CN105621387A - High-density semiconductive single-walled carbon nanotube horizontal array and preparation method thereof - Google Patents
High-density semiconductive single-walled carbon nanotube horizontal array and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-density semiconductive single-walled carbon nanotube horizontal array and its preparation method. The array method is a first method or a second method. The first method comprises the following steps: loading a single crystal growth substrate I with a solution of oxide nanoparticles, airing and calcining in the air atmosphere, and carrying out chemical vapor deposition so as to obtain the array on the substrate I. The second method comprises the following steps: loading a single crystal growth substrate II with a solution of oxide nanoparticles, airing and annealing, calcining in the air atmosphere, and carrying out chemical vapor deposition so as to obtain the array on the substrate II. Problems of low density, strong etching, many defects and the like existing in present prepared semiconductive single-walled carbon nanotube horizontal arrays are overcome. The method of the invention is simple and easy to control, is low-cost, has good repeatability, has no metal catalyst residue, and has a wide application prospect in high-end fields of nano-electronics devices, biological medicine and catalytic synthesis, etc.
Description
Technical field
The invention belongs to semiconductor applications, relate to a kind of high-density semiconductor SWCN horizontal array and preparation method thereof.
Background technology
SWCN has perfect conjugated structure and excellent physical property, is always up in nano science field the focus of research, the material of main part in mole epoch nanometer electronic device after being also considered as. SWCN is according to the curling monodimension nanometer material of certain direction vector by Graphene, according to the difference of structure have metallicity and semiconductive point. Owing to the performances such as the electricity of SWCN excellence, optics and mechanics make it have broad application prospects at numerous areas such as nanometer electronic device, energy conversion, bio-sensing and composites. But, restricting current SWCN is in nanometer electronic device field, and especially in large scale integrated circuit, the key issue of application is to obtain high-density semiconductor SWCN horizontal array. The preparation present situation of existing SWCN horizontal array be every micron under the density of actual SWCN less than 50, and there is no metallicity and semiconductive selectivity, if introducing semi-conductive single-walled carbon nanotubes growth conditions, density often declines to a great extent. Therefore, grasping the technology of preparing of high-density semiconductor SWCN horizontal array, be the basis of a lot of follow-up work, its importance and meaning are self-evident.
Summary of the invention
It is an object of the invention to provide a kind of high-density semiconductor SWCN horizontal array and preparation method thereof.
The method preparing high-density semiconductor SWCN horizontal array provided by the invention, for following method one or method two;
Wherein, method one comprises the steps:
Crystal growth substrate I loads the solution of oxide nano-particles, calcines in air atmosphere after drying, then carry out chemical vapour deposition (CVD), in described crystal growth substrate I, namely obtain described high-density semiconductor SWCN horizontal array;
Method two comprises the steps:
Crystal growth substrate II loads the solution of oxide nano-particles, it is annealed after drying, air atmosphere is calcined, then carries out chemical vapour deposition (CVD), in described crystal growth substrate II, namely obtain described high-density semiconductor SWCN horizontal array.
In said method, the material constituting described crystal growth substrate I is that ST cuts quartz or R cuts quartz, it is preferable that ST cuts quartz;
The material constituting described crystal growth substrate II is a face alpha-aluminium oxide, r face alpha-aluminium oxide or magnesium oxide, it is preferable that a face alpha-aluminium oxide;
In the solution of described oxide nano-particles, oxide nano-particles is selected from Ce2O3��Cr2O3��Ga2O3��In2O3��La2O3��MnO2��Nb2O5��TiO2��V2O5��Yb2O3��ZnO��ZrO2��Al2O3��MgO��B2O3And V2O3In at least one;
Solvent is selected from least one in ethanol, isopropanol and hexamethylene;
In the solution of described oxide nano-particles, the concentration of oxide nano-particles is 0.01mmol/L��50mmol/L, is specially 0.5mmol/L.
