CN205898686U - A molecular vehicle for unimolecule detects - Google Patents
A molecular vehicle for unimolecule detects Download PDFInfo
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- CN205898686U CN205898686U CN201620689637.0U CN201620689637U CN205898686U CN 205898686 U CN205898686 U CN 205898686U CN 201620689637 U CN201620689637 U CN 201620689637U CN 205898686 U CN205898686 U CN 205898686U
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Abstract
The utility model relates to a molecular vehicle for unimolecule detects, its include a base plate and set up in the metal level of substrate surface, wherein, the base plate includes a basement and a plurality of the setting in the arch of the patterning of this substrate surface, the arch of patterning includes that a plurality of sand grip cross arrangements form network structure to define a plurality of holes, the metal level set up in the bellied surface of patterning. The utility model discloses a molecular vehicle has following beneficial effect: the metal level sets up on the bellied surface of patterning, and the arch of patterning includes that a plurality of sand grip cross arrangements form network structure, and consequently, under of the arousing of external incident light electromagnetic field, metal surface plasma takes place resonance absorption, and the sand grip of cross arrangement plays surface enhanced raman scattering's effect, can improve SERS enhancement factor, reinforcing raman scattering.
Description
Technical field
This utility model is related to a kind of molecular vehicle for Single Molecule Detection, its preparation method and using the inspection of this carrier
Survey monomolecular method.
Background technology
Single Molecule Detection (single molecule detection, smd) technology is different from general conventional sense skill
Art, observe is the individual behavior of individual molecule, and molecule detection is in Environmental security, biotechnology, sensor, food
The fields such as safety are widely used.Single Molecule Detection reaches the limit of molecular detection, is the target that people pursue for a long time.With biography
The analysis method of system is compared, and Single Molecule Detection method research system is in the individual behavior under nonequilibrium condition, or under poised state
Fluctuation behavior, therefore be particularly suitable for research chemistry and biochemical reaction kinetics, the interaction of biomolecule, structure and function
Information, major disease early diagnosiss, pathological study and high-flux medicaments sifting etc..
At present it is known that having many methods for Single Molecule Detection, and the structure of molecular vehicle is sent out to molecule detection
Exhibition and and testing result play highly important influence.In existing multiple monomolecular detection method, molecular vehicle
Collargol is coated in glass surface by structure, and Argent grain adheres to glass surface by colloid, is then stained with silver by described
The glass of grain, through ultrasonic washing, forms scattered Argent grain in glass surface, forms molecular vehicle.Then determinand is divided
Son is arranged at molecular vehicle surface, provides laser emission by Raman detection system to the determinand molecule on its molecular vehicle.
Photon in laser is collided with determinand molecule, thus changing the direction of photon, produces Raman scattering.In addition, photon with
There is energy exchange in determinand molecule, change energy and the frequency of photon, makes this photon have the structure letter of determinand molecule
Breath.Radiation signal from determinand molecule is received by sensor, forms Raman collection of illustrative plates, using computer to described determinand
Molecule is analyzed.
However, in prior art, because the surface of described glass is a smooth planar structure, the Raman scattering letter of generation
Number not strong, so that the resolution of described Single Molecule Detection is low, it is not suitable for the detection of low concentration and micro-example, thus should
It is restricted with scope.
Utility model content
In view of this, it is necessory to provide a kind of molecular vehicle that can improve Single Molecule Detection resolution.
A kind of molecular vehicle for Single Molecule Detection, its metal including a substrate and being arranged at described substrate surface
Layer；Wherein, described substrate includes a substrate and the projection of multiple patterning being arranged at this substrate surface, described patterning
Raised inclusion multiple raised lines formation arranged in a crossed manner network structure, thus define multiple holes；Described metal level is arranged at described figure
The surface of the projection of case.
As above-mentioned molecular vehicle, further, the plurality of raised line includes multiple the first raised lines extending along a first direction
With the second raised line extending along second direction, and the angle of described first direction and second direction be more than or equal to 30 degree less than etc.
In 90 degree.
As above-mentioned molecular vehicle, further, the width of described raised line is 20 nanometers～150 nanometers, highly for 50 nanometers～
Spacing between 1000 nanometers, and two adjacent parallel raised lines is 10 nanometers～300 nanometers.
As above-mentioned molecular vehicle, further, the width of described raised line is 20 nanometers～50 nanometers, highly for 500 nanometers～
Spacing between 1000 nanometers, and two adjacent parallel raised lines is 10 nanometers～50 nanometers.
As above-mentioned molecular vehicle, further, described metal level is continuous layer structure, and is arranged at the plurality of raised line
In hole between surface and raised line.
As above-mentioned molecular vehicle, further, described metal level is discontinuous layer structure, and is only arranged at described raised line
Side wall and adjacent raised line between substrate surface.
As above-mentioned molecular vehicle, further, the material of described metal level is one of gold, silver, platinum, copper, ferrum and aluminum
Or it is multiple.
As above-mentioned molecular vehicle, further include that a composite structure of carbon nano tube is arranged at the top of the projection of described patterning
Between face and this metal level, and described composite structure of carbon nano tube is identical with the pattern of the projection of described patterning.
As above-mentioned molecular vehicle, further, described composite structure of carbon nano tube includes a carbon nano tube structure and a bag
It is overlying on the preformed layer on this carbon nano tube structure surface, and this carbon nano tube structure includes multiple CNTs arranged in a crossed manner.
As above-mentioned molecular vehicle, further, described carbon nano tube structure includes two stackings and carbon nanometer arranged in a crossed manner
Periosteum, the CNT in described carbon nano-tube film is joined end to end by Van der Waals force and arranges in the same direction.
