CN105529401A - P-n junction diode in carbon nanotube molecule and preparation method thereof - Google Patents
P-n junction diode in carbon nanotube molecule and preparation method thereof Download PDFInfo
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- CN105529401A CN105529401A CN201610060895.7A CN201610060895A CN105529401A CN 105529401 A CN105529401 A CN 105529401A CN 201610060895 A CN201610060895 A CN 201610060895A CN 105529401 A CN105529401 A CN 105529401A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 85
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000000609 electron-beam lithography Methods 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 15
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 229920002873 Polyethylenimine Polymers 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010894 electron beam technology Methods 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 238000004626 scanning electron microscopy Methods 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004880 explosion Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002238 carbon nanotube film Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000002109 single walled nanotube Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229910021404 metallic carbon Inorganic materials 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K10/00—Organic devices specially adapted for rectifying, amplifying, oscillating or switching; Organic capacitors or resistors having potential barriers
- H10K10/701—Organic molecular electronic devices
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
- H10K85/221—Carbon nanotubes
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Light Receiving Elements (AREA)
- Electrodes Of Semiconductors (AREA)
Abstract
The invention discloses a p-n junction diode in a carbon nanotube molecule and a preparation method thereof. The preparation method comprises the steps of manufacturing metal electrodes at two ends of a carbon nanotube positioned on a substrate by an electron beam lithography and magnetron sputtering manner, then respectively performing p-type doping and n-type doping on left and right parts of the single carbon nanotube after spin-coating photoresist and selectively exposing, and thereby obtaining the p-n junction diode in the carbon nanotube molecule. According to the preparation method provided by the invention, the chemical doping method is used, the prepared device is good in rectification characteristic, stable in performance at room temperature in the air; and the diode can be freely regulated and controlled through applying different grid voltages and changing the doping parameter.
Description
Technical field
The present invention relates to a kind of diode fabrication technology, specifically p-n junction diode and preparation method thereof in a kind of carbon nanotube molecule.
Background technology
Along with the development of electronic technology, the size of electronic device enters into nanoscale by micron order.But along with reducing further of device size, due to the impact of quantum effect, traditional material is no longer applicable.Carbon nano-tube a kind ofly has excellent mechanical performance and the monodimension nanometer material of Electronic Performance, is considered to the first-selection making following nano-device.At present, a lot of nano electron devices based on carbon nano-tube are successfully made, such as field-effect transistor, rectifier and memory etc.
Similar with microelectronic component, various nano junction will be the formant that following nanometric circuit builds.At present, mainly utilize the method for physics to construct various nano junction, method is complicated, and performance is difficult to regulation and control.Similar with traditional silicon device, utilize the method for chemical doping to regulate and control the conductive characteristic of carbon nano-tube, make its one end present p-type, and the other end presents N-shaped, so just can make p-n junction diode in carbon nanotube molecule.In this molecule, diode shows good rectification characteristic, can be used to make rectification circuit and logic gates.
Through finding the retrieval of prior art, Chinese patent literature CN101656278, open (bulletin) day 2010.02.24, disclose a kind of preparation method of the solar micro battery based on unordered mesh carbon nanotube film of energy field, self-assembling technique is adopted to prepare unordered mesh carbon nanotube film, use methane plasma selective etch method or big current method of blowing to remove metallic carbon nanotubes, obtain the light-sensitive material of large-area unordered reticulated semiconductor carbon nano-tube film as solar micro battery.The metal with asymmetric work function is used to contact with semiconductor carbon nanometer tube respectively as the asymmetric electrode of device, unsymmetrical knot is formed respectively in the contact position, two ends of semiconductor carbon nanometer tube, thus strong internal electric field is formed in single wall semiconductor carbon nanometer tube, impel photo-generate electron-hole to separation.But unordered mesh carbon nanotube film adds the contact resistance between carbon nano-tube and carbon nano-tube, thus the excellent properties of carbon nano-tube cannot be played completely.In addition, unsymmetric structure can not realize the regulation and control to device performance.
Summary of the invention
The present invention is directed to defect and the deficiency of above-mentioned prior art, propose p-n junction diode and preparation method thereof in a kind of carbon nanotube molecule with chemical doping, this device has good rectification characteristic and stability.
