CN1434461A - Method for preparing probe tip of nano tube - Google Patents
Method for preparing probe tip of nano tube Download PDFInfo
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- CN1434461A CN1434461A CN 03112968 CN03112968A CN1434461A CN 1434461 A CN1434461 A CN 1434461A CN 03112968 CN03112968 CN 03112968 CN 03112968 A CN03112968 A CN 03112968A CN 1434461 A CN1434461 A CN 1434461A
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Abstract
The invention is a method for manufacturing nano tube probe tip; the pin applies to various mode of atom microscope. At first, the method decorates hydrophobe single layer film on the surface of various silicon probe pin, then it uses electrical field to eliminate the film or oxides the film into hydrophile film, it calculates the size of the activated area through the action that the pin acts on the standard sample surface, then it fixed catalyst particles in the hydrophile area on the surface of the pin, finally, puts the pin which carries catalyst nano particles in the nano reactor and forms into nano tube.
Description
One, technical field
What the present invention relates to is a kind of method for preparing the nanotube probe needle point, belongs to the technical field that nano-device is made.
Two, background technology
Atomic force microscope energy high resolving power is surveyed the shape of atom and molecule, determine electricity, magnetic and the mechanical property of body surface, becoming and carrying out the conventional instrument that microstructure detects, nanoscale is processed in the fields such as physics, chemistry, biology, microelectronics and material science.Probe tip is a key component of atomic force microscope, and it directly determines microscopical resolution, influences microscopical various uses.Scan-probe is normally prepared by manufacturing procedures such as sputtering sedimentation, etchings by semiconductor material, and used semiconductor material comprises silicon nitride, the various monocrystalline silicon etc. that mixes.Probe is made up of micro-cantilever and needle point, divides bar shaped cantilevered, " V " shape cantilevered etc.With the needle point that the semi-conductor industry method processes, except that out-of-shape, its radius is generally in a few nanometer to tens nanometer range.So use different needle points, resulting result is difficult to directly make comparisons.Solution is normally measured shape, the size of used needle point earlier with Electronic Speculum, perhaps extrapolate by the scanning standard sample, and then remove the influence of needle point from experimental result, and these methods are not only loaded down with trivial details, and the utmost point is ineffective.Therefore it is all most important to the repeatability of the explanation of measurement result and experiment to prepare the single probe tip of shape, size.What is more important, radius can further improve the resolution of scanning probe microscopy less than the needle point of 1～2 nanometer, detects meticulousr structure of material and character, can widen range of application widely for scanning probe microscopy.
CNT is a kind of novel nano-material of special construction.The diameter of multiple wall and Single Walled Carbon Nanotube (MWNT and SWNT) is respectively～10 and～1 nanometer range.They not only have very high aspect ratio (10
2～10
4), and have very big yang type modulus (～1TPa), and be electric conductor.The ideal that these character make CNT become atomic-force microscope needle-tip prepares material.Nanotube successfully has been used for preparing the probe tip of atomic force microscope, and has proved that the nanotube needle point has bigger superiority than traditional silicon and silicon nitride needle point really in scanning imagery and manipulation.Up to now, mainly contain two kinds of methods and prepare the CNT probe tip: mechanical means and growth in situ method.Typical patent has: United States Patent (USP) " 5307693,5703979,5756887,5824470,6159742,6346189,6457350 " etc.Mechanical means is exactly by the synthetic good CNT of robotic manipulation, CNT is fixed on silicon or the silicon nitride needle point with chemical glue, the method program is simple, but operation is not easy and time-consuming, and particularly handling diameter almost is impossible at the single-wall carbon tube of～1 nanometer range.The growth in situ method is earlier catalyzer to be adsorbed on the needle point, and growth in situ on needle point goes out the carbon pipe by chemical vapor deposition or graphite arc discharge then.The advantage of this method is simple to operate, but because uncontrollable location of growing point and size, the direction of growth also at random, therefore the carbon tube needle of preparation point forms the spininess point easily, so this preparation method's efficient is very low.
Three, summary of the invention
1, technical matters
The purpose of this invention is to provide a kind of nanotube fixed point, oriented growth that makes on the needle point, reach Dan Shu, single wall is controlled, satisfy to improve the resolution of scanning probe microscopy and the method for preparing the nanotube probe needle point of carrying out application demands such as needle point heterogeneity modification.