In the solution step of described loading oxide nano-particles, loading method is by the solution spin coating of described oxide nano-particles or drop coating or the surface dipping described crystal growth substrate after the pre-treatment;
Described method one also comprises the steps:
Before the solution step of described loading oxide nano-particles, described crystal growth substrate I is carried out pretreatment;
Described pretreatment specifically includes following steps: each ultrasonic cleaning 10min in ultra-pure water, acetone, ethanol and ultra-pure water successively by described crystal growth substrate I, after nitrogen dries up, constant temperature 8h after being risen to 900 DEG C by room temperature in 2h, then in 10h, it is cooled to 300 DEG C, then it is naturally cooling to room temperature;
Described method two also comprises the steps:
Before the solution step of described loading oxide nano-particles, described crystal growth substrate II is carried out pretreatment;
Described pretreatment specifically includes following steps: each ultrasonic cleaning 10min in ultra-pure water, acetone, ethanol and ultra-pure water successively by described crystal growth substrate II, after nitrogen dries up, constant temperature 8h after being risen to 1100 DEG C by room temperature in 2h, then in 10h, it is cooled to 300 DEG C, then it is naturally cooling to room temperature.
The annealing of described method two comprises the steps:
In air atmosphere, risen to after annealing temperature after constant temperature 3min��24h by room temperature in 2h, then in 10h, be cooled to 300 DEG C, then be naturally cooling to room temperature;
Described annealing temperature is 600-1300 DEG C, is specially 1100 DEG C; Annealing time is specially 8h;
In the calcining step of described method one and method two, calcination atmosphere is air atmosphere; Calcining heat is 800-850 DEG C; Calcination time is 3-60min, is specially 20min.
In described chemical vapor deposition step method, carbon source is to be easier carbonaceous gas or the carbonaceous liquid that cracks more greatly and easily of vapour pressure, the concretely CH of cracking under 700 DEG C��1000 DEG C reaction temperatures4��C2H4, ethanol or isopropanol; Ethanol carbon source is produced by Ar gas bell alcoholic solution;
The gas flow of carbon source is 10sccm-500sccm, is specially 100sccm, 150sccm, 200sccm;
Reducing atmosphere is hydrogen atmosphere; The gas flow of hydrogen is 30-500sccm, is specially 50sccm, 100sccm, 150sccm, 200sccm, 250sccm, 300sccm, 400sccm;
Carrier gas used by reducing atmosphere is argon or nitrogen; The air flow rate of described carrier gas is 50-500sccm, is specially 300sccm;
Growth temperature is 600 DEG C-900 DEG C, is specially 830 DEG C;
Growth time is 1min��1h, is specially 30min.
Described method also comprises the steps: after described chemical vapor deposition step, system is lowered the temperature;
Described cooling is specially Temperature fall or programme-control cooling.
It addition, the high-density semiconductor SWCN horizontal array prepared according to the method described above, fall within protection scope of the present invention. In described high-density semiconductor SWCN horizontal array, the radical of semi-conductive single-walled carbon nanotubes accounts for the percentage ratio of the total radical of SWCN and is not less than 90%; The density of described high-density semiconductor SWCN horizontal array is 60��80 pieces/micron.
In the present invention, conductor oxidate (TiO2��ZnO��ZrO2And Cr2O3) the SWCN horizontal array for preparing under certain growth conditions has quasiconductor selectivity, semi-conductive single-walled carbon nanotubes content can be regulated and controled by changing hydrogen and comparing of ethanol in growth atmosphere, and under the same conditions, insulator oxide thing SiO2The SWCN horizontal array of preparation does not have quasiconductor selectivity.
The SWCN horizontal array of preparation in the present invention is carried out wavelength Raman spectrum and field-effect transistor performance test characterizes, semi-conductive single-walled carbon nanotubes content >=90%. Meanwhile, high resolution scanning electron microscope (SEM) and atomic force microscope (AFM) characterize its density and reach 60��80 pieces/micron.
The present invention is from Catalyst Design angle, select a series of semiconductive oxide particles as appropriate carbon nanotube growth catalysts, utilize the difference that semiconductive oxide particles contacts with different conductive properties carbon nanotube interface, selectivity prepares high-density semiconductor SWCN horizontal array, overcomes and existing prepares the problems such as semi-conductive single-walled carbon nanotubes horizontal array density etching low, strong, many defects. The method is simple and easy to control, with low cost, reproducible, and non-metal catalyst residual, in nanometer electronic device, biological medicine with the high-end field such as catalyze and synthesize and have broad prospect of application.
