CN103943458A - Method for removing metal carbon nano tube in carbon nano tube array - Google Patents

Method for removing metal carbon nano tube in carbon nano tube array Download PDF

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Publication number
CN103943458A
CN103943458A CN201410119928.1A CN201410119928A CN103943458A CN 103943458 A CN103943458 A CN 103943458A CN 201410119928 A CN201410119928 A CN 201410119928A CN 103943458 A CN103943458 A CN 103943458A
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carbon nano
nano tube
carbon nanotubes
source
pipe array
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CN201410119928.1A
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仲东来
张志勇
彭练矛
王胜
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Peking University
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Peking University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02524—Group 14 semiconducting materials
    • H01L21/02527—Carbon, e.g. diamond-like carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02587—Structure
    • H01L21/0259—Microstructure
    • H01L21/02606—Nanotubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
    • H01L21/02664—Aftertreatments

Abstract

The invention provides a method for removing a metal carbon nano tube in a carbon nano tube array. When carbon nano tubes make contact with metal, a semi-conductor carbon nano tube will form a Schottky barrier, the metal carbon nano tube will not form a Schottky barrier, so that the resistance, formed in a contacting mode, of the semi-conductor carbon nano tube is higher, and the current of the semi-conductor carbon nano tube is lower than that of the metal carbon nano tube under the same voltage. Based on this, the metal carbon nano tube in the carbon nano tube array can be removed through a current firing method, a microwave-assisted burnout method, a thermal capillary gel method and the like. The method for removing the metal carbon nano tube in the carbon nano tube array is simple in preparing process, the ratio between the usable carbon nano tubes and the whole carbon nano tube is higher, the overall tube diameter of the obtained semi-conductor carbon nano tube is smaller, and electric performance is better. The metal carbon nano tube can be completely removed, the semi-conductor carbon nano tube with the purity of 100% can be obtained, the switch ratio is larger, and the obtained semi-conductor carbon nano tube is suitable for a high-speed digital circuit.

