CN101520430B - Method for manufacturing biological detector of field effect transistor based on carbon nano tube - Google Patents
Method for manufacturing biological detector of field effect transistor based on carbon nano tube Download PDFInfo
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Abstract
The invention relates to a method for manufacturing a biological detector of a field effect transistor based on a non-covalent modified single-walled carbon nano tube, which belongs to the technical field of nano electronic device manufacture and biological analysis and detection. The method comprises the following steps: setting up the single-walled carbon nano tube (beam) between an interdigitalsource electrode and a drain electrode made on a silicon substrate of which the surface contains an insulating oxide according to a photoetching technique; constructing the field effect transistor ba sed on the carbon nano tube; and modifying a non-covalent glycosylation organism on the surface of the carbon nano tube to obtain a field effect transistor based on the carbon nano tube for the detection of the recognition function of saccharide-protein specificity. The method can selectively modify different sugar molecules to detect specificity combining actions between different sugar ligands and receptors so as to form the universal, flexible and efficient biological detector of the field effect transistor based on the carbon nano tube.
Description
Technical field
The present invention relates to a kind of manufacturing approach of the field effect transistor biological detector based on the non-covalent modification SWCN, belong to nanometer electronic device manufacturing and bioanalysis detection technique field.
Background technology
Because the good electric property of SWCN (SWNTs), the field effect transistor of based semiconductor conductive single-walled carbon nanotubes is by broad research.At present, the preparation method mainly contains several big type: the one, and template on the silicon substrate that is processed with specific pattern and catalyzer island, utilizes the CVD method to grow SWCN, combines microelectronic processing technique to reach good Ohmic contact again; The 2nd, the electrode method, earlier with the ultrasonic dispersion of CNT, be uniformly distributed on the silicon substrate, utilize focused ion beam technology on interested CNT, to deposit metal electrode then; The 3rd, at first utilize micro-processing method on substrate, to process nano electrode; Be dispersed in the organic solvent CNT is ultrasonic again; Mode with unrestrained or Spin Coating (spin coating) is dispersed on the substrate surface that is processed with nano electrode; The part CNT is connected between the metal electrode, thereby constitutes the FET device.Also have one type for employing adds auxiliary electric field, the CNT orientation that is dispersed in the organic suspension liquid is connected between the source-drain electrode.Each class methods respectively has relative merits, and application is respectively arranged.Patent documentation (Chinese patent publication number CN1697146A in invention " method of structuring field effect transistor in multiple channels from Nano carbon tubes "; Open day is on November 16th, 2005) in; People such as Zhang Yafei improve the method that adds auxiliary electric field; Many CNTs are connected between the electrode structure with being separated from each other, have proposed a kind of method of structuring field effect transistor in multiple channels from Nano carbon tubes.But be not suitable for follow-up biological detection among the present invention; Reason is may when carbon nano tube surface absorption companion's canavaline (ConA), cause between many CNTs to disturb each other; Influence detects; So the present invention adopts unrestrained method that the single-root carbon nano-tube bundle is connected between the source-drain electrode, constitutes the FET device of single-root carbon nano-tube bundle.Though there is randomness in unrestrained method, the shortcoming of inconvenience control, simple and efficient, can select suitable device as required flexibly, so adopt.
The absorption of molecule to be detected on SWCN in the environment can make the electric property of carbon nanotube field-effect tube device significantly change.Carbon nano tube sensor is in sensitivity; But operate under the room temperature; Have small size and all significant advantage is arranged than traditional metal oxide fax sense material to adapt to aspects such as microminiaturized and integrated needs; Be used as chemical sensor and detected oxygen, ammonia, water vapor, nitrogen dioxide, thereby also by the quite sensitive biological detection instrument of hope conduct.Recently, CNT and semiconductor nanowires field effect transistor successfully are used to detect albumen, tumor markers, micromolecule and some virus.But seldom see the report that detects sugar-albumen effect with the carbon nanotube field-effect pipe.Sugar-albumen effect is the key of a series of life processes, like hemoglutination, and immune response, the embryo forms and cellular signal transduction.In addition, these biomolecule actions also relate to the process of viral disease, like cancer metastasis, and bacterium and virus infections, rheumathritis and inflammation etc.The manufacturing of sugar-albumen activity detector spare helps development more general, biology sensor efficiently and application and development in fields such as life process, medical diagnosis on disease treatment among the present invention.