The present invention is achieved through the following technical solutions:
The present invention relates to a kind of preparation method of the p-n junction diode based on single-root carbon nano-tube, metal electrode is made by adopting electron beam lithography and magnetron sputtering mode at the two ends being positioned on-chip carbon nano-tube, then after selectivity exposure, p-type doping and N-shaped doping are carried out respectively to left and right two parts of single-root carbon nano-tube by spin coating photoresist, thus prepare p-n junction diode in single-root carbon nano-tube molecule.
Described location, by the carbon nano-tube solution through ultrasonic disperse is coated on substrate surface, after solvent evaporates is complete, by scanning electron microscopy substrate observed and select the carbon nano-tube that length is more than 3 μm, by means of the cross mark that substrate makes in advance, carbon nano-tube being positioned.
Described carbon nano-tube, be preferably single wall semiconductive carbon nano tube, diameter is 0.9 ~ 1.8nm, and length is 2 ~ 5 μm.
The solvent of described carbon nano-tube solution adopts but is not limited to the volatile solvents such as isopropyl alcohol, ethanol, methyl alcohol.
Described substrate adopts but is not limited to have SiO
2the silicon chip of thermal oxide layer.
Described cross mark can adopt mask lithography and magnetron sputtering technique to obtain.
Described electron beam lithography, adopts grating 10, voltage 20kv, line value 100; Described magnetron sputtering, makes metal electrode thickness reach 100nm by regulation and control power, time parameter.
Described metal electrode is preferably symmetrical Au electrode, and its width is 0.5 ~ 1.5 μm, is 2 ~ 10 μm to interelectrode distance, and thickness is 100nm, and wherein Ti is prime coat, and thickness is 10nm.
Described selectivity exposure refers to: the part that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part will be subject to the protection of photoresist PMMA.
Described selectivity exposure, its size can regulate according to carbon length of tube used, is generally 0.5*1 μm ~ 1.5*3 μm.
Described photoresist divides two-layer: the PMMA photoresist of ground floor molecular weight 495, and thickness is about 200nm, and the PMMA photoresist of second layer molecular weight 950, thickness is about 100nm.
Described photoresist, preferably at high temperature carries out drying glue after every layer of spin coating.
Described doping refers to: be soaked in chlordene metaantimmonic acid triethyl group oxygen solution by the device after exposure, be exposed to outer carbon nano-tube one end and will realize p-type doping, or the other end of carbon nano-tube is carried out windowing exposure and be soaked in polyethylenimine solution realizing N-shaped doping, thus obtain p-n junction diode in single-root carbon nano-tube molecule.
The solvent of described chlordene metaantimmonic acid triethyl group oxygen solution (OA) is dichloroethanes, and the concentration of this solution is preferably 10mg/mL.
The solvent of described polyethylenimine solution (PEI) is methyl alcohol, and the concentration of this solution is preferably 20wt%.
The present invention relates to the p-n junction diode based on single-root carbon nano-tube that said method prepares, comprise successively: substrate, SiO
2thermal oxide layer, single-root carbon nano-tube and be positioned at the symmetrical Au electrode at its two ends.
The present invention relates to the application of the above-mentioned p-n junction diode based on single-root carbon nano-tube, use it for the various circuit of preparation and photovoltaic device, be specially: rectification circuit, logical circuit or solar cell.
Technique effect
Compared with prior art, the present invention adopts the method for chemical doping, and the device prepared has excellent rectification characteristic, stable performance in air at room temperature.The present invention, by applying different grid voltage and changing doping parameters, can freely realize regulating and controlling diode behavior.
Accompanying drawing explanation
Fig. 1 be embodiment 1 prepare carbon nanotube molecule in p-n junction diode SEM figure;
Fig. 2 is the I-V curve of p-n junction diode in the carbon nanotube molecule prepared of embodiment 1.
Embodiment
Embodiment 1
The present embodiment comprises the following steps:
Concentration is that the semi-conductive single-walled carbon nanotubes aqueous isopropanol of 0.025mg/mL is coated on silicon chip surface by the first step.Until solvent evaporates completely after, by scanning electron microscopy it observed and select the single-root carbon nano-tube that length is 3 μm, by means of the cross mark that substrate makes in advance, carbon nano-tube being positioned.
Second step, utilize electron beam lithography and magnetron sputtering technique to make Au electrode (as Fig. 1) at carbon nano-tube two ends, be 2 μm to electrode spacing, width is 2 μm.