As above-mentioned molecular vehicle, further, the material of described preformed layer be metal, metal-oxide, metal sulfide, non-
One or more in metal-oxide, non-metallic carbide and non-metal nitride etc..
Compared to prior art, molecular vehicle of the present utility model has the advantages that metal level is arranged on pattern
The surface of the projection changed, and the projection patterning includes multiple raised lines formation arranged in a crossed manner network structure, therefore, extraneous incident
Under the exciting in photoelectricity magnetic field, there is resonance absorption in metal surface plasma body, and raised line arranged in a crossed manner plays surface enhanced and draws
The effect of graceful scattering, can improve sers (surface enhanced raman scattering) enhancer, strengthen Raman and dissipate
Penetrate.
Brief description
The structural representation of the molecular vehicle that Fig. 1 provides for this utility model first embodiment.
The sectional view in the molecular vehicle edge-direction that Fig. 2 provides for this utility model first embodiment.
The stereoscan photograph of the substrate surface of the molecular vehicle that Fig. 3 provides for this utility model first embodiment.
Fig. 4 is the partial enlarged drawing of the stereoscan photograph of Fig. 3.
The preparation method flow chart of the molecular vehicle that Fig. 5 provides for this utility model first embodiment.
The sectional view of the vi-vi along the line of the composite structure of carbon nano tube of Fig. 6 Fig. 5.
The stereoscan photograph of the CNT membrane that Fig. 7 adopts for this utility model first embodiment.
The stereoscan photograph of the carbon nano tube line of the non-twisted that Fig. 8 adopts for this utility model first embodiment.
The stereoscan photograph of the carbon nano tube line of the torsion that Fig. 9 adopts for this utility model first embodiment.
The stereoscan photograph of the composite structure of carbon nano tube that Figure 10 provides for this utility model first embodiment.
The cladding aluminium sesquioxide layer of the composite structure of carbon nano tube that Figure 11 provides for this utility model first embodiment
The stereoscan photograph of single-root carbon nano-tube.
The top surface stereoscan photograph of the molecular vehicle that Figure 12 is prepared for this utility model first embodiment.
The cross-sectional scans electromicroscopic photograph of the molecular vehicle that Figure 13 is prepared for this utility model first embodiment.
The flow chart of the monomolecular detection method that Figure 14 provides for this utility model first embodiment.
Figure 15 detects the Raman light of rhodamine molecule for the monomolecular detection method that this utility model first embodiment provides
Spectrum testing result.
The structural representation of the molecular vehicle that Figure 16 provides for this utility model second embodiment.
The preparation method flow chart of the molecular vehicle that Figure 17 provides for this utility model second embodiment.
The structural representation of the molecular vehicle that Figure 18 provides for this utility model 3rd embodiment.
Main element symbol description
Molecular vehicle 10,
Substrate 12
Substrate 120
Surface 121
The projection 122 of patterning
Hole 124
Metal level 14
Survey thing molecule 16
Raman spectrum 18
Composite structure of carbon nano tube 110
Carbon nano tube structure 112
Preformed layer 114
Specific embodiment
The utility model is described in further detail below in conjunction with the accompanying drawings and the specific embodiments.
Refer to Fig. 1 to Fig. 4, this utility model first embodiment provides a kind of molecular vehicle for Single Molecule Detection
10, the metal level 14 that described molecular vehicle 10 includes a substrate 12 and is arranged at described substrate 12 surface.Described substrate 12 wraps
Include a substrate 120 and the projection 122 of multiple patterning being arranged in this substrate 120.The projection 122 of described patterning includes
Multiple raised line formation network structure arranged in a crossed manner, thus define multiple holes 124.The infall of the plurality of raised line is integrated knot
Structure.
Described substrate 12 can be insulated substrate or semiconductor substrate.Specifically, the material of described substrate 12 can for silicon,
Silicon dioxide, silicon nitride, quartz, glass, gallium nitride, GaAs, sapphire, aluminium oxide or magnesium oxide etc..Described substrate 12
Shape does not limit, and only need to have two surfaces being oppositely arranged.In the present embodiment, described substrate 12 be shaped as a flat board
Shape.The size of described substrate 12, thickness do not limit, can according to actual Single Molecule Detection need select.In the present embodiment, described
Substrate 12 is silicon chip.
Described substrate 120 and integrative-structure or different materials multiple structure that raised line can be identical material.Institute
State raised line to be arranged at a surface of described substrate 120 or be respectively arranged at two relative surfaces of described substrate 120.This
The raised line that a utility model definition part extends along a first direction is the first raised line, and another part extends along second direction
Raised line is the second raised line.The angle of described first direction and second direction be more than 0 degree be less than or equal to 90 degree it is preferable that be more than etc.
In 30 degree.The plurality of first raised line is substantially parallel, and the plurality of second raised line is substantially parallel.Raised line base of the present utility model
This parallel feature is because the bearing of trend of CNT in the CNT mask of employing in its preparation method is substantially parallel
Feature determine.The length of each raised line does not limit, and width is 20 nanometers～150 nanometers, highly for 50 nanometers～1000 nanometers,
Parallel and adjacent to raised line between spacing be 10 nanometers～300 nanometers.Therefore, the opening size of described hole 124 is received for 10
Rice～300 nanometers, depth is 50 nanometers～1000 nanometers.Preferably, the width of each raised line is 20 nanometers～50 nanometers, highly
For 500 nanometers～1000 nanometers, spacing is 10 nanometers～50 nanometers.In the present embodiment, the plurality of first raised line is perpendicular to many
Individual second raised line.Described raised line is from described substrate 120 while extending to another side.