Summary of the invention
The object of the present invention is to provide a kind of with the biological detection instrument of carbon nanotube field-effect transistor as sensitivity; Detect the manufacturing approach of the detection means of sugar-protein-specific recognition reaction; Also can select the different sugar molecular modification to detect not isoacceptor, thereby constitute a kind of general, sensitive biological detector.
For realizing above-mentioned purpose, the present invention adopts following technical scheme, and concrete steps are following:
1) SWCN is carried out purification process, and with 1, the 2-ethylene dichloride disperses, and processes the CNT extremely dilute solution of stable dispersion;
2) contain on the surface and adopt photoetching technique to produce interdigital electrode on the silicon chip of insulation course, as source, the drain electrode of FET device to pattern;
3) scattered carbon nano-tube solution is dropped in the interdigital electrode processed through step 2 to the surface, CNT (bundle) is being built after the solvent evaporates between source-drain electrode;
4) apply+grid voltage of 10V, apply big Dc bias simultaneously, ablate metals property CNT keeps semiconductive carbon nano tube, obtains the FET device based on CNT (bundle);
5) select well behaved device and under room temperature, be statically placed in the glycosyl amphipathic compound octadecyl sugar amide aqueous solution and soak, flushing dries up, and obtains non-covalent glycosylated carbon nanotube field-effect transistor device;
6) glycosylated device immerses agglutinin/PBS (PBS) cultivation, makes the carbon nanotube field-effect transistor biological detector that can detect sugar-agglutinin specific recognition.
Described CNT purification process is meant; With CNT in 1: 30 ratio little shape refluxed 12 hours of boiling in the hydrochloric acid of 6M; Heated 1 hour in 350 ℃ of following air in tubular furnace dry back; Soaked 24 hours in the ultrasonic again hydrochloric acid that is scattered in 8M, 420 ℃ of heating 30 minutes down in tubular furnace are again removed impurity such as graphite scrap, agraphitic carbon particle and metallic catalyst effectively after the collection in roasting and dissolving with hydrochloric acid; Improve the purity of CNT, make it easy to dissolving and disperse and electricity performance measurement; The purifying carbon nano-tube powder of drying is placed 1, is to disperse 10 minutes under the ultrasound wave of 40KHz in frequency in the 2-ethylene dichloride, makes the CNT extremely dilute solution of stable dispersion.
Described method for making its electrode is meant; Containing the heavily doped silicon chip surface of p type of 200nm thick silicon dioxide insulation course, preparing interdigitation source, drain electrode by the ultraviolet photolithographic and (lift-off) technology of peeling off, electrode pair length is 5 μ m; Width is between 2-4 μ m, and electrode separation is between 2-4 μ m; Electrode material is a kind of among Au, Pt, Al, the Cu.
Described metallic carbon nanotubes ablation way is meant with the silicon substrate to be back of the body grid; Apply+grid voltage of 10V, make the carrier depletion of semiconductive SWNTs be in cut-off state, on source-drain electrode, apply bigger Dc bias simultaneously; Electric current is nearly all passed through from metallic SWNTs; Metallic SWNTs is blown, and the SWNTs of semiconductive carries over as conducting channel, thereby constitute the carbon nanotube field-effect tube device.
Described glycosyl amphipathic compound octadecyl sugar acid amides is reacted under 60 ℃ in dimethyl sulfoxide (DMSO) by octadecylamine and saccharic acid lactone and made in 2 days; Glycan molecule is a kind of in glucose, maltose, mannose, lactose, the galactose.
Described glycosylation is meant, with soaked overnight in the octadecyl sugar amide solution that is statically placed in 0.5wt% under the carbon nanotube field-effect transistor device room temperature, makes octadecyl sugar acid amides through long alkyl chain (C
18Aliphatic chain) and the hydrophobic effect of carbon nano tube surface be adsorbed on the carbon tube-surface, and the saccharide residue of cluster trends towards stretching in the solution, makes carbon nano tube surface accomplish non-covalent glycosylation, is convenient to the specific recognition of sugar and agglutinin; Clean device repeatedly with deionized water, to remove carbon nano tube surface and the unnecessary sugared acid amides of octadecyl of silicon chip surface on every side.
Described sugar-agglutinin identifying is meant; Glycosylated device immersed under uniform temperature, to leave standstill in certain density agglutinin/PBS (PBS) cultivated 1 hour; Take out, wash repeatedly with the agglutinin molecule of removal non-specific adsorption and with N with deionized water
2Air-blowing is done; Agglutinin is a kind of in companion canavaline (ConA), mannose binding lectin (MBP), the gala agglutinin.