Accompanying drawing explanation
Fig. 1 is different oxide catalyst at different hydrogen than under the argon of bulging ethanol, the Raman statistical result of the semiconductive carbon nano tube content of growing single-wall carbon nano tube horizontal array.
Fig. 2 is TiO2As catalyst, 200sccm argon drum ethanol, under 200sccm hydrogen growth conditions, the electrical properties of the semiconductive carbon nano tube content of the SWCN horizontal array of preparation measures statistical result.
Fig. 3 is the SEM figure of high-density semiconductor SWCN horizontal array; Wherein, a), b), c), d) scheme for the SEM under same sample different amplification, corresponding scale size respectively 1mm, 100 ��m, 10 ��m and 400nm.
Fig. 4 is the AFM figure of VHD SWCN horizontal array; Wherein, a) and b) for the AFM under same sample different scanning scope scheming, corresponding sweep limits is 5 ��m and 1 ��m respectively.
Fig. 5 is the wavelength Raman figure of high-density semiconductor SWCN horizontal array, schemes spectrum a) illustrating excitation wavelength 514nm, schemes spectrum b) illustrating excitation wavelength 633nm
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following example. Described method is conventional method if no special instructions. Described raw material all can obtain from open commercial sources if no special instructions.
Embodiment 1
1) ethanolamine of phthalandione four butyl ester and 61 �� L pipetting 34 �� L with liquid-transfering gun is dissolved in the ethanol solution of 150mL, stir, by mixed solution (the ethanol 50mL of ethanol and ultra-pure water, ultra-pure water 9 �� L) it is added dropwise in above-mentioned mixed solution, continue stirring and obtain the vitreosol that titanium elements concentration is 0.5mmol/L.
2) a small amount of above-mentioned TiO is dipped2Colloidal sol, utilizes micro-contact-printing to prepare the catalyst band of line style patterning in ST-cut single crystal quartz substrate, and strip direction is vertical with substrate surface lattice direction. The substrate being loaded with catalyst is inserted in chemical gas-phase deposition system, is warming up to 800 DEG C, air is calcined 20min, it is thus achieved that TiO2Nanoparticle, passes into air in 300sccm argon 5min discharge system, then with 200sccm bubbling argon ethanol, and passes into a certain amount of hydrogen, grows 30min under the growth temperature of 800 DEG C. regulate the argon different volumes ratio (1:2 of hydrogen and bubbling ethanol, 1:1, 3:2, 2:1, 5:2), corresponding hydrogen flowing quantity is 100sccm, 200sccm, 300sccm, 400sccm and 500sccm, obtain different semiconductor material content SWCN horizontal array, high resolution scanning electron microscope (SEM) and atomic force microscope (AFM) characterize its density and reach 60��80 pieces/micron, Fig. 1 is shown in its multi-wavelength (514nm and 633nm) Raman statistical result, when hydrogen flowing quantity is 200sccm, Raman statistical result shows that in gained SWCN horizontal array, the content of semiconductive carbon nano tube is 92.3%, basically identical with electrical testing statistical result 90% (see Fig. 2), absolutely prove that under this condition, the SWCN horizontal array of preparation has higher quasiconductor selectivity.
Embodiment 2
1) prepare TiO 2 sol by the method for embodiment 1, be spin-coated on the alpha-aluminium oxide of a face, spin coating has the substrate of catalyst be placed in Muffle furnace, 1100 DEG C of annealing 8h in air, then 10h is cooled to 300 DEG C, then naturally cools to room temperature.
2) alumina substrate that above-mentioned loading catalyst has moved back fire is inserted in chemical gas-phase deposition system, it is warming up to 850 DEG C, air is calcined 20min, pass into 300sccm argon 5min, then with 150sccm bubbling argon ethanol, and pass into 300sccm hydrogen, under the growth temperature of 850 DEG C, grow 30min, prepare high-density semiconductor SWCN horizontal array.
