CN104359941B - The local locating method of one-dimensional material - Google Patents
The local locating method of one-dimensional material Download PDFInfo
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- CN104359941B CN104359941B CN201410682661.7A CN201410682661A CN104359941B CN 104359941 B CN104359941 B CN 104359941B CN 201410682661 A CN201410682661 A CN 201410682661A CN 104359941 B CN104359941 B CN 104359941B
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Abstract
The invention discloses a kind of local locating method of one-dimensional material.The method is by first forming the integument formed by lapping on one-dimensional material surface so as to visible under observation condition；Local integument to be positioned on one-dimensional material is removed afterwards, so as to parcel section and the naked section corresponding to local are formed on one-dimensional material, the one-dimensional material of the parcel section is visible under observation condition, the one-dimensional material of naked section is exposed to invisible under observation condition in surrounding, sightless naked section is positioned as telltale mark using this visible parcel section, facilitate the operations such as the follow-up thermal conductivity for such as determining one-dimensional material.Compared with prior art compared with the invention provides one kind reversibly realizes one-dimensional material visible method under an optical microscope, and being operated to one-dimensional material using the method so that the practical application of one-dimensional material is more extensive.The method is simple and practical, effect is reversible, and the physical property of material itself is not interfered with after recovering original appearance.
Description
Technical field
The present invention relates to technical field of nano material, more particularly, to a kind of local locating method of one-dimensional material.
Background technology
One-dimensional material, especially monodimension nanometer material, be one kind in two geometry dimensions size it is minimum and at another
The material of macroscopic scale is closely sized to or is reached in geometry dimension.This material has special not available for some macroscopic materials
Excellent Jie see performance, excellent electric property, the calorifics better than macroscopic material, optical property such as to structure height sensitivity etc..
Therefore, this material has broad application prospects.
Yet with its minimum size, characterizing its pattern can only be shown by means of scanning electron microscope even transmitted electron
The expensive devices such as micro mirror, and complex steps, require to sample making process and properties of samples very high.Have in application or sign
The manipulation of effect is similarly very difficult.So just needing a kind of side for causing one-dimensional material visualization under an optical microscope badly
Method.Although at present the existing visualization method of some one-dimensional materials is reported, existing method complex operation and can not at present
It is inverse, it is easily caused the distinctive excellent properties of one-dimensional material forfeiture itself.
The Accurate Determining of the physical property of one-dimensional material itself is requisite for the application of this material.And it is this
The measure of the physical properties such as the calorifics of material, optics is relatively difficult always.The measurement of thermal conductivity such as in calorifics, needs to obtain
Accurate temperature of the measured matter in ad-hoc location, or the thermal power value that some section passes through.In addition, positive for cross section
Little one-dimensional material, in addition it is also necessary to which positioning precision can be accurate at least micron level, it is difficult to realize such as with traditional infrared radiation thermometer
This little detection accuracy and spatial accuracy.On the other hand, the minimum size of one-dimensional material itself causes its thermal capacity minimum.Use
During traditional contact temperature-measuring method, the temperature of material itself is also resulted in when macro-scale temperature probe contact material
Huge change is generated, the thermal conditions of one-dimensional material are had a strong impact on, the measurement of thermal property is hindered.The object of other macroscopic view
Touching one-dimensional material is also easily caused one-dimensional material and damaged, the physical property of the tested one-dimensional material of destruction occurs, and measures
Journey operation difficulty is also very big.So for the measure of one-dimensional material thermal property, to need a kind of contactless, spatial accuracy badly accurate
True method.
In addition, it is all faint that the less size of one-dimensional material also causes surveyed thermal signals, this is for measuring instrument
Requirement is higher, and the requirement of design and preparation process to measurement device is also very harsh, so if a kind of heat of material
Learn signal to show with oneself, and the alternatively this heat sensitive reaction for oneself showing of simple detection,
Can be experimentally of great advantage.