Principle of work of the present invention is: adopt extremely rare SWNT/1; The 2-dichloroethane solution can make SWNT 1, and stable dispersion becomes tiny tube bank in the 2-ethylene dichloride; Be convenient to the tiny tube bank of single S WNT and build between source-drain electrode, make in subsequent treatment, being blown easily of metallicity SWNT.1, the volatility of 2-ethylene dichloride own is extremely strong, can in electrode, not introduce impurity, has guaranteed the purity of SWNT.With simple glycosyl compound octadecyl sugar acid amides non-covalent modification SWNT tube bank; Make CNT become the multivalence array platform of glucide through physisorption; The structure and the electric property that have kept SWNT; The high-hydrophilic that dense saccharide residue has carbon nano tube surface has reduced the non-specific adsorption of protein molecular, thereby has guaranteed that carbohydrate ligands combines with specificity between the acceptor.With the biological detection instrument of carbon nanotube field-effect transistor, detected the specificity cohesive process of sugar and agglutinin effectively as sensitivity.
Advantage of the present invention and effect are: the CNT glycosylation is simply quick in the method for the present invention; Simplified the synthetic process of carbohydrate ligands compound; Make CNT become the multivalence array platform of glucide through physisorption; Guaranteed that carbohydrate ligands combines with specificity between the acceptor, and kept the inherent structure of nanotube and good electric property effectively, the high-hydrophilic that dense saccharide residue has carbon nano tube surface has reduced the non-specific adsorption of other protein moleculars.Based on the biological detector of carbon nanotube field-effect transistor, detected the specificity cohesive process of sugar and agglutinin delicately.Can select to modify different glycan molecules and detect not isoacceptor, constitute a kind of general, sensitive, biological detector efficiently.
Description of drawings
Fig. 1 is the structural representation of carbon nanotube field-effect transistor device of the present invention.
Fig. 2 is the photo in kind of carbon nanotube field-effect transistor device of the present invention.
Wherein: a is the right microphotograph of source-drain electrode of the carbon nanotube field-effect transistor device of preparation; B is scanning electron microscope (SEM) photo of having built the carbon nanotube field-effect transistor device of a little SWNTs tube bank between the source-drain electrode.
Fig. 3 is the synoptic diagram of the SWNTs surface specific adsorption process of companion canavaline ConA after glycosylation modified.
Fig. 4 is the transfer characteristic curve in carbon nanotube field-effect transistor device initial performance and each modification stage.Wherein illustration is atomic force microscope (AFM) photo that has adsorbed ConA glycosylation SWNTs afterwards.
Embodiment
Embodiment 1: present embodiment adopts unrestrained method to make up carbon nanotube field-effect transistor fast, carries out non-covalent glycosylation modifiedly, and detects the specific recognition effect of sugar-Con A.At first SWCN is carried out purification process; With CNT in 1: 30 ratio slight boiling condition refluxed 12 hours in the hydrochloric acid of 6M; Filter membrane with 0.8 μ m aperture carries out suction filtration, and dry back is heating 1 hour in 350 ℃ of following air in tubular furnace, soaks 24 hours in the ultrasonic again hydrochloric acid that is scattered in 8M after the grinding; In tubular furnace, heated 30 minutes under 420 ℃ again after the collection; Impurity such as graphite scrap, agraphitic carbon particle and metallic catalyst are removed in roasting and dissolving with hydrochloric acid effectively, improved the purity of CNT, its convenient dissolving is disperseed and electricity performance measurement.The purifying carbon nano-tube powder of drying is placed 1, is under the ultrasound wave of 40KHz ultrasonic 1 hour in frequency in the 2-ethylene dichloride, makes the CNT extremely dilute solution of stable dispersion.
