CN1994864B - Method for preparing two-dimensional controllable nano element by carbon nanotube - Google Patents
Method for preparing two-dimensional controllable nano element by carbon nanotube Download PDFInfo
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- CN1994864B CN1994864B CN2006101472363A CN200610147236A CN1994864B CN 1994864 B CN1994864 B CN 1994864B CN 2006101472363 A CN2006101472363 A CN 2006101472363A CN 200610147236 A CN200610147236 A CN 200610147236A CN 1994864 B CN1994864 B CN 1994864B
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Abstract
The invention relates to a method for preparing two-dimension controllable nanometer element via carbon nanometer tube, wherein it comprises that: first preparing one single-wall, dual-wall or multi-wall carbon nanometer tube; then embedding the carbon nanometer tube into insulated polymer to form composite; then slicing the composite to obtain single-hole film; fixing the film into insulated solid support, to obtain the final element. The inventive product has cylinder nanometer hole, high rigidity, non static, while it can recognize electric molecules as dNMPs, rNMPs, and aas, and test the sequence of DNA, RNA and protein.
Description
Technical field
The present invention relates to a kind of preparation method of field of nanometer technology, be specifically related to a kind of method of preparing two-dimensional controllable nano element by carbon nanotube.
Background technology
Exist natural protein hole on the biological protoplast membrane, can carry out in the cell and extracellular ion-exchange, can detect the ion mobility status with patch-clamp.Infect two adipose membranes with AH and form a kind of anisopleural protein nano hole, also can be used for the detection of ion stream, the dynamics research that is used for nucleic acid and single stranded deoxyribonucleic acid (general designation nucleic acid) perforation at present in a large number, detect the size of nucleic acid molecule fragment, and the potentiality of measuring nucleic acid base sequence are arranged, but because the pore volume that this nano-pore is a protein to be formed on two adipose membranes is easily aging, can not tolerate higher voltage, it is bigger that permeability is influenced by pH and salinity, also may exist with nucleic acid and do the site mutually, under effective electric-field intensity, nucleic acid is too fast by the speed of nano-pore, the resolution ratio (1 signal of telecommunication/millisecond) that has exceeded current patch-clamp, can not accurately put down in writing the signal of telecommunication of each base, though the punching rate of nucleic acid has been reduced to the 3nt/ microsecond by regulating electrophoresis liquid component etc., but still having exceeded 3 orders of magnitude of instrumental resolution, these all make the nano-pore order-checking become complicated.In order to overcome the natural defect that the albumen hole exists, carry out methods such as chemical etching, thin polymer film bundle hole and the interior plating of low-density commercial membranes again after people bore a hole with ion beam, electron beam lithography or sputter, heavy ion and prepare solid film, but the three dimension scale of preparation gained nano-pore is uncontrollable, very irregular.Therefore, how the controlled nano-pore of preparation scale has become to improve the key that detects charged molecule such as signal of telecommunication accuracys such as nucleic acid, nucleic acid one phosphoric acid or picodna one phosphoric acid, and the accuracy of DNA and RNA order-checking is played decisive role.
Find through literature search prior art, Sun, L. and Crooks, R.M. at " Journalof the American Chemical Society " (" Journal of the American Chemical Society ", 2000 the 122nd volume 12340-12345 pages or leaves) delivered the article that is entitled as " Single carbon nanotube membranes:Awell-defined model for studying mass transport through nanoporousmaterials " (" single carbon nano-tube film: ") for the accurate model that passes through mano-porous material research in a large number, following technical scheme is proposed: multi-walled carbon nano-tubes is embedded in the epoxy resin, cut into thin slice perpendicular to the nanotube direction again, obtain single hole diameter 153nm, the film of thickness (hole depth) 660nm.But the aperture of this nano-component is too big, can only be used for the detection of diameter at the granules of polystyrene of 100nm, detects ion or less charged molecule such as nucleic acid or its component nucleosides or deoxyribonucleoside one phosphoric acid of diameter and can not be directly used in.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method of preparing two-dimensional controllable nano element by carbon nanotube is proposed, achieve control, improve resolution ratio molecular weight, the variant charged molecule of three-dimensional structure to nano-component two dimension (aperture and hole depth) yardstick.
The inventive method is achieved through the following technical solutions, at first be to obtain single-root carbon nano-tube, single-root carbon nano-tube be embedded into and form complex in the insulating polymer thereafter, then complex is cut into slices, obtain the single hole film, at last the single hole film is fixed on the solid insulation supporter, obtains two-dimensional controllable nano element.