2, technical scheme
The method for preparing the nanotube probe needle point of the present invention comprises following steps:
(1) on the surface of probe tip, modify hydrophobic monofilm,
(2) the hydrophobic monofilm of the needle point tip being located by impulse electric field dissociates or it is oxidized to hydrophilic film,
(3) detect needle point that electric field action crosses the size that is used for calculating activating area by scanning probe microscopy on the standard model surface,
(4) at the most advanced and sophisticated hydrophilic area fixed catalyst particle of locating of needle point,
(5) needle point that will be loaded with the catalyst nano particle is placed on growing nano-tube in the nanotube reactor.
Probe tip can be the needle point that silicon semiconductor material is made, and also can be through metal or nonmetal filming or silicon needle point that compound is filmed.Hydrophobic monofilm on the probe tip can be bonded in needle surface by chemical reaction, also can form by physisorption, the reagent that carries out chemical bonding comprise hydrophobic chain and an end contain can with the functional group of needle surface reaction, the chain length of hydrophobic monofilm can be from 15 carbon ranges of three carbon to two.
The impulse electric field that carries out oxidized activating is to be realized by the pulse voltage that is added between needle point and the conductive electrode.Carrying out the required impulse electric field of oxidized activating can directly operate on scanning probe microscopy, and pulse voltage is added between needle point and the conductive substrates.
Calculate the size in oxidized activating zone,, can directly detect capillary force and calculate the contact mode needle point.Calculate the size in oxidized activating zone, to the percussion mode needle point, can directly detect the size that capillary force calculates the oxidized activating zone, also can calculate the size of activating area by the variation that detects the needle point resonance amplitude that causes by capillary force or resonant frequency.The diameter in oxidized activating zone in 2.0 nanometers to 100 nanometer range.
The method of the hydrophilic area fixed catalyst particle at the most advanced and sophisticated place of needle point is to make the hydrophilic area of needle surface adsorb the suspension that can form the solution of catalyzer or contain the catalyst nano particle, forms catalyst granules and be fixed on the most advanced and sophisticated place of needle point behind high temperature.
The solution that can form catalyzer comprises ferric nitrate, iron sulfate, and ferric chloride in aqueous solution or its mixed solution, or ferric nitrate, the liquid that iron sulfate, iron chloride form in hydrophilic solvent is as ethanol etc.The catalyst nano particle comprises ferric oxide particle and iron nano-particle, and the nano particle of iron, molybdenum, cobalt, nickel, ruthenium, zinc etc. and oxide thereof.The solution of catalyzer comprises the compound water solution of iron, molybdenum, cobalt, nickel, ruthenium, zinc.Nanotube on the needle point comprises CNT, multiple wall and Single Walled Carbon Nanotube, nano-tube, gold nanotubes, nitride nanowires and carbide nanometer line.The method of growing nano-tube comprises chemical gaseous phase depositing process on needle point, arc discharge and laser evaporation method.