High resolution scanning electron microscope (SEM) and atomic force microscope (AFM) characterize its density and reach 60��80 pieces/micron, as shown in Fig. 3, Fig. 4. Its Raman spectrogram such as Fig. 5 a and 5b (Fig. 5 a illustrates the spectrum of excitation wavelength 514nm, and Fig. 5 b illustrates the spectrum of excitation wavelength 633nm), its semi-conductive single-walled carbon nanotubes content >=90%.
Reference examples 1
1) pipette 23 �� L tetraethyl orthosilicates with liquid-transfering gun and be dissolved in the ethanol solution of 100mL, stir, pipette in the ethanol solution that the concentrated nitric acid of 18 �� L adds another part of 100mL with liquid-transfering gun again, by two solution mix homogeneously, 70 DEG C of water-baths, it is heated to reflux 2h, obtains element silicon concentration and be about the vitreosol of 0.5mmoL/L.
2) similar with embodiment 1 method, dip a small amount of above-mentioned SiO2The substrate being loaded with catalyst, in ST-cut single crystal quartz substrate, is then inserted in chemical gas-phase deposition system by colloidal sol, is warming up to 800 DEG C, calcines 20min, it is thus achieved that SiO in air2Nanoparticle, passes into air in 300sccm argon 5min discharge system, then with 100sccm bubbling argon ethanol, and passes into a certain amount of hydrogen, grows 30min under the growth temperature of 800 DEG C. Regulate argon different volumes ratio (1:2,1:1, the 3:2 of hydrogen and bubbling ethanol, 2:1,5:2), corresponding hydrogen flowing quantity is 50sccm, 100sccm, 150sccm, 200sccm and 250sccm, the SWCN horizontal array obtained, its multi-wavelength (514nm and 633nm) Raman statistical result such as accompanying drawing 1, semiconductive carbon nano tube content is only 65%, and insulator oxide thing SiO is described2The SWCN horizontal array of preparation does not have quasiconductor selectivity.
Claims (8)
1. the method preparing high-density semiconductor SWCN horizontal array, for following method one or method two;
Wherein, method one comprises the steps:
Crystal growth substrate I loads the solution of oxide nano-particles, calcines in air atmosphere after drying, then carry out chemical vapour deposition (CVD), in described crystal growth substrate I, namely obtain described high-density semiconductor SWCN horizontal array;
Method two comprises the steps: to load the solution of oxide nano-particles in crystal growth substrate II, it is annealed after drying, air atmosphere is calcined, carry out chemical vapour deposition (CVD) again, in described crystal growth substrate II, namely obtain described high-density semiconductor SWCN horizontal array.
2. method according to claim 1, it is characterised in that: the material constituting described crystal growth substrate I is that ST cuts quartz or R cuts quartz, it is preferable that ST cuts quartz;
The material constituting described crystal growth substrate II is a face alpha-aluminium oxide, r face alpha-aluminium oxide or magnesium oxide, it is preferable that a face alpha-aluminium oxide;
In the solution of described oxide nano-particles, oxide nano-particles is selected from Ce2O3��Cr2O3��Ga2O3��In2O3��La2O3��MnO2��Nb2O5��TiO2��V2O5��Yb2O3��ZnO��ZrO2��Al2O3��MgO��B2O3And V2O3In at least one;
Solvent is selected from least one in ethanol, isopropanol and hexamethylene;
In the solution of described oxide nano-particles, the concentration of oxide nano-particles is 0.01mmol/L��50mmol/L, is specially 0.5mmol/L.
3. method according to claim 1 and 2, it is characterised in that: described method one also comprises the steps:
Before the solution step of described loading oxide nano-particles, described crystal growth substrate I is carried out pretreatment;
Described pretreatment specifically includes following steps: each ultrasonic cleaning 10min in ultra-pure water, acetone, ethanol and ultra-pure water successively by described crystal growth substrate I, after nitrogen dries up, constant temperature 8h after being risen to 900 DEG C by room temperature in 2h, then in 10h, it is cooled to 300 DEG C, then it is naturally cooling to room temperature;
Described method two also comprises the steps:
Before the solution step of described loading oxide nano-particles, described crystal growth substrate II is carried out pretreatment;
Described pretreatment specifically includes following steps: each ultrasonic cleaning 10min in ultra-pure water, acetone, ethanol and ultra-pure water successively by described crystal growth substrate II, after nitrogen dries up, constant temperature 8h after being risen to 1100 DEG C by room temperature in 2h, then in 10h, it is cooled to 300 DEG C, then it is naturally cooling to room temperature.