Described metal level 14 is arranged in the hole 124 between the plurality of raised line surface and raised line.Described metal level
14 can be continuous layer structure or discontinuous layer structure.Described metal level 14 can be tied for monolayer stratiform
Structure or multilayer laminar structure.The table of the substantially uniform substrate 120 being deposited between raised line surface and raised line of described metal level 14
Face.Form a gap (gap), the surface of metal level 14 has surface plasma body resonant vibration, thus producing herein at described hole 124
Raw Raman scattering strengthens.The thickness of described metal level 14 is 2 nanometers～200 nanometers it is preferred that the thickness of described metal level 14 is equal
One.The material of described metal level 14 does not limit, and can be the metals such as gold, silver, platinum, copper, ferrum or aluminum.It is appreciated that described metal level 14
Material be not limited to above several, under any room temperature be solid-state metal material can.In the present embodiment, described metal level
The gold that 14 is 20 nanometers for thickness.
Refer to Fig. 5 and Fig. 6, this utility model first embodiment provides a kind of side preparing above-mentioned molecular vehicle 10
Method, it comprises the following steps:
Step s10, provides a substrate 12；
Step s20, provides a composite structure of carbon nano tube 110 with multiple micropores 116, this composite structure of carbon nano tube
110 include the preformed layer 114 that a carbon nano tube structure 112 and is coated on this carbon nano tube structure 112 surface, and this carbon is received
Nanotube structures 112 include multiple CNTs arranged in a crossed manner；
Step s30, described composite structure of carbon nano tube 110 is arranged at a surface 121 of described substrate 12, so that
Surface 121 part of described substrate 12 exposes；
Step s40, with this composite structure of carbon nano tube 110 for mask dry etch described substrate 12, thus to one tool
There is the substrate 12 of the projection 122 of patterning, and the projection 122 of this patterning includes multiple raised lines arranged in a crossed manner；
Step s50, removes described composite structure of carbon nano tube 110；
Step s60, deposits a metal level 14 on the surface of the projection 122 of described patterning.
In described step s10, the material of described substrate 12 does not limit, and can be formed for the material such as silicon dioxide, silicon nitride
The metal basal board or the half of the formation of the material such as silicon, gallium nitride, GaAs that the materials such as insulated substrate, gold, aluminum, nickel, chromium, copper are formed
Conductor substrate, as long as described substrate 12 is in follow-up etching process, can be etched.The size of described substrate 12 and thickness
Can select as needed.In the present embodiment, the gallium nitride that described substrate 12 is 300 microns for a thickness.
In described step s20, described carbon nano tube structure 112 includes multiple ordered arrangement and carbon nanometer arranged in a crossed manner
Thus forming multiple micropores, described preformed layer 114 is coated on the surface of the plurality of CNT to pipe.Preferably, described preformed layer
114 whole surfaces being coated on each CNT.The plurality of CNT passes through Van der Waals force and closely connects so that being somebody's turn to do
Carbon nano tube structure 112 and composite structure of carbon nano tube 110 form a self supporting structure.So-called self supporting structure refers to this structure
Can a supporter and keep a specific membrane structure.Thus, described composite structure of carbon nano tube 110 has self-supporting
Property and can partly vacantly arrange.Described CNT is included in SWCN, double-walled carbon nano-tube and multi-walled carbon nano-tubes
One or more.Described CNT is parallel to the surface of described carbon nano tube structure 112.Described SWCN straight
Footpath be 0.5 nanometer～10 nanometers, a diameter of 1.0 nanometers～15 nanometers of double-walled carbon nano-tube, multi-walled carbon nano-tubes a diameter of
1.5 nanometers～50 nanometers.The length of described CNT is more than 50 microns.Preferably, the length of this CNT is 200 microns
～900 microns.
Described carbon nano tube structure 112 includes at least one carbon nano-tube film, at least one carbon nano tube line or a combination thereof.Described
Carbon nano-tube film includes multiple equally distributed CNTs.Multiple CNTs in this carbon nano-tube film prolong in one direction
Stretch, the plurality of CNT forms multiple carbon nano-tube bundles, and the bearing of trend of described CNT is parallel to described CNT
The surface of film.Specifically, this carbon nano-tube film may include a CNT membrane.This carbon nano tube line can be a non-twisted
Carbon nano tube line or the carbon nano tube line of torsion.When described carbon nano tube structure 112 includes multiple carbon nano tube line, the plurality of
Carbon nano tube line be parallel to each other interval and cross arrangement at an angle and form the carbon nano tube structure of a stratiform.This stratiform
Carbon nano tube structure includes multiple micropores, and this micropore is the through hole of the thickness direction of a carbon nano tube structure running through this stratiform.
The size of this micropore is 1 nanometer～0.5 micron.
Refer to Fig. 7, specifically, this CNT membrane includes carbon nano-tube bundle that is multiple continuous and aligning.Should
Multiple carbon nano-tube bundles are joined end to end by Van der Waals force.Each carbon nano-tube bundle includes multiple CNTs being parallel to each other,
The plurality of CNT being parallel to each other is combined closely by Van der Waals force.A diameter of 10 nanometers～the 200 of this carbon nano-tube bundle
Nanometer is it is preferred that 10 nanometers～100 nanometers.CNT in this CNT membrane is arranged of preferred orient in the same direction.
Described CNT membrane includes multiple micropores.This micropore is the logical of the thickness direction of a carbon nano tube structure running through this stratiform
Hole.This micropore can be hole and/or gap.When described carbon nano tube structure 112 only includes single-layer carbon nano-tube membrane, this carbon
Between adjacent CNT fragment in nanotube membrane, there is gap, wherein, the size in this gap is 1 nanometer～0.5 micron.