Contain on the surface and adopt photoetching technique to produce the Au interdigital electrode on the p type silicon chip of 200nm thick silicon dioxide insulation course, the long 5 μ m of electrode pair, wide 3 μ m, electrode separation 3 μ m pattern.Fig. 1 is the structural representation of carbon nanotube field-effect transistor device, and Fig. 2 a is the right microphotograph of source-drain electrode of the carbon nanotube field-effect transistor device of preparation.Get scattered CNT extremely dilute solution 2 μ L with micropipettor and drop in interdigital electrode the surface; After treating solvent evaporates; Being chosen in the device (Fig. 2 b) of having built CNT (or tiny bundle) between the source-drain electrode by scanning electron microscope sem, is back of the body grid with the silicon substrate, applies+grid voltage of 10V; Employing applies big method of current and blows metallicity SWNT, obtains the FET device based on CNT (bundle).Under the room temperature device is statically placed in soaked overnight in glycosyl amphipathic compound octadecyl maltose acid amides (NOMA) WS (0.5wt%); Make the physisorption of octadecyl maltose acid amides to carbon nano tube surface; Take out; Deionized water washes repeatedly, to remove carbon nano tube surface and the unnecessary octadecyl maltose acid amides of silicon chip surface on every side.N
2Air-blowing is done, and obtains non-covalent glycosylated carbon nanotube field-effect transistor device.(pH 7.06 for PBS, 0.1M, contain 0.1mM CaCl again substrate to be immersed the ConA/PBS solution of 10mL 0.1mg/mL
2, 0.1mM MnCl
2, 0.1M NaCl) in cultivated 1 hour down in 25 ℃, take out, wash repeatedly with the ConA that removes non-specific physisorption and with N with deionized water
2Air-blowing is done.Make the SWCN field effect transistor biological detector (Fig. 3, illustration among Fig. 4) that can detect sugar-agglutinin specific recognition.Fig. 4 is each modification stage, the transfer characteristic curve of carbon nanotube field-effect transistor detection means.Source-drain voltage (V
SD) when being 1V, grid voltage (V
G)-10V～+ scan between 10V.Can see that from figure before octadecyl maltose acid amides was modified, device was at certain V
SD(1V), along with V
GIncrease, output current I
SDReduce, work as V
GChannel conduction is very little during greater than 5V, and carbon nanotube field-effect transistor is turned off, and demonstrates p type FET characteristic.But after modifying octadecyl maltose acid amides, device performance significantly changes, and presents n type characteristic.This is likely because secondary amine in the octadecyl maltose amide molecule (has NH) that electron donation causes.Adsorbed after the Con A output current I that device is measured
SDThan significantly reducing before modifying, and shutoff voltage has big displacement to negative direction, show companion's canavaline Con A molecule through with the maltose residue combine successfully to be adsorbed on the biological detector after the glycosylation.
Claims (7)
1. manufacturing approach based on the biological detector of SWCN field effect transistor; It is characterized in that; Adopt photoetching technique to contain on the surface on the silicon base of silicon dioxide insulating layer and make source, the drain electrode of interdigital electrode as FET device; Carbon nanotube bundles is built between source, drain electrode as communication channel, and as grid, structure is based on the field effect transistor of SWCN with the Si substrate; To the non-covalent glycosylation bio-modification in carbon nanotube bundles surface; Obtained being used for the SWCN field effect transistor biological detector that sugar-protein-specific identification detects, selected to modify the different sugar molecule and can detect specificity combination behavior between different sugar part and acceptor respectively; This method mainly may further comprise the steps:
1) SWCN is carried out purification process, and with 1, the 2-ethylene dichloride disperses, and processes the SWCN extremely dilute solution of stable dispersion;
2) contain on the surface and adopt photoetching technique to produce interdigital electrode on the silicon base of silicon dioxide insulating layer, as source, the drain electrode of FET device to pattern;
3) with scattered SWCN drips of solution in the interdigital electrode of processing through step 2 to the surface, carbon nanotube bundles is being built after the solvent evaporates between source-drain electrode;
4) apply+grid voltage of 10V, apply big Dc bias simultaneously, the ablate metals conductive single-walled carbon nanotubes keeps semi-conductive single-walled carbon nanotubes, obtains the FET device based on carbon nanotube bundles;
5) select well behaved device and under room temperature, be statically placed in the glycosyl amphipathic compound octadecyl sugar amide aqueous solution and soak, obtain non-covalent glycosylated SWCN FET device;
6) glycosylated device immerses agglutinin/PBS (PBS) cultivation, but makes the specific SWCN field effect transistor of detection and Identification sugar-agglutinin biological detector.
