surface that is being shaped on electrode when hanging drop in advance formed in the short time of liquid level, CNT is in free movable state, applying the high frequency alternating electric field can make the CNT bidirectional-movement form the structure that is arranged in parallel, the phase mutual interference that the conducting channel that form to separate can reduce electronics when transmit in CNT, the electrology characteristic of raising field-effect transistor.Use ultraviolet ray that CNT is carried out radiation treatment, the alkyl chain of carbon nano tube surface is decomposed, make to form good Ohmic contact between CNT and metal electrode.
The invention has the beneficial effects as follows: the CNT near vertical forms separated parallel highdensity array structure in electrode surface, has avoided tangling mutually between the CNT, and can form good Ohmic contact between metal electrode; The carbon nanotube device of preparation has good performance, and has better structural stability.Whole process need not high-temperature process.
The specific embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
At first CNT is carried out surface activation process, with CNT in the nitration mixture that 3: 1 proportionings of aqueous sulfuric acid (mass percent concentration is 98%) and aqueous solution of nitric acid (mass percent concentration is 68%) are made 100 ℃ refluxed 30 minutes down.Produce carboxyl in carbon nano tube surface, make things convenient for carbon nano tube surface grafting octadecylamine with activity.With the CNT after the surface activation process and octadecylamine, N, N '-dicyclohexylcarbodiimide reacts with the ratio of 1: 100: 30 (mass ratio), 60 ℃ of reactions 24 hours down, makes octadecylamine in the carbon nano tube surface grafting; Use the filter membrane in 2 μ m apertures to carry out suction filtration during cleaning, do not participate in the octadecylamine that reacts towards clear CNT to remove repeatedly with chloroform and alcohol simultaneously, dry then.Dried CNT is placed isopropyl alcohol, and be to disperse 1 minute under the ultrasonic wave of 20KHz in frequency, form the carbon nano tube suspension of stable dispersion.
Adopt photoetching technique to produce the Au electrode pair pattern of two parallel poles to structure on the silicon chip that contains 500nm thick silicon dioxide insulating barrier, the spacing of two electrodes is 1 μ m in this electrode pair, and the partly overlapping relatively width of two electrodes is 10 μ m in this electrode pair.Between source-drain electrode, adding a frequency is 10MHz, and the P-to-P voltage value is the high frequency sinusoidal voltage of 5V.With concentration is that the carbon nano tube suspension of 0.5g/mL drops on the source-drain electrode, makes its orientated deposition under the effect of alternating electric field, and sedimentation time is 40s, and depositing temperature is 25 ℃.Many parallel CNTs are parallel between two electrodes, certain spacing is arranged each other.Use power 10W, the ultraviolet ray of wavelength 175nm was carried out radiation treatment 5 minutes to the nano-device that makes, and the alkyl chain of carbon nano tube surface is decomposed, and also can form good Ohmic contact between CNT and metal electrode simultaneously, finished oriented alignment and handled.The average headway of adjacent carbons nanotube can reach 150nm respectively and not tangle after present embodiment is handled, and obtains having the nano-device of superperformance.
Embodiment 2
At first CNT is carried out surface activation process, with CNT in the nitration mixture that 3: 1 proportionings of aqueous sulfuric acid (mass percent concentration is 98%) and aqueous solution of nitric acid (mass percent concentration is 68%) are made 100 ℃ refluxed 30 minutes down.Produce carboxyl in carbon nano tube surface, make things convenient for carbon nano tube surface grafting octadecylamine with activity.With the CNT after the surface activation process and octadecylamine, N, N '-dicyclohexylcarbodiimide reacts with the ratio of 1: 100: 30 (mass ratio), 60 ℃ of reactions 24 hours down, makes octadecylamine in the carbon nano tube surface grafting; Use the filter membrane in 2 μ m apertures to carry out suction filtration during cleaning, do not participate in the octadecylamine that reacts towards clear CNT to remove repeatedly with chloroform and alcohol simultaneously, dry then.Dried CNT is placed chloroform, and be to disperse 2 minutes under the ultrasonic wave of 30KHz in frequency, form the carbon nano tube suspension of stable dispersion.