It is appreciated that in the carbon nano tube structure 112 being made up of multilayer carbon nanotube membrane, in two neighboring CNT membrane
The orientation of CNT has an angle α, and 0 ° of ＜ α≤90 °, so that the carbon nanometer in adjacent two layers CNT membrane
Pipe intersects and forms a network structure, and this network structure includes multiple holes, and the plurality of hole uniformly and is regularly distributed on carbon
In nano tube structure 112, wherein, this pore diameter is 1 nanometer～0.5 micron.The thickness of described CNT membrane is 0.01
Micron～100 microns.Described CNT membrane can be directly obtained by pulling a carbon nano pipe array.Described CNT
Structure of membrane and preparation method thereof refers to model and keeps filed in kind et al. on 2 9th, 2007, public on May 26th, 2010
No. cn101239712b Chinese issued patents " carbon nano-tube thin-film structure and preparation method thereof " accused, applicant: Tsing-Hua University is big
Learn, Hongfujin Precise Industry (Shenzhen) Co., Ltd..For saving space, only it is incorporated in this, but all technology of above-mentioned application disclose
Also should be regarded as a part for this utility model application technology exposure.
Refer to Fig. 8, the carbon nano tube line of this non-twisted includes multiple carbon nano tube line length directions along this non-twisted
The CNT of arrangement.Specifically, the carbon nano tube line of this non-twisted includes multiple CNT fragments, the plurality of CNT
Fragment is joined end to end by Van der Waals force, each CNT fragment include multiple be parallel to each other and pass through Van der Waals force closely tie
The CNT closing.This CNT fragment has arbitrary length, thickness, uniformity and shape.The carbon nanometer of this non-twisted
Length of pipeline does not limit, a diameter of 0.5 nanometer～100 microns.The carbon nano tube line of non-twisted is by having by CNT membrane
Machine solvent processes and obtains.Specifically, organic solvent is infiltrated the whole surface of described CNT membrane, organic molten in volatility
In the presence of the surface tension producing during agent volatilization, the multiple CNTs being parallel to each other in CNT membrane pass through model moral
Hua Li combines closely, so that CNT membrane is punctured into the carbon nano tube line of a non-twisted.This organic solvent is volatility
Organic solvent, such as ethanol, methanol, acetone, dichloroethanes or chloroform, adopt ethanol in the present embodiment.Processed by organic solvent
The carbon nano tube line of non-twisted compared with the carbon nano-tube film processing without organic solvent, specific surface area reduce, viscosity reduce.
The carbon nano tube line of described torsion is to be turned round described CNT membrane two ends in opposite direction using a mechanical force
Turn and obtain.Refer to Fig. 9, the carbon nano tube line of this torsion includes multiple arrangements of the carbon nano tube line axial screw around this torsion
CNT.Specifically, the carbon nano tube line of this torsion includes multiple CNT fragments, and the plurality of CNT fragment is passed through
Van der Waals force joins end to end, and each CNT fragment is included multiple carbon being parallel to each other and being combined closely by Van der Waals force and receives
Mitron.This CNT fragment has arbitrary length, thickness, uniformity and shape.The CNT line length of this torsion is not
Limit, a diameter of 0.5 nanometer～100 microns.Further, the CNT of this torsion can be processed using a volatile organic solvent
Line.In the presence of the surface tension producing when volatile organic solvent volatilizees, phase in the carbon nano tube line of the torsion after process
Adjacent CNT is combined closely by Van der Waals force, makes specific surface area reduction, density and the intensity of the carbon nano tube line of torsion
Increase.
Described liner structure of carbon nano tube and preparation method thereof refer to model keep kind et al. in September in 2002 application on the 16th
, in No. cn100411979c Chinese issued patents " a kind of Nanotubes and its manufacturer of August in 2008 bulletin on the 20th
Method ", applicant: Tsing-Hua University, Hongfujin Precise Industry (Shenzhen) Co., Ltd., and filed in 16 days December in 2005,
No. cn100500556c Chinese issued patents application " carbon nano-tube filament and its making side on June 17th, 2009 bulletin
Method ", applicant: Tsing-Hua University, Hongfujin Precise Industry (Shenzhen) Co., Ltd..For saving space, only it is incorporated in this, but above-mentioned
Apply for that all technology disclose the part that also should be regarded as the exposure of this utility model application technology.
In the present embodiment, the CNT membrane that described carbon nano tube structure 112 is arranged for two-layer square crossing, described carbon
Nanotube membrane directly pulls from the carbon nano pipe array having grown and obtains, the multiple carbon nanometers in this carbon nano tube structure 112
Gutron is crossed Van der Waals force and is joined end to end and arrange in the same direction.
The material of described preformed layer 114 can be the metal such as gold, nickel, titanium, ferrum, aluminum, titanium, chromium, aluminium oxide, magnesium oxide, oxidation
At least one in the metal-oxides such as zinc, hafnium oxide or metal sulfide etc..It is appreciated that the material of described preformed layer 114
Material be not limited to above-mentioned enumerate material, can also be the non-metallic carbide such as nonmetal oxide, carborundum or the nitrogen such as silicon dioxide
Non-metal nitrides such as SiClx etc., as long as can be with the surface being deposited on described carbon nano tube structure 112 of physical property, and follow-up
Etch substrate 12 during be not etched.The deposition of described physical property refers to that described preformed layer 114 is not received with described carbon
There is chemical reaction in nanotube structures 112, but combined closely with described carbon nano tube structure 112 by Van der Waals force, and invests
The surface of CNT in described carbon nano tube structure 112.The thickness of described preformed layer 114 does not limit, and can receive for 3 nanometers～50
Rice.In order to obtain the nano-wire array 105 of nano-grade size, and avoid the micropore in described carbon nano tube structure 112
Excessive is covered by described preformed layer 114, and the thickness of described preformed layer 114 is preferably 3 nanometers～20 nanometers.Described CNT
Micropore 116 aperture of composite construction 110 is less than the micropore size in described carbon nano tube structure 112.