2. the manufacturing approach of the biological detector based on the SWCN field effect transistor according to claim 1; It is characterized in that; Described SWCN purification process is meant; In 1: 30 ratio slight boiling condition refluxed 12 hours in the hydrochloric acid of 6M, dry back is heating 1 hour in 350 ℃ of following air in tubular furnace with SWCN, soaks 24 hours in the ultrasonic again hydrochloric acid that is scattered in 8M; In tubular furnace, heated 30 minutes under 420 ℃ again after the collection; Graphite scrap, agraphitic carbon particle and metallic catalyst impurity are removed in roasting and dissolving with hydrochloric acid effectively, improved the purity of SWCN, make it easy to dissolving and disperse and electricity performance measurement; The purifying SWCN powder of drying is placed 1, is to disperse 10 minutes under the ultrasound wave of 40KHz in frequency in the 2-ethylene dichloride, makes the SWCN extremely dilute solution of stable dispersion.
3. the manufacturing approach of the biological detector based on the SWCN field effect transistor according to claim 1; It is characterized in that described method for making its electrode is meant, is containing the heavily doped silicon chip surface of p type of 200nm thick silicon dioxide insulation course; Prepare interdigitation source, drain electrode by the ultraviolet photolithographic and (lift-off) technology of peeling off; Electrode pair length is 5 μ m, and width is between 2-4 μ m, and electrode separation is between 2-4 μ m; Electrode material is a kind of among Au, Pt, Al, the Cu.
4. the manufacturing approach of a kind of biological detector based on the SWCN field effect transistor according to claim 1 is characterized in that, described metallic single-wall carbon nano-tube ablation way is meant with the silicon base to be back of the body grid; Apply+grid voltage of 10V, make semi-conductive single-walled carbon nanotubes, i.e. SWNTs; Carrier depletion be in cut-off state; Simultaneously on source, drain electrode, apply bigger Dc bias, electric current is nearly all passed through from metallic SWCN, metallic SWCN is blown; And the SWCN of semiconductive carries over as conducting channel, thereby constitutes the SWCN FET device.
5. the manufacturing approach of the biological detector based on the SWCN field effect transistor according to claim 1; It is characterized in that described glycosyl amphipathic compound octadecyl sugar acid amides is reacted under 60 ℃ in dimethyl sulfoxide (DMSO) by octadecylamine and saccharic acid lactone and made in 2 days; Glycan molecule is a kind of in glucose, maltose, mannose, lactose, the galactose.
6. the manufacturing approach of the biological detector based on the SWCN field effect transistor according to claim 1; It is characterized in that; Described glycosylation is meant; With soaked overnight in the octadecyl sugar amide aqueous solution that is statically placed in 0.5wt% under the SWCN FET device room temperature, make octadecyl sugar acid amides pass through C
18The hydrophobic effect on alkyl fatty long-chain and SWCN surface is adsorbed on the SWCN surface, and the saccharide residue of cluster trends towards stretching in the solution, makes the SWCN surface accomplish non-covalent glycosylation, is convenient to the specific recognition of sugar and agglutinin; Clean device repeatedly with deionized water, to remove SWCN surface and the unnecessary octadecyl sugar acid amides in silicon base surface on every side.
7. the manufacturing approach of the biological detector based on the SWCN field effect transistor according to claim 1; It is characterized in that; Described sugar-agglutinin identifying is meant; Glycosylated device immersed under uniform temperature, to leave standstill in certain density agglutinin/PBS solution cultivated 1 hour, take out, wash repeatedly with the agglutinin molecule of removing non-specific adsorption and with N with deionized water
2Air-blowing is done; Agglutinin is a kind of in companion canavaline (Con A), mannose binding lectin (MBP), the Galectins.
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| CN104931560A (en) * | 2015-07-17 | 2015-09-23 | 王天星 | Biosensor and preparation method and application thereof |
| CN105336792B (en) * | 2015-11-02 | 2019-03-01 | 京东方科技集团股份有限公司 | Carbon nanotube semiconductor devices and preparation method thereof |
| KR101706732B1 (en) * | 2015-12-30 | 2017-02-27 | 주식회사 엔디디 | Bio-sensing device |
| US20190128829A1 (en) * | 2017-10-10 | 2019-05-02 | Thermo Electron Scientific Instruments Llc | Carbon Nanotube-Based Device for Sensing Molecular Interaction |
| CN110844900B (en) * | 2019-11-11 | 2022-05-24 | 天津大学 | Method for preparing carbon nano tube by taking waste tire as raw material |
| CN113851536A (en) * | 2020-06-28 | 2021-12-28 | 华为技术有限公司 | Field effect transistor, preparation method thereof and semiconductor structure |
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