Description

A kind of method of removing metallic carbon nanotubes in carbon nano pipe array
Technical field
The present invention relates to a kind of method of removing metallic carbon nanotubes in carbon nano pipe array, is to utilize when metallic carbon nanotubes contacts with Titanium with semiconductor carbon nanometer tube, and Schottky barrier size has difference, causes electric current under same voltage to be distinguished to some extent.Based on this, can remove metallic carbon nanotubes, obtain all-semiconductor carbon nano pipe array.
Background technology
Can scale carbon nano-tube parallel array material in quartz substrate, meet the demand of follow-up scale fabricate devices and integrated circuit, the existing semiconductor carbon nanometer tube of carbon nano pipe array of self-sow, have again the metallic carbon nanotubes of zero band gap, and the latter's existence is unallowed absolutely to realizing carbon nano-tube digital integrated circuit.The method that may address this problem at present, has three kinds:
(1) in the carbon nano tube growth stage, use some special carbon sources, as isopropyl alcohol, or add special catalyst, as water, can realize certain selective growth, improve the ratio of semiconductor carbon nanometer tube, problem is that the ratio of semiconductor alloy need to reach at least 100:1, just likely meets the required on-off ratio of digital circuit, and this is difficult to accomplish;
(2) electric current calcination method, utilizes grid that semiconductor carbon pipe is turn-offed, and adds larger voltage, and power surpasses 90 μ W/ μ m, just metallic carbon nanotubes can be blown, and this can cause damage to the performance of semiconductor carbon nanometer tube, and metal tube does not remove completely simultaneously;
Within (3) 2013 years, J.A.Rogers delivers one piece of Using nanoscale thermocapillary flows to create arrays of purely semiconducting single-walled carbon nanotubes on Nature Nanotechnology, the inside is mentioned at the carbon nano-pipe array of having grown and is listed TPPA(Trishydroxyphenylethylisopropylbezene in steaming), by part grid, turn-off semiconductor carbon nanometer tube, and metal tube electric current is unaffected, making alive 1.33 μ W/ μ m, 60 ℃ of base reservoir temperatures, switch on 5 minutes, glue on metal tube can be by boiled, dry etching again, remove photoresist and just can obtain semiconductor carbon nanotube array, but grid preparation method is complicated, carbon nano-tube utilance is not high.
Summary of the invention
For problems of the prior art, the present invention aims to provide a kind of metallic carbon nanotubes of removing of simply, not damaging semiconductor carbon nanometer tube performance, and obtains the method for all-semiconductor carbon nano pipe array.
Technical scheme of the present invention is as follows:
A method of removing metallic carbon nanotubes in carbon nano pipe array, comprises the following steps:
1) in substrate, prepare carbon nano pipe array;
2) in the substrate of the carbon nano pipe array of having grown, make source-drain electrode, make the metal of source-drain electrode for can form with semiconductor carbon nanometer tube the metal of Schottky contacts;
3) use constant pressure source or seasonal power to source-drain electrode making alive, blow metallic carbon nanotubes;
4) remove source-drain electrode.
In the present invention, carbon nano pipe array is in the various substrates that have a crystal lattice orientation, as quartz, sapphire etc., and the carbon nano pipe array that the method by chemical vapor deposition (CVD) method or other extra electric fields prepares;
Source-drain electrode in the present invention can be the various metals of Schottky contacts that can form with semiconductive carbon nano tube such as Ti, Al, Cu, Cr, Ca, contact can both can adopt symmetrical contact also can adopt asymmetric contact, being that source-drain electrode metal used can be all in Ti, Al, Cu, Cr, Ca, can be also their combination of two.Channel length is from 2 μ m to 30 μ m;
Further, in step 3), use constant pressure source is to source-drain electrode institute making alive for more than 5V/ μ m, and energising is more than 5 minutes.
Further, in step 3), also comprise to source-drain electrode is alive and carbon nano pipe array is imposed to microwave simultaneously, the auxiliary metallic carbon nanotubes of blowing.
Further, in step 3), also comprise before energising evaporation one deck TPPA heat substrate in substrate, periodic power supply adds the voltage that rises to successively 14V/ μ m from 8V/ μ m, the TPPA in boiled metallic carbon nanotubes between source-drain electrode; After etching away the metallic carbon nanotubes of not protected by TPPA, remove TPPA cull.
Further, in step 4), use KI/I 2solution etc. dissolve source-drain electrode.
In the present invention, relate to microwave, microwave frequency be 2GHz to 3GHz, preferred 2.45GHz, is absorbed manyly by metallic carbon nanotubes, generate heat more.
In the present invention, relate to and need to heat substrate, heating-up temperature can to 100 ℃ from 60 ℃.
In the present invention, relate to etching, use the various dry etching equipments such as ICP or RIE, reacting gas is O 2/ CF 41:1 mixes, and etch period is that 25s is to 30s.
Further, use dry etching that metallic carbon nanotubes is etched away, with an organic solvent or high temperature method remove TPPA cull.
In the present invention, relate to the method for TPPA cull, can be in a vacuum or 600 ℃ of the lower high temperature of inert gas (as Ar gas) protection and more than, 5 hours and above evaporation, or by some organic solvent dissolutions.
Compared with prior art, good effect of the present invention is:
1, realize Schottky contacts, preparation technology is simple, only need a photoetching, a plated film, and the method that regulates and controls to turn-off semiconductor carbon nanometer tube by grid, at least need Twi-lithography, twice plated film and an ald, processing step still less can guarantee to reduce the damage to carbon nano-tube performance;
2, carbon nano-tube utilance is high, use the method for grid regulation and control, in quartz substrate, must use top grid, grid itself need to contact with a part for carbon nano-tube, and this part carbon nano-tube is to utilize, and use the method for Schottky contacts, only need to plate source-drain electrode just passable, so that available carbon nano-tube occupies whole carbon nano-tube ratio is higher;
3, the whole caliber of semiconductor carbon nanometer tube less (average 1.1nm) obtaining, because the semiconductor carbon nanometer tube for Large Diameter Pipeline, the Schottky barrier forming with metal is very little, therefore also can be removed in removal metal tube process, semiconductor carbon nanometer tube band gap for pipe with small pipe diameter is larger, on-off ratio higher (10^5);