Preparation process 1 of the present invention (on the surface of probe tip, modifying hydrophobic monofilm), to all kinds silicon probe tip, adopt classic method at the hydrophobic monofilm of its surperficial covalent bonding, can use various hydrocarbyl si lanes reagent, from several carbon chain length to tens carbon chain length, the reactive group of participating in bonding can be silicon chlorine or silica isoreactivity functional group.Also can be earlier on the silicon needle point coating by vaporization one deck gold film, with assembling the single layer of hydrophobic film on the golden film with the alkane of an end band sulfydryl.Preparation process 2 of the present invention (the hydrophobic monofilm at the most advanced and sophisticated place of needle point is dissociated or it is oxidized to hydrophilic film by impulse electric field) activates into hydrophilic area with needle point top hydrophobic region by electric field.Activation can directly be operated on scanning probe microscopy, and voltage is added between needle point and the conductive substrates, also can make special device control institute's making alive and needle point and to the distance between the electrode surface.According to the characteristics of Electric Field Distribution, the most advanced part of needle point is oxidized at first.Preparation process 3 of the present invention (detecting needle point that electric field action the crosses size that is used for calculating activating area on the standard model surface by scanning probe microscopy) detects needle point that oxidized activating the crosses size that is used for calculating activating area on the standard model surface by scanning probe microscopy.Preparation process 4 of the present invention (hydrophilic area fixed catalyst particle) at the most advanced and sophisticated place of needle point, the hydrophobic region of needle surface can not the adsoption catalyst aqueous solution, very little hydrophilic area adsorbs the little amount of catalyst aqueous solution and forms drop, forms the catalyst nano particle after drying.The size of nano particle on the other hand can be by regulating the concentration control of catalyst solution on the one hand by the area control of hydrophilic region.Preparation process 5 of the present invention (needle point that will be loaded with the catalyst nano particle is placed on growing nano-tube in the nanotube reactor), the needle point that is loaded with the catalyst nano particle is placed in the nanotube reactor, can use conventional method growing nano-tubes such as chemical vapor deposition, arc discharge, owing to have only most advanced place that the catalyst nano particle is arranged on the needle point, grow at most advanced place so controlled nanotube effectively.As long as the control catalyst nano particle just can grow single, single-walled nanotube effectively.
3, technique effect
The present invention compares following advantage than the method for existing preparation nanotube probe needle point: owing to controlled most advanced position and the catalyst particle size that catalyzer is fixed on needle point, therefore the growth of nanotube has obtained effective control, has improved to prepare efficient single, single-walled nanotube.This method is also controlled the direction of growth of nanotube effectively simultaneously.The invention provides a kind of nanotube fixed point, oriented growth that makes on the nanotube needle point, reach Dan Shu, single wall is controlled, satisfy to improve the resolution of scanning probe microscopy and the method for preparing the nanotube probe needle point of carrying out application demands such as needle point heterogeneity modification.Not only equipment needed thereby is simple for method of the present invention, operation is convenient, and single, the Single Walled Carbon Nanotube of growing expeditiously, is applicable to suitability for industrialized production.
The invention will be further described below in conjunction with accompanying drawing.
Four, description of drawings
Fig. 1 is the synoptic diagram that probe tip is carried out chemical modification.Needle point tip 3, needle point tip end surface 4, chemical modification process 5, single layer of hydrophobic film 6 that cantilever 1, needle point 2, amplification are wherein arranged.
Fig. 2 is that the needle point after adopting the electric field method with chemical modification carries out oxidation, fixed catalyst nano particle, the synoptic diagram of regrowth nanotube.The nanotube 18 that power supply 7, electrode 8, electric field 9, oxidizing process 10, hydrophilic film 11, adsorptive liquid process 12, catalyzer drop 13 are wherein arranged, contains nano particle drop 14, grows on the high temperature drying process 15, catalyst nano particle 16, preparation nanotube process 17, needle point.
Five, embodiment
The method for preparing the nanotube probe needle point of the present invention, comprise following steps: (1) modifies hydrophobic monofilm on the surface of probe tip, (2) the hydrophobic monofilm of the needle point tip being located by impulse electric field is removed or it is oxidized to hydrophilic film, (3) detect needle point that electric field action crosses the size that is used for calculating activating area by scanning probe microscopy on the standard model surface, (4) the hydrophilic area adsoption catalyst drop at the most advanced and sophisticated place of needle point fixes catalyst granules, and the needle point that (5) will be loaded with the catalyst nano particle is placed on growing nano-tube in the nanotube reactor.
Probe tip can be the needle point that silicon semiconductor material is made, and also can be through metal or nonmetal filming or silicon needle point that compound is filmed.
Hydrophobic monofilm on the probe tip can be bonded in needle surface by chemical reaction, also can form by physisorption, the reagent that carries out chemical bonding comprise hydrophobic chain and an end contain can with the functional group of needle surface reaction, the chain length of hydrophobic monofilm can be from 15 carbon ranges of three carbon to two.
The impulse electric field that carries out oxidized activating is to be realized by the pulse voltage that is added between needle point and the conductive electrode, carries out oxidized activating and also can directly operate on scanning probe microscopy, and pulse voltage is added between needle point and the conductive substrates.