Described composite structure of carbon nano tube 110 can be prepared by the following method: first, by described carbon nano tube structure
112 are at least partly vacantly arranged；Then, deposit preformed layer 114 on described carbon nano tube structure 112 surface.
Described carbon nano tube structure 112 has relative two surface, and described carbon nano tube structure 112 can pass through a framework
Fixing, partly vacantly arranging positioned at lower portion, so that carbon nano tube structure 112 fully exposes, it is beneficial to follow-up
Form described preformed layer 114 on two relative surfaces of carbon nano tube structure 112 simultaneously.Described framework is the structure of a hollow,
There is a through hole.The edge of described carbon nano tube structure 112 is securable in described framework, passes through described positioned at middle part
Through hole comes out and vacantly arranges.By described framework so that the edge of described carbon nano tube structure 112 can firmly be consolidated
Determine, and the carbon nano tube structure 112 remaining at lead to the hole site fully exposes.In the present embodiment, described framework is one " mouth "
The frame of font, the edge of described carbon nano tube structure 112 is fixed by described frame.It is appreciated that described CNT knot
The mode that structure 112 is vacantly arranged can also be other means, such as metallic mesh, has ring bodies of hollow structure etc., as long as
Realization makes this carbon nano tube structure 112 vacantly.Described preformed layer 114 can be deposited on by described carbon by e-beam evaporation
The surface of nano tube structure 112.It is appreciated that the method for described deposition is not limited to the above-mentioned method enumerated, it can also be magnetic control
The vapour deposition processes such as sputtering method, atomic layer deposition method, as long as it is described to ensure that described preformed layer 114 does not destroy during deposition
The form of carbon nano tube structure 112 and structure.
Because described carbon nano tube structure 112 is vacantly arranged, thus the two of described carbon nano tube structure 112 surface all quilts
Described preformed layer 114 covers.Specifically, this preformed layer 114 coats in described carbon nano tube structure 112 multiple CNTs extremely
Small part surface.Described carbon nano tube structure 112 includes multiple microcellular structures it will be understood that also can divide in described microcellular structure
It is furnished with described preformed layer 114.CNT in described carbon nano tube structure 112 is combined closely with described preformed layer 114, is formed
Holistic composite structure of carbon nano tube 110.Wherein, described carbon nano tube structure 112 plays support and makees to described preformed layer 114
With.Described composite structure of carbon nano tube 110 includes multiple micropores 116.Described micropore 116 is to run through described carbon nanotube composite structures
The dented space of the thickness direction of structure 110, this dented space can be gap or micropore.
In the present embodiment, preformed layer 114 is arranged on the surface of described carbon nano tube structure 112 by e-beam evaporation and obtains
To described composite structure of carbon nano tube 110, the material of described preformed layer 114 is aluminium oxide, and the thickness of described preformed layer 114 is 5
Nanometer.Each CNT in described carbon nano tube structure 112 is coated completely by described preformed layer 114.Referring to Figure 10, for this
The stereoscan photograph of the composite structure of carbon nano tube 110 that embodiment adopts.Refer to Figure 11, be that the carbon that the present embodiment adopts is received
The stereoscan photograph of the single-root carbon nano-tube of coated aluminum oxide layer in mitron composite construction 110.
In described step s30, described composite structure of carbon nano tube 110 can be directly arranged at the surface of described substrate 12
121.Specifically, first described framework can be transferred to together with described composite structure of carbon nano tube 110 surface of described substrate 12
121, then remove described framework.Because described composite structure of carbon nano tube 110 has multiple micropores 116, thus described substrate 12
Surface 121 part come out by the plurality of micropore 116.Described composite structure of carbon nano tube 110 and described substrate 12
Be in close contact between surface 121 and non-fully, the surface 121 of the composite structure of carbon nano tube of part 110 and described substrate 12 it
Between there may be air.
After described composite structure of carbon nano tube 110 is arranged at the surface 121 of described substrate 12, can also wrap further
Include one by solvent, described composite structure of carbon nano tube 110 to be processed, so that described composite structure of carbon nano tube 110 is attached to
The step on the surface on surface 121 of described substrate 12.When the surface Deca solvent to described composite structure of carbon nano tube 110, institute
State solvent and can infiltrate described composite structure of carbon nano tube 110, soften described composite structure of carbon nano tube 110, and described carbon is received
Air between the surface 121 of mitron composite construction 110 and described substrate 12 is discharged.After described solvent is removed, described carbon
Nanotube composite construction 110 is formed with the surface on the surface 121 of described substrate 12 and closely contacts.Described solvent can be water, have
Machine solvent etc..Described organic solvent is volatile organic solvent, such as ethanol, methanol, acetone, dichloroethanes and chloroform.This enforcement
In example, described solvent is ethanol, by by described ethanol Deca in the surface of described composite structure of carbon nano tube 110, then from
So air-dry so that described composite structure of carbon nano tube 110 adhere well to the surface 121 of described substrate 12.
In described step s40, described dry etching refers to that being passed through a gas obtains a plasma under electric field action,
This plasma can be reacted with the material that is etched and obtain volatile material, such as: inductively coupled plasma etching
(icpe), reactive ion etching (rie).In the present embodiment, etched described sudden and violent by inductively coupled plasma etching method
The surface 121 of the substrate 12 of dew.Specifically, by being passed through a gas to a plasma system, described gas can for oxygen,
Chlorine, hydrogen, chlorine, argon, carbon tetrafluoride etc..Described gas is not limited to above-mentioned enumerate gas, as long as this gas can be with substrate
12 react.Preferably, described substrate 12, wherein, institute are etched using the reactive ion etching method of chlorine and argon
The power stating plasma system is 20 watts～70 watts, and the speed that is passed through of chlorine plasma is that 10 mark condition milliliters are per minute
(standard-state cubic centimeter per minute, sccm), the speed that is passed through of argon plasma is
25sccm, the air pressure of formation is 6 handkerchiefs, and etch period is 10 seconds～60 seconds.It is exposed by reactive ion etching method etching
The part surface of substrate 12, because plasma is fully reacted with substrate 12, therefore, this process reaction time is short, and efficiency is higher.