The inventive method concrete steps are as follows:
1. the acquisition of single-root carbon nano-tube: prepare single SWCN or isolate single commercial single wall, double-walled or multi-walled carbon nano-tubes with dispersant, AFM or transmission electron microscope are auxiliary, choose the CNT of internal diameter at 1-3nm;
2. the embedding of single-root carbon nano-tube: the single-root carbon nano-tube of selecting is embedded in the insulating polymer, treats that insulating polymer solidifies the back and forms complex;
3. the section of complex: with diamond cutter (also claiming diamond tool) or laser knife, press 0.2-100 μ m thickness cutting complex perpendicular to the CNT direction, to micron-sized single hole film, AFM confirms that the thickness of single hole film is the hole depth of nano-pore to acquisition thickness in nanometer;
4. the reinforcing of single hole film: the single hole film of the acquisition of will cutting into slices is fixed on insulation solid phase (as silicon chip or the bakelite) supporter and obtains two-dimensional controllable nano element.
Described dispersant is meant dodecane sulfo group acid sodium, octadecylamine or soluble conductive polypyrrole etc.Described insulating polymer is epoxy resin or TEFLON (teflon) etc.
Utilize that nano-pore is the tubular of rule in the two-dimensional controllable nano element of the inventive method preparation, the aperture can be controlled in 1-3nm, and hole depth can be controlled in 0.2-100 μ m, has overcome the irregular problem of the nano-pore for preparing in the prior art.The two-dimensional controllable nano element of the inventive method preparation will be for providing crucial sensor based on DNA, the RNA of excision enzyme and protein single-molecule sequencing and other charged molecules perforation dynamics research.
Description of drawings
Fig. 1 is the inventive method process schematic diagram
The specific embodiment
As shown in Figure 1, make or pick out single single wall, double-walled or the multi-walled carbon nano-tubes 1 of internal diameter at 1-3nm, then with it with epoxy resin or TEFLON embedding, treat that epoxy resin or TEFLON solidify the back and form complex 2, perpendicular to CNT 1 longitudinal axis, press 0.2-100 μ m thickness complex 2 is cut into slices with diamond cutter or laser knife 3, obtain single hole film 4, after AFM is confirmed, single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.
Embodiment 1
With the directed overlength of making of chemical vapour deposition technique, internal diameter is at the single SWCN 1 (realizing the first dimension control) of 1-3nm, with epoxy resin that this CNT 1 is down sticking from pedestal, treat epoxy resin solidify the back with CNT 1 towards last mode, this CNT 1 is placed the rectangular die (three dimension scale is at 5-50mm) that fills epoxy resin, CNT 1 longitudinal axis is consistent with the mould y direction, packing volume is that half of mould is advisable, adding epoxy resin again above CNT 1 fills up mould, fixing back obtains the complex 2 of CNT and epoxy resin, complex 2 is fixed on the microtome, with diamond cutter 3 perpendicular to CNT 1 longitudinal axis, increase step by step with the thickness about 50nm, cut out the single hole film 4 (200nm-100 μ m) (realizing the second dimension control) of different-thickness, after AFM characterizes and confirms, again above-mentioned single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.The insulation solid support adopts silicon chip or bakelite, and there is the aperture of a diameter at 2-10 μ m at the center, and profile can be square or rectangle, yardstick: long and wide about 1cm, thickness is in the mm level, and is suitable to be operable as by hand.
Effect: utilize with single SWCN with the epoxy resin embedding after, cut into slices through diamond cutter again, the two-dimensional controllable nano element of reinforcing at last and obtaining, it is sturdy and durable, tubular nano-pore regular shape in the nano-component, the bright and clean no static of hole wall, and aperture and hole depth are controlled at nanoscale, to the recognition accuracy of dNMPs person's handwriting at 99-100%.
Embodiment 2
Purchase commercial double-walled or multi-walled carbon nano-tubes, after dodecane sulfo group acid sodium mixes, mixed liquor is spread upon on glass or the silicon chip, AFM is checked, find out the single-root carbon nano-tube 1 (realize first dimension control) of internal diameter at 1-3nm, with epoxy resin that it is down sticking from pedestal, after treating that epoxy resin solidifies, with CNT 1 towards on be placed in the rectangular die (three dimension scale is at 5-50mm) that fills epoxy resin, CNT 1 longitudinal axis is consistent with the mould y direction, packing volume is that half of mould is advisable, and adds epoxy resin again above CNT 1 mould is filled up, and fixing back obtains the complex 2 of CNT and epoxy resin; Complex 2 is fixed on the microtome, with diamond cutter 3 perpendicular to CNT 1 longitudinal axis, increase (realizing that second dimension is in nano level control) step by step with the thickness about 50nm, cutting complex 2, obtain the single hole film 4 (200nm-100 μ m) of different-thickness, after AFM characterizes and confirms, again single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.The insulation solid support adopts silicon chip or bakelite, and there is the aperture of a diameter at 2-10 μ m at the center, and profile can be square or rectangle, yardstick: long and wide about 1cm, thickness is in the mm level, and is suitable to be operable as by hand.