3rd step, substrate applies electron beam resist, utilizes electron beam lithography to carry out windowing exposure to one end of carbon nano-tube, and window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (1 μm) will be subject to the protection of photoresist PMMA.
4th step, is soaked in device in chlordene metaantimmonic acid triethyl group oxygen solution, is exposed to half outer root carbon nano-tube and will realizes p-type doping, remove PMMA photoresist with acetone.
5th step, applies electron beam resist again on substrate, utilizes electron beam lithography to carry out windowing exposure to the other end of carbon nano-tube, and window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (1 μm) will be subject to the protection of photoresist PMMA.Be soaked in polyethylenimine solution the N-shaped doping realizing second half carbon nano-tube.
The present embodiment is prepared p-n junction diode in carbon nanotube molecule and carry out I-V performance test in dark conditions, measuring voltage scope is-10V to+10V.Result shows the increase along with forward voltage, and device current increases in the mode of index; When applying reverse biased, device does not almost have electric current, and device shows good rectification characteristic (as Fig. 2).
Embodiment 2
The present embodiment comprises the following steps:
The first step, is coated with one deck protecting glue at the front side of silicon wafer with the thick thermal oxide layer of 100nm and etches its back side.Layer of metal Au is sputtered immediately as backgate after back-etching cleaning.Protecting glue is fallen with acetone solution, and clean by washed with de-ionized water.
Concentration is that the semi-conductive single-walled carbon nanotubes aqueous isopropanol of 0.025mg/mL is coated on silicon chip front surface by second step.Until solvent evaporates completely after, by scanning electron microscopy it observed and select the single-root carbon nano-tube that length is 3 μm, by means of the cross mark that substrate makes in advance, carbon nano-tube being positioned.
3rd step, utilize electron beam lithography and magnetron sputtering technique to make Au symmetry electrode at carbon nano-tube two ends, be 2 μm to electrode spacing, width is 2 μm.
4th step, substrate applies electron beam resist, utilizes electron beam lithography to carry out windowing exposure to one end of carbon nano-tube, and window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (1 μm) will be subject to the protection of photoresist PMMA.
5th step, is soaked in device in chlordene metaantimmonic acid triethyl group oxygen solution, is exposed to half outer root carbon nano-tube and will realizes p-type doping, remove PMMA photoresist with acetone.
5th step, applies electron beam resist again on substrate, and utilize electron beam lithography to carry out windowing exposure to second half of carbon nano-tube, window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (1 μm) will be subject to the protection of photoresist PMMA.Be soaked in polyethylenimine solution the N-shaped doping realizing second half carbon nano-tube.
The present embodiment is prepared p-n junction diode in carbon nanotube molecule and carry out I-V performance test in dark conditions, measuring voltage scope is-10V to+10V.Apply grid voltage to device to regulate and control, grid voltage scope is-20V to 20V simultaneously.Result shows the regulation and control that can realize p-n junction diode behavior in carbon nanotube molecule by applying grid voltage.Grid voltage is larger, and the rectification characteristic of device is better.
Embodiment 3
The present embodiment comprises the following steps:
Concentration is that the semi-conductive single-walled carbon nanotubes aqueous isopropanol of 0.025mg/mL is coated on silicon chip surface by the first step.Until solvent evaporates completely after, by scanning electron microscopy it observed and select the carbon nano-tube that length is 4 μm, by means of the cross mark that substrate makes in advance, carbon nano-tube being positioned.
Second step, utilize electron beam lithography and magnetron sputtering technique to make Au electrode at carbon nano-tube two ends, be 3 μm to electrode spacing, width is 2 μm.
3rd step, substrate applies electron beam resist, utilizes electron beam lithography to carry out windowing exposure to one end of carbon nano-tube, and window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (2 μm) will be subject to the protection of photoresist PMMA.
4th step, is soaked in device in chlordene metaantimmonic acid triethyl group oxygen solution, is exposed to outer carbon nano-tube one end and will realizes p-type doping, remove PMMA photoresist with acetone.
5th step, applies electron beam resist again on substrate, utilizes electron beam lithography to carry out windowing exposure to the other end of carbon nano-tube, and window size is 1 μm * 2 μm.The part (1 μm) that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing.Unexposed part (2 μm) will be subject to the protection of photoresist PMMA.Be soaked in polyethylenimine solution the N-shaped doping realizing other end carbon nano-tube.The part of middle undoped retains the reset condition (i) of carbon nano-tube.