During etching described substrate 12, described etching gas occur chemistry anti-with the part of the substrate 12 being exposed
Should, and chemical reaction does not occur with the preformed layer 114 of described composite structure of carbon nano tube 110 or occurs with preformed layer 114
The speed of chemical reaction and degree are far smaller than the chemical reaction that etching gas are occurred with substrate 12.That is, described CNT is multiple
Close the effect that structure 110 plays mask.Described etching gas be can be found in down with the material of substrate 12 and the material of preformed layer 114
Table 1.
The material with substrate for table 1 etching gas, the corresponding table of the material of preformed layer
During etching, there is not chemical reaction in etching gas and preformed layer 114 due to selecting, but and substrate
12 generation chemical reactions, thus the surface of the substrate 12 being exposed can gradually be etched, and this substrate 12 is by described CNT
The surface that composite construction 110 covers will not change.And, due to described composite structure of carbon nano tube 110 and described substrate 12
Surface combine closely, thus the figure that the surface that covered by described composite structure of carbon nano tube 110 of this substrate 12 is formed, with
The figure being formed to the forward projection of described substrate 12 when described composite structure of carbon nano tube 110 is hanging is consistent.I.e. last
The global pattern of projection 122 of the patterning arriving is substantially consistent with the global pattern of described composite structure of carbon nano tube 110.
In the present embodiment, when described carbon nano tube structure 112 is using the CNT membrane being intersected using multilamellar, by changing
The intersecting angle of the adjacent CNT membrane of change can obtain the projection 122 with the patterning of different pattern.When using just
To the CNT membrane intersecting as carbon nano tube structure when, the projection 122 of the described patterning obtaining include multiple along two
The raised line of individual vertical direction cross arrangement.
The raised line of the projection 122 of described patterning is class strip or list structure.The width of described raised line be 20 nanometers～
150 nanometers.Spacing between adjacent two width on the bearing of trend of CNT is received for 10 nanometers～300
Rice.Size on the direction perpendicular to the surface of described substrate 12 for the raised line of the projection 122 of described patterning is defined as raised line
Height.The height of described raised line does not limit, can be according to the time of concrete etching depending on, can be 50 nanometers～1000 nanometers.Described
It is in a network structure that multiple raised lines are mutually perpendicular to cross-distribution.Referring to Fig. 3-4, it is the projection of patterning manufactured in the present embodiment
122 surface sweeping electromicroscopic photograph.In the present embodiment, the width of described raised line is 20 nanometers～50 nanometers, and spacing is 10 nanometers～50
Nanometer, highly for 500 nanometers～1000 nanometers.
It is appreciated that due to compound after the CNT cladding preformed layer 114 in described composite structure of carbon nano tube 110
A diameter of tens nanometers of structure, spacing is tens nanometers, therefore, the raised line width of the projection 122 of the patterning preparing
Also it is tens nanometers with spacing.Therefore, the projection 122 of patterning on described substrate 12 surface and multiple hole 124 are and receive
Rice structure.And, the spacing of the spacing of adjacent raised line and adjacent holes 124 is tens nanometers, therefore, substantially increases described
The density of the nanostructured on substrate 12 surface, thus improve sers enhancer, strengthens Raman scattering.For example, when adjacent convex
The spacing of the spacing of bar and adjacent holes 124 is 20 nanometers, in 1 micron of width range, described raised line and hole 124
Quantity is 50.And in prior art, the preparation of micro structure generally adopts photoetching technique, due to being limited by rate respectively, raised
It is difficult to all control in tens nanometer range with the nanostructured yardstick of depression.
In described step s50, the described method removing composite structure of carbon nano tube 110 does not limit, and can be ultrasonic method, remove
Method, oxidizing process etc..In the present embodiment, described composite structure of carbon nano tube 110 is removed using ultrasonic method.Specifically, by band
The substrate 12 stating composite structure of carbon nano tube 110 is placed in ultrasonic several minutes in the solution of a n- methyl pyrrolidone, due to n- first
The polarity of base ketopyrrolidine is larger, thus readily can separate described composite structure of carbon nano tube 110 with substrate 12.
In described step s60, do not limit in the method for the surface deposited metal layer 14 of the projection 122 of described patterning, can
Using modes such as electron beam evaporation, ion beam sputtering, ald, magnetron sputtering, evaporation, chemical vapor depositions.Described gold
Belong to the surface that layer 14 is deposited on the substrate 12 between the surface of each raised line and adjacent raised line.The thickness of described metal level 14 is
2 nanometers～200 nanometers, the material of described metal level 14 does not limit, and can be the metals such as gold, silver, copper, ferrum or aluminum.In the present embodiment,
The vertical golden metallic film being deposited with 20 nano thickness in described substrate 12 surface, thus the projection 122 that will be patterned into all covers.Please
Refering to Figure 12, it is the top surface stereoscan photograph of molecular vehicle 10 manufactured in the present embodiment.Refer to Figure 13, be the present embodiment system
The cross-sectional scans electromicroscopic photograph of standby molecular vehicle 10.