On the silicon chip that contains 500nm thick silicon dioxide insulating barrier, adopt photoetching technique to produce the Au electrode pair pattern of finger-like symmetry electrode to structure, the spacing of two electrodes is 1 μ m in this electrode pair, and the partly overlapping relatively width of two electrodes is 10 μ m in this electrode pair.Between source-drain electrode, adding a frequency is 5MHz, and P-to-P voltage is the high frequency sinusoidal voltage of 5V.With concentration is that the carbon nano tube suspension of 0.5g/mL drops on the source-drain electrode, makes its orientated deposition under the effect of alternating electric field, and sedimentation time is 40s, and depositing temperature is 25 ℃.Many parallel CNTs are parallel between two electrodes, certain spacing is arranged each other.Use power 10W, the ultraviolet ray of wavelength 175nm was carried out radiation treatment 5 minutes to the nano-device that makes, and the alkyl chain of carbon nano tube surface is decomposed, and also can form good Ohmic contact between CNT and metal electrode simultaneously, finished oriented alignment and handled.The average headway of adjacent carbons nanotube can reach 200nm respectively and not tangle after present embodiment is handled, and obtains having the nano-device of superperformance.
Embodiment 3
At first CNT is carried out surface activation process, with CNT in the nitration mixture that 3: 1 proportionings of aqueous sulfuric acid (mass percent concentration is 98%) and aqueous solution of nitric acid (mass percent concentration is 68%) are made 100 ℃ refluxed 30 minutes down.Produce carboxyl in carbon nano tube surface, make things convenient for carbon nano tube surface grafting octadecylamine with activity.With the CNT after the surface activation process and octadecylamine, N, N '-dicyclohexylcarbodiimide reacts with the ratio of 1: 100: 30 (mass ratio), 60 ℃ of reactions 24 hours down, makes octadecylamine in the carbon nano tube surface grafting; Use the filter membrane in 2 μ m apertures to carry out suction filtration during cleaning, do not participate in the octadecylamine that reacts towards clear CNT to remove repeatedly with chloroform and alcohol simultaneously, dry then.Dried CNT is placed chloroform, and be to disperse 2 minutes under the ultrasonic wave of 30KHz in frequency, form the carbon nano tube suspension of stable dispersion.
Adopt photoetching technique to produce the Au electrode pair pattern of interdigital electrode to structure on the silicon chip that contains 500nm thick silicon dioxide insulating barrier, the spacing of two electrodes is 1 μ m in this electrode pair, and the partly overlapping relatively width of two electrodes is 10 μ m in this electrode pair.Between source-drain electrode, adding a frequency is 5MHz, and P-to-P voltage is a 10V high frequency sinusoidal voltage.With concentration is that the carbon nano tube suspension of 0.5g/mL drops on the source-drain electrode, makes its orientated deposition under the effect of alternating electric field, and sedimentation time is 40s, and depositing temperature is 25 ℃.Many parallel CNTs are parallel between two electrodes, certain spacing is arranged each other.Use power 10W, the ultraviolet ray of wavelength 175nm was carried out radiation treatment 5 minutes to the nano-device that makes, and the alkyl chain of carbon nano tube surface is decomposed, and also can form good Ohmic contact between CNT and metal electrode simultaneously, finished oriented alignment and handled.The average headway of adjacent carbons nanotube can reach 120nm respectively and not tangle after present embodiment is handled, and obtains having the nano-device of superperformance.
Claims (10)
1, the carbon nano-tube oriented alignment technology that combines of a kind of functional modification and dielectrophoresis is characterized in that, may further comprise the steps:
The first step, preparation of carbon nano-tube suspension liquid: at first CNT is carried out surface activation process, adopt ultrasonic dispersion treatment that CNT is distributed to then and make carbon nano tube suspension in the organic solvent;
The preparation of second step, nano electron device electrode pair: adopt photoetching technique processing and fabricating on the insulating barrier of silicon chip surface to go out electrode pair, then carbon nano tube suspension is dropped in the electrode pair surface, many CNTs are placed between the electrode of nano-device;
The preparation of film of the 3rd step, high-density carbon nano-tube: adopt the processing of arranging of high frequency alternating electric field at electrode pair, it is separated from each other and is parallel to each other between the electrode pair, with ultraviolet ray silicon chip surface is carried out radiation treatment then, finish oriented alignment and handle.
2, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis is characterized in that described surface activation process is meant and places mix acid liquor to reflux 30 minutes CNT under 50-140 ℃ of environment.
3, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 2 and dielectrophoresis, it is characterized in that described mix acid liquor is meant: mass percent is that 98% aqueous sulfuric acid mixes the mix acid liquor that obtains with the aqueous solution of nitric acid of mass percent 68% with 3: 1 volume ratio.
4, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, described function of surface molecular chemistry is modified and is meant, with the CNT after the surface activation process and octadecylamine, N, N '-dicyclohexylcarbodiimide is 1: 100: 30 the ratio environment that mixes to be placed on 60 ℃-110 ℃ reaction 24h down with mass ratio.
5, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, described ultrasonic dispersion treatment is meant CNT placed organic solvent, and is to disperse 10s-2min under the ultrasonic wave of 10-60KHz in frequency.
6, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis is characterized in that, described insulating barrier is meant a kind of in silica, aluminium oxide, silicon nitride, calcirm-fluoride, epoxy resin or the polyimides.
7, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, described electrode pair is two parallel poles to structure, finger-like symmetry electrode to structure, interdigital electrode to a kind of in the structure of structure or annular comparative electrode, wherein: the spacing of two electrodes is 5nm-50 μ m in the described electrode pair, and the partly overlapping relatively width of two electrodes is 50nm-3mm in this electrode pair.
8, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, the frequency of described high frequency alternating electric field is 1k-100MHz, and the P-to-P voltage of this high frequency alternating electric field is the alternating voltage of 1-50V/ μ m.
9, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, described arrange to handle be meant: it is 5s-5min that sedimentation time is set, temperature be 0 ℃-60 ℃ to the manipulation of arranging of the CNT between the electrode pair.
10, the carbon nano-tube oriented alignment technology that combines of functional modification according to claim 1 and dielectrophoresis, it is characterized in that, described radiation treatment is meant: employing power is 10-300W, wavelength is that the ultraviolet ray of 175nm-365nm is shone the side that silicon chip surface has electrode pair, and irradiation time is 5 minutes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071468A (en) * | 2011-02-24 | 2011-05-25 | 南京师范大学 | Independent polymer nanotube, and preparation method and application thereof |
| CN103193194B (en) * | 2013-03-05 | 2015-10-21 | 西安交通大学 | Based on the ordered nano method for manufacturing microstructure of Nano silver grain dielectrophoresis assembling |
| CN107402244A (en) * | 2017-06-30 | 2017-11-28 | 江苏大学 | A kind of bimodal interaction sensor array chip manufacturing and information acquisition method |
| CN109725177A (en) * | 2019-03-05 | 2019-05-07 | 西安交通大学 | A kind of measurement method of monodimension nanometer material interface bonding energy |
-
2009
- 2009-08-27 CN CN200910194648A patent/CN101628708A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071468A (en) * | 2011-02-24 | 2011-05-25 | 南京师范大学 | Independent polymer nanotube, and preparation method and application thereof |
| CN102071468B (en) * | 2011-02-24 | 2012-10-24 | 南京师范大学 | Independent polymer nanotube, and preparation method and application thereof |
| CN103193194B (en) * | 2013-03-05 | 2015-10-21 | 西安交通大学 | Based on the ordered nano method for manufacturing microstructure of Nano silver grain dielectrophoresis assembling |
| CN107402244A (en) * | 2017-06-30 | 2017-11-28 | 江苏大学 | A kind of bimodal interaction sensor array chip manufacturing and information acquisition method |
| CN109725177A (en) * | 2019-03-05 | 2019-05-07 | 西安交通大学 | A kind of measurement method of monodimension nanometer material interface bonding energy |
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