In terms of optical property measure, as the minimum size of one-dimensional material causes and light interaction zone very little, institute
It is with absorption cross-section, scattering section very little, multiple according to the optical signalling process that existing experimental facilitiess will accurately find out one-dimensional material
It is miscellaneous and equipment needed thereby is expensive.And the photic thermal phenomenon of one-dimensional material itself is spontaneous generation after a kind of material and light interaction
Response signal, and this thermal response changes with the change of light intensity and polarization, can both reduce in continuous mode for poly-
The requirement of the empirical factors such as burnt situation, light-intensity variation, moreover it is possible to reflect material itself for the different response characteristic of light.
The content of the invention
The purpose of the present invention aims to provide a kind of local locating method of one-dimensional material, and the method is by invisible one-dimensional
Material carries out wrapping up volatile substances and making which visible, and then sightless local is positioned, simple and practical and effect can
It is inverse.
To achieve these goals, according to an aspect of the invention, there is provided a kind of local positioning side of one-dimensional material
Method, for positioning to the local of one-dimensional material under an observation condition, needed for carrying out so as to the local to one-dimensional material
Subsequent operation, wherein, one-dimensional material is not certainly directly visible under observation condition；The method comprising the steps of：
An integument is formed on the surface of one-dimensional material along one-dimensional material, so that one-dimensional material and integument thereon
It is visible under observation condition on the whole；Wherein, integument is formed by the lapping that can be removed from one-dimensional material；By one-dimensional material
Need positioning local at integument remove, so as to the parcel section and naked section corresponding to local is formed on one-dimensional material,
Wherein, at parcel section, one-dimensional material keeps being wrapped layer parcel, so that parcel section is visible under observation condition；Naked
It is at dew section, invisible under observation condition during one-dimensional material is directly exposed to surrounding；Thus, it is possible to using visible bag
Wrap up in section to position sightless naked section as telltale mark.
Further, the local locating method of one-dimensional material also includes：One-dimensional material is placed on containing lapping
In the depositional environment of presoma；With adjust depositional environment parameter so that presoma physically or be chemically deposited on it is one-dimensional
The surface of material, to form integument.
Further, gaseous form of the presoma of lapping for lapping, the parameter for regulating and controlling depositional environment include
The temperature of depositional environment is reduced, so that presoma is condensed on the surface of one-dimensional material with liquid or solid-state form.
Further, lapping is the volatile material that is easily heated；The local locating method of one-dimensional material also includes：To one-dimensional
The local of the need positioning of material is heated, to remove the integument at local surfaces.
Further, lapping is the material such as ice or dry ice.
Further, depositional environment can be the solution formed by the presoma of lapping.
Further, presoma is distribution Organic substance in the solution or the ion to dissociate in the solution；Alternatively,
Ion is salt ion；Still optionally further, solution is aqueous solution.
Further, lapping is volatile material.
Further, lapping is the volatile material that is easily heated；The local locating method of one-dimensional material also includes：To one-dimensional
The local of the need positioning of material is heated, to remove the integument at local.
Further, one-dimensional material is monodimension nanometer material, and observation condition is one-dimensional material to be carried out with optical microscope
Observation.
Further, the local locating method of one-dimensional material also includes：Subsequent operation is carried out in the local to one-dimensional material
Afterwards, remove the integument of parcel section.
Further, subsequent operation includes the thermal conductivity for determining one-dimensional material.
Further, the measure of thermal conductivity includes：Heating one-dimensional material is until reach thermally-stabilised poised state；Obtain
The position at the first and second reference points and the temperature under thermally-stabilised poised state on one-dimensional material；Wherein, the first reference
Point is parcel section and the abutment points of the adjoiner of naked section；Second reference point is different from another reference of abutment points selected from naked section
Point；According to the position at the first and second reference points and temperature and based on the thermal conductivity for pre-building and the first and second reference points
The position at place and the calculated relationship of temperature are calculating to obtain thermal conductivity.
Further, heat one-dimensional material until the step of reach thermally-stabilised poised state with by the office of one-dimensional material
The step of integument at portion is removed is same step.
Further, calculated relationship is by naked section and each self-corresponding one-dimensional stable thermic vibrating screen of parcel section are carried out
Associate to set up.
Further, the differentiability of the temperature according to one-dimensional material at abutment points come associate naked section and parcel section one
Stability maintenance state thermic vibrating screen.