Refer to Figure 14, this utility model first embodiment further provides for a kind of list applying described molecular vehicle 10 and divides
Sub- detection method, described detection method mainly comprises the steps that
Step (s11), provides a molecular vehicle 10, and described molecular vehicle 10 includes a substrate 12 and is arranged at described base
The metal level 14 on plate 12 surface；Described substrate 12 includes a substrate 120 and multiple patterning being arranged in this substrate 120
Raised 122；The projection 122 of described patterning includes multiple raised lines formation arranged in a crossed manner network structure, thus defining multiple holes
124；
Step (s12), described metal level 14 away from substrate 12 surface-assembled determinand molecule 16；
Step (s13), is detected to the described determinand molecule 16 being assembled on molecular vehicle 10 using detector.
In described step (s12), described metal level 14 away from the surface-assembled determinand molecule 16 of substrate 12 method
Mainly comprise the steps that
Step (s121), provides the solution of a determinand molecule, the molecular concentration of described determinand solution can be 10- 7Mmol/l～10-12Mmol/l can be prepared according to actual needs, and molecular concentration described in the present embodiment is 10-10mmol/l；
Step (s122), the described molecular vehicle 10 being formed with metal level 14 is immersed in determinand solution, soak time
Can be 2min～60min, preferably 10min, make described determinand molecule uniformly be scattered in the surface of described metal level 14；
Step (s123), described molecular vehicle 10 is taken out, and is rinsed 5～15 with water or ethanol to described molecular vehicle
Secondary, then using drying device such as hair-dryer etc., described molecular vehicle 10 is dried up, make water or the ethanol evaporation of residual, will be described
Determinand molecule 16 is assembled in the surface of metal level 14.
In described step (s13), the described molecular vehicle 10 being assembled with determinand molecule 16 is placed in detection means, profit
With detector such as Raman spectrometer, described determinand molecule is detected.
In the present embodiment, described will about 10-6Rhodamine (rhodamine 6g) solution of g/100ml drops in described molecule
Metal level 14 surface of carrier 10.Using Raman spectrum 18 irradiate described in be assembled with the molecular vehicle 10 of determinand molecule 16.Institute
The detection parameter stating Raman spectrometer is 633 nanometers of he-ne: excitation wavelength, firing time 20 seconds, and plant capacity is 9.0mw, work
The rate of doing work is 0.5mw.Figure 15 is the Raman spectrum testing result of detection rhodamine molecule.
The monomolecular detection method that this utility model provides, has the advantage that metal level 14 is arranged on the convex of patterning
Play 122 surface, and the projection 122 patterning includes multiple raised lines formation arranged in a crossed manner network structure, therefore, extraneous incident
Under the exciting in photoelectricity magnetic field, there is resonance absorption in metal surface plasma body, and raised line arranged in a crossed manner plays surface enhanced and draws
The effect of graceful scattering, can improve sers enhancer, strengthen Raman scattering.Between described sers enhancer and adjacent raised line
Spacing is related, and distance is less, and sers enhancer is bigger.Described sers enhancer theoretical value can be 105～1015, thus can
To obtain more preferable Single Molecule Detection result.The sers enhancer of molecular vehicle 10 described in the present embodiment is more than 1010.Especially
It, the spacing of the spacing of adjacent raised line and adjacent holes 124 is tens nanometers, therefore, substantially increases described substrate 12 table
The density of the nanostructured in face, further increases sers enhancer, thus strengthening Raman scattering.
Refer to Figure 16, this utility model second embodiment provides a kind of molecular vehicle 10a for Single Molecule Detection, institute
State the metal level 14 that molecular vehicle 10a includes a substrate 12 and is arranged at described substrate 12 surface.Described substrate 12 includes one
Substrate 120 and the projection 122 of multiple patterning being arranged in this substrate 120.The projection 122 of described patterning includes multiple
Raised line formation arranged in a crossed manner network structure, thus define multiple holes 124.The infall of the plurality of raised line is structure as a whole.
The knot of the molecular vehicle 10 that the molecular vehicle 10a that this utility model second embodiment provides is provided with first embodiment
Structure is essentially identical, and its difference is, described metal level 14 is discontinuous structure.Specifically, described metal level 14 is only arranged at
Substrate 120 surface between the side wall of described raised line and adjacent raised line.That is, described metal level 14 is only arranged at described hole 124
Side wall and bottom surface on.Described metal level 14 can also be only arranged on the bottom surface of described hole 124.
Refer to Figure 17, this utility model second embodiment provides a kind of method preparing above-mentioned molecular vehicle 10a, its bag
Include following steps:
Step s10a, described composite structure of carbon nano tube 110 is arranged at a surface 121 of described substrate 12, so that
Surface 121 part of described substrate 12 expose；
Step s20a, with this composite structure of carbon nano tube 110 for mask dry etch described substrate 12, thus to one tool
There is the substrate 12 of the projection 122 of patterning, and the projection 122 of this patterning includes multiple raised lines arranged in a crossed manner；
Step s30a, deposits a metal level 14 on the surface of the projection 122 of described patterning, and this metal level 14 will be described
The projection 122 of patterning and composite structure of carbon nano tube 110 all cover；
Step s40a, removes described composite structure of carbon nano tube 110.
The molecule that the preparation method of molecular vehicle 10a that this utility model second embodiment provides is provided with first embodiment
Carrier 10 preparation method essentially identical, its difference is, first deposits a metal on the surface of the projection 122 of described patterning
Layer 14, then removes described composite structure of carbon nano tube 110 again.In step s30a, this metal level 14 is partially depositing in carbon nanometer
Pipe composite construction 110 surface, another part is deposited between raised line side and the adjacent raised line on substrate 12 surface.Step s40a
In, the partial metal layers 14 being deposited on composite structure of carbon nano tube 110 surface go together with this composite structure of carbon nano tube 110
Remove, form discontinuous metal level 14 on substrate 12 surface.In the method for this utility model second embodiment, described CNT
Composite construction 110 both masks as etch substrate 12, and the mask as deposited metal layer 14, have not only saved and have been prepared into
This, and improve preparation efficiency.