Calculate the size in oxidized activating zone,, can directly detect capillary force and calculate the contact mode needle point; To the percussion mode needle point, can directly detect the size that capillary force calculates the oxidized activating zone, also can calculate the size of activating area by the variation that detects the needle point resonance amplitude that causes by capillary force or resonant frequency; The diameter in oxidized activating zone in 2.0 nanometers to 100 nanometer range.
Method at the most advanced and sophisticated hydrophilic area fixed catalyst particle of locating of needle point is to make the hydrophilic area of needle surface adsorb the suspension that can form the solution of catalyzer or contain the catalyst nano particle, forms catalyst granules and be fixed on the most advanced and sophisticated place of needle point behind high temperature.
The solution that can form catalyzer comprises ferric nitrate, iron sulfate, and ferric chloride in aqueous solution or its mixed solution, or ferric nitrate, the liquid that iron sulfate, iron chloride form in hydrophilic solvent is as ethanol.The catalyst nano particle comprises ferric oxide particle and iron nano-particle, and the nano particle of iron, molybdenum, cobalt, nickel, ruthenium, zinc etc. and oxide thereof, and the nano particle size is in 1 nanometer to 50 nanometer range; The solution of catalyzer also comprises the compound water solution of iron, molybdenum, cobalt, nickel, ruthenium, zinc.Nanotube on the needle point comprises CNT, multiple wall and Single Walled Carbon Nanotube, nano-tube, gold nanotubes, nitride nanowires and carbide nanometer line.The method of growing nano-tube comprises chemical gaseous phase depositing process on needle point, arc discharge and laser evaporation method.
To prepare the nanotube probe needle point be to take following scheme to realize for the position of catalyzer and grain size on the control needle point: earlier probe tip is made complete hydrophobic treatments, hydrophobic membrane with tip portion controllably activates into hydrophilic region by pulse voltage or electric field then, the size of hydrophilic region is by added impulse electric field, that is regulation voltage, needle point and to controlling the relative distance and the action time of electrode.The size of hydrophilic region can be calculated by the interaction of measuring between activation needle point and the standard model.This area size can be that several nanometers are to tens nanometers.The solution that contains catalyzer forms droplet at hydrophilic region, is condensed into nano particle after the drying, or directly the catalyst nano particle is adsorbed on hydrophilic area.At last, the needle point that is loaded with the catalyst nano particle is placed in the nanotube reactor, uses method growing nano-tubes such as chemical vapor deposition, arc discharge.
With reference to Fig. 1, probe tip is made up of cantilever 1 and needle point 2, the needle point tip 3 of enlarged diagram, and needle point tip end surface 4, after chemical modification process 5, single layer of hydrophobic film 6 is bonded in needle surface.
With reference to Fig. 2, power supply 7 is added between needle point and the electrode 8, after electric field 9 oxidizing process 10, the hydrophobic membrane at the most advanced and sophisticated place of needle point becomes hydrophilic film 11, take out liquid 12 backs of immersing catalyst solution or containing the catalyst nano particle, needle point is most advanced and sophisticated to be located adsoption catalyst drop 13 or contains nano particle drop 14, and after high temperature drying process 15, catalyst nano particle 16 has been fixed at the place at the tip.This needle point is put into the equipment 17 for preparing nanotube, the nanotube 18 of growing on the needle point.
Embodiment, the needle point hydrophobization is handled: took out after in the benzole soln of clean silicon needle point immersion 0.1% (volume ratio) octadecyl trichlorosilane 26 hours, embathe with chloroform and ethanol successively, dry up with nitrogen.The selection activation of the hydrophobic monofilm of silicon needle point: the needle point of control hydrophobic membrane and the distance between the gold thin film sample, add pulse voltage, finish activation for 100 milliseconds as 0.4 volt of effect.Fixing of catalyst granules: the needle point after will activating immerses in the iron nitrate solution of 0.5 volumetric molar concentration, takes out the back and dries 2 hours in 110 ℃ of drying boxes.Carbon nano-tube: the needle point that will be fixed with catalyzer is put into 0.5L/ minute ethylene gas of feeding in the smelting furnace, grows 30 minutes down at 750 degrees centigrade.