Further, the position of the first and second reference points and temperature are used as the one-dimensional stable thermic vibrating screen of naked section
Two boundary conditions；Two perimeter strips of the position of the first reference point and temperature as the one-dimensional stable thermic vibrating screen of parcel section
One in part.
Further, another in two boundary conditions of the one-dimensional stable thermic vibrating screen for wrapping up section is based on one-dimensional material
Material temperature at infinity for surrounding temperature setting.
Further, calculated relationship is：
Wherein,ΔTH=TH-T0,ΔTM=TM-T0,
T0For the temperature of surrounding；TMFor the temperature at first reference point；XMIt is to be chosen as sitting in the second reference point
The position of the first reference point in the case of mark origin；THFor the temperature at the second reference point；Naked section and week of the g for one-dimensional material
Heat exchange coefficient between collarette border；G ' is the heat exchange coefficient between one-dimensional material and the lapping for wrapping up which；P is one-dimensional
Material girth in the circumferential；Cross-sectional areas of the A for one-dimensional material；To be determined axial thermal conductivities of the κ for one-dimensional material.
Further, the step of wrapping up section and naked section and heating one-dimensional material are formed until making which on one-dimensional material
The step of reaching thermally-stabilised poised state includes：
Lapping is coated on one-dimensional material, wherein, lapping is the volatile material that is heated；
Irradiate wrapped one-dimensional material to heat which with first laser so that in the hot spot of the first laser
Lapping in one segment distance of place and its surrounding is volatilized out because being heated from one-dimensional material, until it reaches thermally-stabilised equilibrium-like
State；Thus, the part being exposed in surrounding because of lapping volatilization in one-dimensional material forms naked section, in one-dimensional material
The part that remain with lapping adjacent with the side of naked section forms parcel section.
Further, include the step of cladding lapping on one-dimensional material：One-dimensional material is positioned over containing easily receiving
In the surrounding of the precursor of hot volatile material, the temperature of surrounding is reduced, so that presoma condenses in one-dimensional material
Surface until parcel one-dimensional material.
Further, presoma is the gaseous form of volatile material of being easily heated；Alternatively, wrap up easily being heated for one-dimensional material
Volatile material is rendered as solid-state；Still optionally further, presoma is vapor, and the volatile material that is easily heated for wrapping up one-dimensional material is
By the ice sheet of steam coagulation.
Further, lapping is arranged to the Jacket thickness of one-dimensional material at least so that with the one-dimensional of lapping
Material is visible under an optical microscope；Preferably, the position of the first and second reference points is obtained under an optical microscope.
Further, the second reference point is the edge of the hot spot in one-dimensional material direction parcel section side of first laser.
Further, the step of obtaining the temperature at the second reference point on one-dimensional material includes：In thermally-stabilised equilibrium-like
Under state and in the case of first laser irradiation, the first Raman spectral peaks peak position at the second reference point is measured；Obtain one-dimensional material
Expect the second Raman spectral peaks peak position at a temperature of environment around；According to the first and second Raman spectral peaks peak positions, the is obtained
Temperature value of two reference points under thermally-stabilised poised state or the temperature increase relative to surrounding；Alternatively, first
It is G moulds with Raman spectral peaks peak position.
Further, the step of obtaining the second Raman spectral peaks peak position includes：By one-dimensional material from thermally-stabilised poised state
It is cooled to the temperature of surrounding；The naked section of one-dimensional material is irradiated with second laser, to obtain the second Raman spectral peaks peak position；
Wherein, power of the power of second laser less than first laser, and the power selection of second laser is not into as much as possible to one
Dimension material produces heats.
Further, volatilization transition temperature of the temperature of the first reference point for lapping.
Further, one-dimensional material is nanoscale or micron order material；Alternatively, nanoscale one-dimensional material includes nanometer
Line, nanotube, nano belt, nanofiber or nanometer rods, preferably single-root carbon nano-tube.
Using technical scheme, integument is formed on its surface along one-dimensional material by elder generation so as in observation bar
It is visible under part, the integument in the local surfaces that need to be positioned is removed afterwards, so as to parcel section and correspondence are formed on one-dimensional material
In the naked section of local such that it is able to sightless naked section is positioned by the use of visible parcel section as telltale mark.