Effect: utilize with after double-walled or the effective epoxy resin embedding of multi-wall carbon nano-tube, cut into slices through diamond cutter again, the two-dimensional controllable nano element of reinforcing at last and obtaining, it is sturdy and durable, tubular nano-pore regular shape in the nano-component, the bright and clean no static of hole wall, and aperture and hole depth are controlled at nanoscale, to the recognition accuracy of dNMPs person's handwriting at 99-100%.
Embodiment 3
With the directed single SWCN 1 (realizing the first dimension control) of making overlength, internal diameter at 1-3nm of chemical vapour deposition technique, with epoxy resin that this CNT 1 is down sticking from pedestal, treat epoxy resin solidify the back with CNT 1 towards on place the rectangular die (three dimension scale is at 5-50mm) that fills epoxy resin, CNT 1 longitudinal axis is consistent with the mould y direction, packing volume is that half of mould is advisable, add epoxy resin again above CNT 1 mould is filled up, fixing back obtains the complex 2 of CNT and epoxy resin.Complex 2 is fixed on the slicer, with laser knife 3 perpendicular to CNT 1 longitudinal axis, increase step by step with the thickness about 100nm, cutting complex 2, obtain the single hole film 4 (200nm-100 μ m) (realizing the second dimension control) of different-thickness, after AFM characterizes and confirms, again single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.The insulation solid support adopts silicon chip or bakelite, and there is the aperture of a diameter at 2-10 μ m at the center, and profile can be square or rectangle, yardstick: long and wide about 1cm, thickness is in the mm level, and is suitable to be operable as by hand.
Effect: utilize with single SWCN with embedding epoxy resin after, cut into slices through laser knife again, the two-dimensional controllable nano element of reinforcing at last and obtaining, it is sturdy and durable, tubular nano-pore regular shape in the nano-component, the bright and clean no static of hole wall, and aperture and hole depth are controlled at nanoscale, to the recognition accuracy of dNMPs person's handwriting at 99-100%.
Embodiment 4
Purchase commercial double-walled or multi-walled carbon nano-tubes, after octadecylamine mixes, mixed liquor is spread upon on glass or the silicon chip, AFM is checked, find out the single-root carbon nano-tube 1 (realize first dimension control) of internal diameter at 1-3nm, this CNT 1 is transferred on the TEFLON pedestal of 400 ℃ of curing, again after pedestal adds liquid TEFLON, be warmed to 400 degree, treat that TEFLON solidify to form complex 2, complex 2 is fixed on the microtome, use laser knife 3 perpendicular to CNT 1 longitudinal axis, increase (realizing that second dimension is in nano level control) step by step with the thickness about 100nm, cut complex 2, obtain the single hole film 4 (200nm-100 μ m) of different-thickness, after AFM characterizes and confirms, again single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.The insulation solid support adopts silicon chip or bakelite, and there is the aperture of a diameter at 2-10 μ m at the center, and profile can be square or rectangle, yardstick: long and wide about 1cm, thickness is in the mm level, and is suitable to be operable as by hand.
Effect: utilize with double-walled or multi-walled carbon nano-tubes with the TEFLON embedding after, cut into slices through laser knife again, the two-dimensional controllable nano element of reinforcing at last and obtaining, it is sturdy and durable, tubular nano-pore regular shape in the nano-component, the bright and clean no static of hole wall, and aperture and hole depth are controlled at nanoscale, to the recognition accuracy of dNMPs person's handwriting at 99-100%.
Embodiment 5
With the directed overlength of making of chemical vapour deposition technique, internal diameter is at the single SWCN 1 of 1-3nm, or disperse commercial double-walled or multi-walled carbon nano-tubes with the soluble conductive polypyrrole, the auxiliary single single wall of internal diameter of selecting down of AFM in the 1-3 nanometer, double-walled or multi-walled carbon nano-tubes 1 (realizing the first dimension control), then it is transferred in half mould that fills the TEFLON base (three dimension scale is at 5-50mm), CNT 1 longitudinal axis is consistent with the mould y direction, adding TEFLON again above CNT 1 fills up mould, fixing back obtains the complex 2 of CNT 1 and TEFLON, complex 2 is fixed on the slicer, press perpendicular to CNT 1 y direction with laser knife 3, increase step by step with the thickness about 100nm, cutting complex 2, obtain the single hole film 4 (200nm-100 μ m) (realizing the second dimension control) of different-thickness, after AFM characterizes and confirms, again single hole film 4 is fixed on the insulation solid support, obtains two-dimensional controllable nano element 5.The insulation solid support adopts silicon chip or bakelite, and there is the aperture of a diameter at 2-10 μ m at its center, and profile can be square or rectangle, and is long and wide about 1cm, and thickness is in the mm level, and is suitable to be operable as by hand.