Claims (10)
1. method for preparing the nanotube probe needle point is characterized in that the method for preparing comprises following steps:
(1) on the surface of probe tip, modify hydrophobic monofilm,
(2) the hydrophobic monofilm of the needle point tip being located by impulse electric field is removed or it is oxidized to hydrophilic film,
(3) detect needle point that electric field action crosses the size that is used for calculating activating area by scanning probe microscopy on the standard model surface,
(4) the hydrophilic area adsoption catalyst drop at the most advanced and sophisticated place of needle point fixes catalyst granules,
(5) needle point that will be loaded with the catalyst nano particle is placed on growing nano-tube in the nanotube reactor.
2. the method for preparing the nanotube probe needle point according to claim 1 is characterized in that probe tip can be the needle point that silicon semiconductor material is made, and also can be through metal or nonmetal filming or silicon needle point that compound is filmed.
3. the method for preparing the nanotube probe needle point according to claim 1 and 2, it is characterized in that the hydrophobic monofilm on the probe tip can be bonded in needle surface by chemical reaction, also can form by physisorption, the reagent that carries out chemical bonding comprise hydrophobic chain and an end contain can with the functional group of needle surface reaction, the chain length of hydrophobic monofilm can be from 15 carbon ranges of three carbon to two.
4. the method for preparing the nanotube probe needle point according to claim 1 and 2, the impulse electric field that it is characterized in that carrying out oxidized activating is to be realized by the pulse voltage that is added between needle point and the conductive electrode, carry out oxidized activating and also can directly operate on scanning probe microscopy, pulse voltage is added between needle point and the conductive substrates.
5, the method for preparing the nanotube probe needle point according to claim 1 and 2 is characterized in that calculating the size in oxidized activating zone, to the contact mode needle point, can directly detect capillary force and calculate; To the percussion mode needle point, can directly detect the size that capillary force calculates the oxidized activating zone, also can calculate the size of activating area by the variation that detects the needle point resonance amplitude that causes by capillary force or resonant frequency; The diameter in oxidized activating zone in 2.0 nanometers to 100 nanometer range.
6, the method for preparing the nanotube probe needle point according to claim 1 and 2, it is characterized in that the method at the most advanced and sophisticated hydrophilic area fixed catalyst particle of locating of needle point is to make the hydrophilic area of needle surface adsorb the suspension that can form the solution of catalyzer or contain the catalyst nano particle, behind high temperature, form catalyst granules and be fixed on the most advanced and sophisticated place of needle point.
7, the method for preparing the nanotube probe needle point according to claim 6 is characterized in that the solution that can form catalyzer comprises ferric nitrate, iron sulfate, ferric chloride in aqueous solution or its mixed solution, or ferric nitrate, iron sulfate, the liquid that iron chloride forms in hydrophilic solvent is as ethanol.
8, the method for preparing the nanotube probe needle point according to claim 1 and 2, it is characterized in that the catalyst nano particle comprises ferric oxide particle and iron nano-particle, and the nano particle of iron, molybdenum, cobalt, nickel, ruthenium, zinc etc. and oxide thereof, the nano particle size is in 1 nanometer to 50 nanometer range; The solution of catalyzer also comprises the compound water solution of iron, molybdenum, cobalt, nickel, ruthenium, zinc.
9, the method for preparing the nanotube probe needle point according to claim 1 and 2 is characterized in that the nanotube on the needle point comprises CNT, multiple wall and Single Walled Carbon Nanotube, nano-tube, gold nanotubes, nitride nanowires and carbide nanometer line.
10, the method for preparing the nanotube probe needle point according to claim 1 and 2 is characterized in that, the method for growing nano-tube comprises chemical gaseous phase depositing process on needle point, arc discharge and laser evaporation method.
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| CN100484867C (en) * | 2004-10-22 | 2009-05-06 | 中国科学院上海应用物理研究所 | Method for separating and replacing nanometer particles |
| US7682591B2 (en) | 2006-04-10 | 2010-03-23 | International Business Machines Corporation | Embedded nanoparticle films and method for their formation in selective areas on a surface |
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| CN101819219A (en) * | 2010-04-29 | 2010-09-01 | 中国科学院上海技术物理研究所 | Method for preparing high-density super sharp silicon probe array |
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