The present invention forms heterojunction structure and thicker by volatile substances are wrapped on one-dimensional material, until size energy
Differentiated by optical microscope, and then realize the observation under optical microscope to one-dimensional material pattern.The one-dimensional material is utilized simultaneously
Pattern can be observed under an optical microscope, and then using (including but not limited to visualization) measurement of the visualization method
One-dimensional material thermal conductivity.Then the present invention is rolled into heterojunction structure, adopts afterwards by first preparing sample and obtaining physical dimension
Laser irradiation heterojunction structure (is irradiated using high power laser light, causes one-dimensional material to be heated, and then cause the volatile of its surface
Material disappears), Raman spectrum characteristic peak is obtained and temperature computation (for calculating the temperature rise of laser facula edge), melts linear measure longimetry
(length in measurement volatile substances disappearance region, for referring to standard as thermal source far point temperature), model analysiss are final to calculate
The thermal conductivity of one-dimensional material.The present invention indicates coordinate as temperature by the use of the disappearance edge of volatile substances, using hot stable state side
Journey has easily calculated the axial thermal conductivity of one-dimensional material.
Compared with prior art compared with the invention provides one kind reversibly realizes that one-dimensional material under an optical microscope may be used
The method seen, the method is simple and practical, effect is reversible, and the physical property of material itself is not interfered with after recovering original appearance.Simultaneously
The measurement of one-dimensional material thermal conductivity is carried out using this method, by contactless spectral measurement with using volatile substances melt as
Temperature refers to standard and combines so that the characteristics of the method has self-adjusting (namely by LASER HEATING much, also just melting much),
Reduce the difficulty of determination experiment.Simultaneously utilize this method, can be also used for optical property especially one-dimensional material from it is different
The sign of the interaction difference of polarization, wavelength and intensity light, using calorifics response reflection material and light interaction information, rule
The difficulty kept away in optical detection.
According to the detailed description below in conjunction with accompanying drawing to the specific embodiment of the invention, those skilled in the art will be brighter
The above-mentioned and other purposes of the present invention, advantages and features.
Description of the drawings
Describe some specific embodiments of the present invention hereinafter with reference to the accompanying drawings by way of example, and not by way of limitation in detail.
In accompanying drawing, identical reference denotes same or similar part or part.It should be appreciated by those skilled in the art that these
What accompanying drawing was not necessarily drawn to scale.In accompanying drawing：
Fig. 1 is that the structure of measure one-dimensional material tested device visualization under an optical microscope in the embodiment of the present invention is shown
It is intended to；
Fig. 2 is the optical microscope of the heterojunction structure that one-dimensional material is observed under an optical microscope in the embodiment of the present invention
Photo；
Fig. 3 is the functional module group of the one-dimensional material thermal conductivity measurement system in the embodiment of the present invention based on visualization method
Into schematic diagram；
Fig. 4 is that one-dimensional material is irradiated with a laser heating and then causes the signal that volatile substances disappear in the embodiment of the present invention
Figure；
Fig. 5 is that one-dimensional material is irradiated with a laser the optical microscope that rear volatile substances disappear and shines in the embodiment of the present invention
Piece；And
Fig. 6 be in the embodiment of the present invention one-dimensional material when being irradiated by high power laser light and substantially no heats when survey
The raman characteristic peak peak position fit-spectra figure of amount.
Specific embodiment
In the present invention, " one-dimensional material " of indication is nanoscale one-dimensional material or micron order one-dimensional material, wherein nanoscale one
Dimension material includes nano wire, nanotube, nano belt, nanofiber or nanometer rods.
In order to the one-dimensional material for solving very small dimensions at present can only be by means of scanning electron microscope when its pattern is characterized
Even the expensive device such as transmission electron microscope and complex steps, manufacturing process and properties of samples require high a series of ask
Topic, and cannot positioning to the one-dimensional material of very small dimensions, so that the problem that cannot be subsequently operated, the present invention is carried
A kind of local locating method of one-dimensional material has been supplied, for positioning to the local of one-dimensional material under an observation condition, with
Just the subsequent operation needed for carrying out to the local of one-dimensional material, one-dimensional material be not certainly directly visible under observation condition.