This utility model second embodiment further provides for a kind of Single Molecule Detection side of the described molecular vehicle 10a of application
Method.The method and this utility model first embodiment further provide for a kind of Single Molecule Detection side applying described molecular vehicle 10
Method is essentially identical, and its difference is, the molecular vehicle of employing is different.
Refer to Figure 18, this utility model 3rd embodiment provides a kind of molecular vehicle 10a for Single Molecule Detection, institute
State molecular vehicle 10b and include a substrate 12 and the composite structure of carbon nano tube 110 being arranged at described substrate 12 surface and metal
Layer 14.Described substrate 12 includes a substrate 120 and the projection 122 of multiple patterning being arranged in this substrate 120.Described figure
The projection 122 of case includes multiple raised lines formation arranged in a crossed manner network structure, thus defining multiple holes 124.The plurality of convex
The infall of bar is structure as a whole.
The knot of the molecular vehicle 10 that the molecular vehicle 10b that during this utility model the, embodiment provides is provided with first embodiment
Structure is essentially identical, and its difference is, further includes that a composite structure of carbon nano tube 110 is arranged at the projection of described patterning
Between 122 top surface and this metal level 14.Projection 122 and composite structure of carbon nano tube that this is patterned by described metal level 14
110 all cover.
This utility model 3rd embodiment further provides for a kind of method preparing above-mentioned molecular vehicle 10b.The method with
The method preparing above-mentioned molecular vehicle 10a is essentially identical, and its difference is, need not remove the step of composite structure of carbon nano tube 110
Rapid s40a.
This utility model 3rd embodiment further provides for a kind of Single Molecule Detection side of the described molecular vehicle 10b of application
Method.The method and this utility model first embodiment further provide for a kind of Single Molecule Detection side applying described molecular vehicle 10
Method is essentially identical, and its difference is, the molecular vehicle of employing is different.
Molecular vehicle 10b in this utility model 3rd embodiment has the advantages that firstly, since described carbon is received
Mitron composite construction 110 is arranged at the top surface of the projection 122 of described patterning, therefore, this composite structure of carbon nano tube 110 and institute
The projection 122 stating patterning forms two layer pattern identical nanostructureds respectively.And, described composite structure of carbon nano tube 110
In CNT can increase described patterning the top surface of projection 122 irregularity degree, thus further improve sers increase
The strong factor, strengthens Raman scattering.Secondly as described composite structure of carbon nano tube 110 is retained in the projection 122 of described patterning
Top surface, therefore, decrease the step removing described composite structure of carbon nano tube 110 in preparation technology, both Simplified flowsheet, reduce
Cost, decreases again and removes the pollution that described composite structure of carbon nano tube 110 brings to substrate 12.
In addition, those skilled in the art can also do other changes in this utility model spirit, these are according to this practicality
The change that new spirit is done, all should be included in the claimed scope of this utility model.
Claims (10)
1. a kind of molecular vehicle for Single Molecule Detection, its metal including a substrate and being arranged at described substrate surface
Layer；It is characterized in that, described substrate includes a substrate and the projection of multiple patterning being arranged at this substrate surface, described figure
The projection of case includes multiple raised lines formation arranged in a crossed manner network structure, thus defining multiple holes；Described metal level is arranged at
The surface of the projection of described patterning.
2. molecular vehicle as claimed in claim 1 is it is characterised in that the plurality of raised line includes multiple prolonging along a first direction
The first raised line of stretching and the second raised line extending along second direction, and the angle of described first direction and second direction is more than etc.
It is less than or equal to 90 degree in 30 degree.
3. molecular vehicle as claimed in claim 2 is it is characterised in that the width of described raised line is 20 nanometers～150 nanometers, high
Spend for 50 nanometers～1000 nanometers, and the spacing between two adjacent parallel raised lines is 10 nanometers～300 nanometers.
4. molecular vehicle as claimed in claim 3 is it is characterised in that the width of described raised line is 20 nanometers～50 nanometers, high
Spend for 500 nanometers～1000 nanometers, and the spacing between two adjacent parallel raised lines is 10 nanometers～50 nanometers.
5. molecular vehicle as claimed in claim 1 it is characterised in that described metal level be continuous layer structure, and arrange
In the hole between the plurality of raised line surface and raised line.
6. molecular vehicle as claimed in claim 1 is it is characterised in that described metal level is discontinuous layer structure, and only
It is arranged at the substrate surface between the side wall of described raised line and adjacent raised line.
7. molecular vehicle as claimed in claim 1 it is characterised in that described metal level material be gold, silver, platinum, copper, ferrum with
One or more of and aluminum.
8. molecular vehicle as claimed in claim 1 is it is characterised in that further include that a composite structure of carbon nano tube is arranged at
Between the top surface of the projection of described patterning and this metal level, and the projection of described composite structure of carbon nano tube and described patterning
Pattern identical.
9. molecular vehicle as claimed in claim 8 is it is characterised in that described composite structure of carbon nano tube includes a CNT
Structure and one is coated on the preformed layer on this carbon nano tube structure surface, and this carbon nano tube structure include multiple arranged in a crossed manner
CNT.
10. molecular vehicle as claimed in claim 9 is it is characterised in that described carbon nano tube structure includes two stackings and hands over
The carbon nano-tube film of fork setting, the CNT in described carbon nano-tube film is joined end to end by Van der Waals force and in the same direction
Arrangement；The material of described preformed layer be metal, metal-oxide, metal sulfide, nonmetal oxide, non-metallic carbide with
And one or more in non-metal nitride etc..
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