Effect: utilize with SWCN with the TEFLON embedding after, cut into slices through laser knife again, the two-dimensional controllable nano element of reinforcing at last and obtaining, it is sturdy and durable, tubular nano-pore regular shape in the nano-component, the bright and clean no static of hole wall, and aperture and hole depth are controlled at nanoscale, to the recognition accuracy of dNMPs person's handwriting at 99-100%.
Claims (7)
1. the method for a preparing two-dimensional controllable nano element by carbon nanotube, it is characterized in that, at first prepare single SWCN or with dispersant with commercial single wall, double-walled and multi-walled carbon nano-tubes are isolated single-root carbon nano-tube, down auxiliary at AFM or transmission electron microscope, choose the single-root carbon nano-tube of internal diameter at 1-3nm, obtain single-root carbon nano-tube, this CNT be embedded into and form complex in the insulating polymer thereafter, then with complex section with diamond cutter or laser knife perpendicular to the CNT direction, cut above-mentioned complex by 200nm-100 μ m thickness, obtain the single hole film, at last the single hole film is fixed on the insulation solid phase support thing, obtains two-dimensional controllable nano element.
2. the method for preparing two-dimensional controllable nano element by carbon nanotube according to claim 1 is characterized in that, described dispersant is dodecane sulfo group acid sodium, octadecylamine or soluble conductive polypyrrole.
3. the method for preparing two-dimensional controllable nano element by carbon nanotube according to claim 1, it is characterized in that, described with the single-root carbon nano-tube embedding, be specially: the single-root carbon nano-tube of above-mentioned internal diameter at 1-3nm is embedded in the insulating polymer, treats that insulating polymer solidifies the back and forms complex.
4. according to the method for claim 1 or 3 described preparing two-dimensional controllable nano element by carbon nanotube, it is characterized in that described insulating polymer is epoxy resin or TEFLON.
5. the method for preparing two-dimensional controllable nano element by carbon nanotube according to claim 1 is characterized in that, described single hole film, its thickness is the hole depth of nano-pore, in nanometer to micron order.
6. the method for preparing two-dimensional controllable nano element by carbon nanotube according to claim 1, it is characterized in that, described insulation solid phase support thing is silicon chip or bakelite, its center have a diameter aperture, the profile of 2-10 μ m be square or rectangle, length and wide at 1cm, thickness in the mm level.
7. the method for preparing two-dimensional controllable nano element by carbon nanotube according to claim 1 is characterized in that, nano-pore is tubular, aperture 1-3nm, the hole depth 0.2-100 μ m of rule in the described two-dimensional controllable nano element.
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| US8557097B2 (en) * | 2011-09-09 | 2013-10-15 | International Business Machines Corporation | Embedding a nanotube inside a nanopore for DNA translocation |
| CN103820313B (en) * | 2014-03-10 | 2015-07-08 | 东南大学 | Three-channel parallel DNA (deoxyribonucleic acid) sequencing sensor based on nanopore and AFM (atomic force microscopy) and detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1659101A (en) * | 2002-06-03 | 2005-08-24 | 独立行政法人农业·生物系特定产业技术研究机构 | Polymer coated carbon nanotube |
| JP2006028421A (en) * | 2004-07-20 | 2006-02-02 | Osaka Gas Co Ltd | Polymer-modified nanoscale carbon tube and its manufacturing method |
| CN1867626A (en) * | 2003-10-21 | 2006-11-22 | 纳幕尔杜邦公司 | Insulating polymers containing polyaniline and carbon nanotubes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1659101A (en) * | 2002-06-03 | 2005-08-24 | 独立行政法人农业·生物系特定产业技术研究机构 | Polymer coated carbon nanotube |
| CN1867626A (en) * | 2003-10-21 | 2006-11-22 | 纳幕尔杜邦公司 | Insulating polymers containing polyaniline and carbon nanotubes |
| JP2006028421A (en) * | 2004-07-20 | 2006-02-02 | Osaka Gas Co Ltd | Polymer-modified nanoscale carbon tube and its manufacturing method |
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