4, metallic carbon nanotubes is removed completely, can obtain the semiconductor carbon nanometer tube of purity 100%;
5, the semiconductor carbon nanometer tube electric property obtaining is better, does not need carbon nano-tube modifiedly, can not introduce defect, and the carbon nano-tube obtaining is cleaner, so mobility is higher, (can reach 1000cm 2/ Vs), be applicable to doing high-speed digital circuit.
Accompanying drawing explanation
Fig. 1 (a) shows is the energy band diagram of metal while contacting with semiconductor carbon carbon nano tube.
Fig. 1 (b) shows is metal energy band diagram while contacting with metallic carbon nanotubes.
Fig. 2 shows while being metallic carbon nanotubes, semiconductor carbon nanometer tube and Metal Contact, between source-drain electrode, add onesize voltage, the difference of electric current, I-V characteristic relation when wherein (I) represents metallic carbon nanotubes and Metal Contact, (II) represents the I-V characteristic relation of semiconductor carbon nanometer tube and Metal Contact.
Fig. 3 shows that the present invention removes the method flow diagram of metallic carbon nanotubes in carbon nano pipe array.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, further describe the present invention, but do not limit the present invention in any way.
The present invention removes the method for metallic carbon nanotubes in carbon nano pipe array, to utilize when carbon nano-tube and Metal Contact, the Fermi level of metal is between semiconductor carbon nanometer tube conduction band and valence band, can form Schottky barrier, as shown in Fig. 1 (a), and metallic carbon nanotubes does not have band gap, can not form Schottky barrier, as shown in Fig. 1 (b), therefore the resistance that semiconductive carbon nano tube contact forms is larger, cause under same voltage semiconductive carbon nano tube current ratio metallic carbon nanotubes electric current little, as shown in Figure 2, between source-drain electrode, add onesize voltage (V ds) time, electric current (I when metallic carbon nanotubes and Metal Contact ds) be obviously greater than the electric current (I of semiconductor carbon nanometer tube and Metal Contact ds).
Based on this, can adopt that electric current calcination, microwave are auxiliary blows and the method such as hot capillary glue method is removed metallic carbon nanotubes in carbon nano pipe array, as shown in Figure 3, concrete facility scheme of the present invention has three to method flow:
Embodiment 1, large electric current blow method
1, by chemical vapour deposition (CVD), in quartz substrate, prepare carbon nano pipe array.Plated film after the photoetching of use double-layer glue (AR-P3510T-AR BR5480), plates the metallic film that 0.5nm is thick, and carbon source is used methane, ethanol and isopropyl alcohol etc.;
2, by photoetching or electron beam exposure, then electron beam plated film, in the substrate of the carbon nano pipe array of having grown, plate Ti/Au(20/30nm), electrode width is 2 μ m, spacing is that 10 μ m are to 30 μ m;
3, under atmospheric environment, at source-drain electrode, add voltage more than 50V, switch on 5 minutes;
4, remove source-drain electrode Ti/Au, first use SU-8 glue to be spin-coated on slice, thin piece, utilize photoetching having the place of metal electrode to output window, use 20g KI/5g I 2/ 400ml H 2the solution that O is mixed to get soaks 1 minute, and metal is leaked in removal source.
Embodiment 2, the auxiliary method of blowing of microwave
1, by chemical vapour deposition (CVD), in quartz substrate, prepare carbon nano pipe array.Plated film after the photoetching of use double-layer glue (AR-P3510T-AR BR5480), plates the metallic film that 0.5nm is thick, and carbon source is used methane, ethanol and isopropyl alcohol etc.;
2, by photoetching or electron beam exposure, then electron beam plated film, in the substrate of the carbon nano pipe array of having grown, plate Ti/Au(20/30nm), electrode width is 2 μ m, spacing is that 10 μ m are to 30 μ m;
3, under atmospheric environment, at source-drain electrode, add voltage more than 50V, to switch on 5 minutes, the microwave that simultaneously in addition frequency is 2.45GHz is auxiliary;
4, remove source-drain electrode Ti/Au, first use SU-8 glue to be spin-coated on slice, thin piece, utilize photoetching having the place of metal electrode to output window, use 20g KI/5g I 2/ 400ml H 2the solution that O is mixed to get soaks 1 minute, and metal is leaked in removal source.
Embodiment 3, hot capillary glue method
1, by chemical vapour deposition (CVD), in quartz substrate, prepare carbon nano pipe array.Plated film after the photoetching of use double-layer glue (AR-P3510T-AR BR5480), plates the metallic film that 0.5nm is thick, and carbon source is used methane, ethanol and isopropyl alcohol etc.;
2, by photoetching or electron beam exposure, then electron beam plated film, in the substrate of the carbon nano pipe array of having grown, plate Ti/Au(20/30nm), electrode width is 2 μ m, spacing is that 10 μ m are to 30 μ m;
3, by thermal evaporation plated film instrument, steam the upper thick TPPA film of 25nm, full name A, A, A '-tri-(4-hydroxyphenyl)-1-ethyl-4-isopropylbenzene; Slice, thin piece is placed into (atmospheric environment) on pyrometric probe platform and is heated to 90 ℃, between leaking, source adds successively 8V, 10V, 12V, 14V each 5 minutes, the voltage object that raises is successively to be placed under large voltage, the defective metal tube of part can blow, thereby do not reach the object of removing metallic carbon nanotubes completely, the TPPA covering in metallic carbon nanotubes so can be by boiled, and the existence of semiconductor Schottky barrier owing to contacting with metal Ti, electric current is smaller, generate heat low, major part still can be covered by glue; In ICP, O is set 2/ CF 4(1:1 mixing) etching 25s, to 30s, removes metallic carbon nanotubes, CF 4the effect of gas is the anti-etching ability that strengthens TPPA, and semiconductor carbon nanometer tube can not be etched under the protection of TPPA; Remove TPPA cull, CF 4there is halogenating reaction in gas and TPPA, generates fluoric ether, and general solvent comprises that ethanol, acetone, NMP etc. cannot remove totally, need to be under the protection of Ar gas or in vacuum, and 600 ℃ of above calcinations more than 5 hours, just can be removed cull totally completely;
4, remove source-drain electrode Ti/Au, first use SU-8 glue to be spin-coated on slice, thin piece, utilize photoetching having the place of metal electrode to output window, use 20g KI/5g I 2/ 400ml H 2the solution that O is mixed to get soaks 1 minute, and metal is leaked in removal source;
5, the carbon nano-tube of removing under source-drain electrode is residual, and O is set in ICP 2/ CF 4(1:1 mixing) etching 25s is to 30s, and etching carbon nano-tube, is finally that SU-8Remover removes SU-8 glue.