In the carbon nanotube molecule prepared by the present embodiment, p-i-n junction diode carries out I-V performance test in dark conditions, and measuring voltage scope is-10V to+10V.Result shows the regulation and control that can realize p-n junction diode behavior in carbon nanotube molecule by increasing i district, increases the appearance that i district can avoid Zener breakdown.
Above-mentioned concrete enforcement can carry out local directed complete set to it by those skilled in the art in a different manner under the prerequisite not deviating from the principle of the invention and aim; protection scope of the present invention is as the criterion with claims and can't help above-mentioned concrete enforcement and limit, and each implementation within the scope of it is all by the constraint of the present invention.
Claims (11)
1. the preparation method of p-n junction diode in a carbon nanotube molecule, it is characterized in that, metal electrode is made by adopting electron beam lithography and magnetron sputtering mode at the two ends being positioned on-chip carbon nano-tube, then after selectivity exposure, p-type doping and N-shaped doping are carried out respectively to left and right two parts of single-root carbon nano-tube by spin coating photoresist, thus prepare p-n junction diode in single-root carbon nano-tube molecule.
2. preparation method according to claim 1, it is characterized in that, described location, by the carbon nano-tube solution through ultrasonic disperse is coated on substrate surface, after solvent evaporates is complete, by scanning electron microscopy substrate observed and select the carbon nano-tube that length is more than 3 μm, by means of the cross mark that substrate makes in advance, carbon nano-tube being positioned.
3. preparation method according to claim 1 and 2, is characterized in that, described carbon nano-tube is single wall semiconductive carbon nano tube, and diameter is 0.9 ~ 1.8nm, and length is 2 ~ 5 μm.
4. preparation method according to claim 1, is characterized in that, described metal electrode is symmetrical Au electrode, and in this Au electrode, Ti is prime coat, and thickness is 10nm.
5. the preparation method according to claim 1 or 4, is characterized in that, the width of described metal electrode is 0.5 ~ 1.5 μm, is 2 ~ 10 μm to interelectrode distance, and thickness is 100nm.
6. preparation method according to claim 1, is characterized in that, described electron beam lithography, adopts grating 10, voltage 20kv, line value 100; Described magnetron sputtering, makes metal electrode thickness reach 100nm by regulation and control power, time parameter.
7. preparation method according to claim 1, it is characterized in that, described selectivity exposure refers to: substrate applies electron beam resist, electron beam lithography is utilized to carry out window explosion to one end of carbon nano-tube, wherein: the part that carbon nano-tube is exposed will be exposed in atmosphere after developing and be fixing, and unexposed part will be subject to the protection of photoresist PMMA;
Described electron beam resist divides two-layer: the PMMA photoresist of ground floor molecular weight 495, the PMMA photoresist of second layer molecular weight 950.
8. preparation method according to claim 1, it is characterized in that, described doping refers to: be soaked in chlordene metaantimmonic acid triethyl group oxygen solution by the device after exposure, be exposed to outer carbon nano-tube one end and will realize p-type doping, or the other end of carbon nano-tube is carried out windowing exposure and be soaked in polyethylenimine solution realizing N-shaped doping, thus obtain p-n junction diode in single-root carbon nano-tube molecule, wherein: the solvent of chlordene metaantimmonic acid triethyl group oxygen solution is dichloroethanes, and the solvent of polyethylenimine solution is methyl alcohol.
9. the preparation method according to claim 1 or 8, is characterized in that, the concentration of described chlordene metaantimmonic acid triethyl group oxygen solution is 10mg/mL; The concentration of described polyethylenimine solution is 20wt%.
10. a p-n junction diode in the single-root carbon nano-tube molecule prepared by method described in above-mentioned arbitrary claim, be is characterized in that, comprise successively: substrate, SiO
2thermal oxide layer, single-root carbon nano-tube and be positioned at the symmetrical Au electrode at its two ends.
In 11. 1 kinds of single-root carbon nano-tube molecules prepared according to described method arbitrary in claim 1 ~ 10, the application of p-n junction diode, is characterized in that, use it for and prepare rectification circuit, logical circuit or solar cell.
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