4. according to the arbitrary described method of claim 1-3, it is characterised in that: the annealing of described method two comprises the steps:
In air atmosphere, risen to after annealing temperature after constant temperature 3min��24h by room temperature in 2h, then in 10h, be cooled to 300 DEG C, then be naturally cooling to room temperature;
Described annealing temperature is 600-1300 DEG C, is specially 1100 DEG C; Annealing time is specially 8h;
In the calcining step of described method one and method two, calcination atmosphere is air atmosphere; Calcining heat is 800-850 DEG C; Calcination time is 3-60min, is specially 20min.
5. according to the arbitrary described method of claim 1-4, it is characterised in that: in described chemical gaseous phase depositing process, carbon source is CH4��C2H4, ethanol or isopropanol; The gas flow of carbon source is 10-500sccm;
Reducing atmosphere is hydrogen atmosphere; The gas flow of hydrogen is 30-500sccm;
Carrier gas used by reducing atmosphere is argon or nitrogen; The air flow rate of described carrier gas is 50-500sccm, is specially 300sccm;
Growth temperature is 600 DEG C-900 DEG C, is specially 830 DEG C;
Growth time is 1min��1h, is specially 30min.
6. according to the arbitrary described method of claim 1-5, it is characterised in that: described method all also comprises the steps: after described chemical vapor deposition step, system is lowered the temperature;
Described cooling is specially Temperature fall or programme-control cooling.
7. the high-density semiconductor SWCN horizontal array that the arbitrary described method of claim 1-6 prepares.
8. array according to claim 7, it is characterised in that: in described high-density semiconductor SWCN horizontal array, the radical of semi-conductive single-walled carbon nanotubes accounts for the percentage ratio of the total radical of SWCN and is not less than 90%;
The density of described high-density semiconductor SWCN horizontal array is 60��80 pieces/micron.
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Cited By (5)
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| CN109678138A (en) * | 2019-01-09 | 2019-04-26 | 温州大学 | A kind of preparation method of unidextrality single-walled carbon nanotube |
| CN109881157A (en) * | 2019-03-19 | 2019-06-14 | 南京航空航天大学 | A method of periodically regulation vanadium dioxide film phase transition property |
| CN111943171A (en) * | 2020-08-21 | 2020-11-17 | 温州大学 | Controllable preparation method of high-density single-walled carbon nanotube horizontal array |
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
| CN116374998A (en) * | 2023-04-20 | 2023-07-04 | 温州大学 | Preparation method for directly growing single-walled carbon nanotube horizontal array by using silicon oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109678138A (en) * | 2019-01-09 | 2019-04-26 | 温州大学 | A kind of preparation method of unidextrality single-walled carbon nanotube |
| CN109678138B (en) * | 2019-01-09 | 2022-04-26 | 温州大学 | Preparation method of single-chiral single-walled carbon nanotube |
| CN109881157A (en) * | 2019-03-19 | 2019-06-14 | 南京航空航天大学 | A method of periodically regulation vanadium dioxide film phase transition property |
| CN111943171A (en) * | 2020-08-21 | 2020-11-17 | 温州大学 | Controllable preparation method of high-density single-walled carbon nanotube horizontal array |
| CN113788474A (en) * | 2021-11-04 | 2021-12-14 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
| CN113788474B (en) * | 2021-11-04 | 2023-03-17 | 航天特种材料及工艺技术研究所 | Graphene nanoribbon horizontal array and preparation method and application thereof |
| CN116374998A (en) * | 2023-04-20 | 2023-07-04 | 温州大学 | Preparation method for directly growing single-walled carbon nanotube horizontal array by using silicon oxide |
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