Claims (10)

1. a method of removing metallic carbon nanotubes in carbon nano pipe array, comprises the following steps:
1) in substrate, prepare carbon nano pipe array;
2) in the substrate of the carbon nano pipe array of having grown, make source-drain electrode, make the metal of source-drain electrode for can form with semiconductor carbon nanometer tube the metal of Schottky contacts;
3) use constant pressure source or seasonal power to source-drain electrode making alive, blow metallic carbon nanotubes;
4) remove source-drain electrode.
2. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, is characterized in that, in step 1), described substrate is the substrate that has crystal lattice orientation, comprises quartz and sapphire.
3. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, is characterized in that step 2) in, the metal of making source-drain electrode comprises Ti, Al, Cu, Cr, Ca; Described Schottky contacts is symmetrical contact or asymmetric contact; The channel length of described source-drain electrode is 2-30 μ m.
4. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, is characterized in that, in step 3), use constant pressure source is to source-drain electrode institute making alive for more than 5V/ μ m, and energising is more than 5 minutes.
5. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, is characterized in that, in step 3), also comprises to source-drain electrode is alive and carbon nano pipe array is imposed to microwave simultaneously, the auxiliary metallic carbon nanotubes of blowing.
6. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 5, is characterized in that, the microwave frequency of described microwave is 2-3GHz.
7. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, it is characterized in that, in step 3), also comprise before energising evaporation one deck TPPA heat substrate in substrate, periodic power supply adds the voltage that rises to successively 14V/ μ m from 8V/ μ m, the TPPA in boiled metallic carbon nanotubes between source-drain electrode; After etching away the metallic carbon nanotubes of not protected by TPPA, remove TPPA cull.
8. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 7, is characterized in that, the temperature of heating substrate is 60-100 ℃.
9. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 7, is characterized in that, uses dry etching to etch away the metallic carbon nanotubes of not protected by TPPA, and reacting gas is O 2/ CF 41:1 mixes, and etch period is 25-30s; With an organic solvent or high temperature method remove TPPA cull.
10. the method for metallic carbon nanotubes in removal carbon nano pipe array as claimed in claim 1, is characterized in that, in step 4), uses KI/I 2solution dissolves source-drain electrode.
CN201410119928.1A 2014-03-27 2014-03-27 Method for removing metal carbon nano tube in carbon nano tube array Pending CN103943458A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105067479A (en) * 2015-09-01 2015-11-18 解海龙 Method for implementing hybrid type fly ash carbon content online detection device
CN113130620A (en) * 2020-01-15 2021-07-16 清华大学 Field effect transistor

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CN101701927A (en) * 2009-10-14 2010-05-05 苏州纳米技术与纳米仿生研究所 Carbon nanotube array organic pollutant sensor and application thereof
CN102856395A (en) * 2011-06-30 2013-01-02 清华大学 Pressure-control thin film transistor and application thereof

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CN101701927A (en) * 2009-10-14 2010-05-05 苏州纳米技术与纳米仿生研究所 Carbon nanotube array organic pollutant sensor and application thereof
CN102856395A (en) * 2011-06-30 2013-01-02 清华大学 Pressure-control thin film transistor and application thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105067479A (en) * 2015-09-01 2015-11-18 解海龙 Method for implementing hybrid type fly ash carbon content online detection device
CN113130620A (en) * 2020-01-15 2021-07-16 清华大学 Field effect transistor
CN113130620B (en) * 2020-01-15 2023-07-18 清华大学 Field effect transistor

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Application publication date: 20140723