The local locating method includes step：An integument is formed on the surface of one-dimensional material along one-dimensional material, so that
Obtain one-dimensional material and integument thereon is visible under observation condition on the whole；Wherein, integument is by can remove from one-dimensional material
Lapping formed；The integument at local that the need of one-dimensional material are positioned is removed, so as to bag is formed on one-dimensional material
Wrap up in section and the naked section corresponding to local.Wherein, at parcel section, one-dimensional material keeps being wrapped layer parcel, so that bag
Wrap up in section visible under observation condition.At naked section, during one-dimensional material is directly exposed to surrounding under observation condition not
It can be seen that, thus, it is possible to be positioned to sightless naked section by the use of visible parcel section as telltale mark.
In one embodiment of the invention, the method for the local positioning also includes：One-dimensional material is placed on containing bag
In the depositional environment of the presoma for wrapping up in material, the parameter of depositional environment is adjusted, so that presoma physically or is chemically deposited
On the surface of one-dimensional material, to form integument.Wherein depositional environment is probably surrounding, it is also possible to be not, such as in water
Depositional packages layer in solution, removes portion envelops layer after then taking out again, and depositional environment now is exactly aqueous solution, with week
Collarette border is different.
In an exemplary embodiments of the present invention, depositional environment is the solution formed by the presoma of lapping.Its
In, presoma is distribution Organic substance in the solution or the ion to dissociate in the solution.Wherein dissociate in the solution from
Son is preferably salt ion, and solution is preferably aqueous solution.
The method of the local positioning of the present invention also includes：The local that the need of one-dimensional material are positioned is heated, to remove
Integument at local.Integument is to be deposited on one-dimensional material to be formed by lapping.It is real in another typical case of the present invention
Apply in example, the presoma of lapping is the gaseous form of lapping, will now cause lapping to be deposited on one-dimensional material
On, need to regulate and control the parameter of depositional environment.Wherein, the parameter for regulating and controlling depositional environment includes the temperature of reduction depositional environment
Degree, so that presoma is condensed on the surface of one-dimensional material with liquid or solid-state form.Lapping can be volatile material
Material, volatile material can be that volatile, or due to other ambient parameters changes of being heated cause which volatile.It is preferred that
Ground, the volatile material that is heated can be ice or dry ice.
In an exemplary embodiments of the present invention, the local locating method of one-dimensional material also includes：To one-dimensional material
Local carry out subsequent operation after, remove parcel section integument.By the integument for removing parcel section, such one-dimensional material
The integument on surface is removed completely, and whole one-dimensional material is completely exposed in surrounding, and is become under observation condition
It is invisible.One-dimensional material being wrapped up using the method for the present invention and being removed does not have any impact to the property of material itself,
Therefore the visualization method is reversible.
The subsequent operation of indication in the present invention includes the thermal conductivity for determining one-dimensional material, but is not limited thereto.Current pole
Undersized one-dimensional material needs to be accurately positioned precision in measuring thermal conductivity, is difficult to realize little chi with traditional infrared radiation thermometer
Macro-scale temperature probe contact one-dimensional material in very little detection accuracy and spatial accuracy, and traditional contact temperature-measuring method
The temperature for being easily caused material itself produces the problem of great variety, is based on the problems referred to above, present invention also offers a kind of
The assay method of the thermal conductivity of one-dimensional material.The assay method includes：On one-dimensional material formed one wrap up section and with parcel section
An adjacent naked section.Wherein, at parcel section, one-dimensional material is different from the lapping parcel of one-dimensional material；Exposed
At section, one-dimensional material is exposed in surrounding.Heating one-dimensional material is until reach thermally-stabilised poised state, acquisition is one-dimensional
The position at the first and second reference points and the temperature under thermally-stabilised poised state on material.Wherein, the first reference point is
The abutment points of the adjoiner of parcel section and naked section, the second reference point are different from another reference point of abutment points selected from naked section.
According to the position at the first and second reference points and temperature and based at the thermal conductivity for pre-building and the first and second reference points
Position and temperature calculated relationship calculating to obtain thermal conductivity.For position and the temperature selection of the first and second reference points
And can be discussed in detail behind calculated relationship.
Wherein, heat one-dimensional material until the step of reach thermally-stabilised poised state with by the local of one-dimensional material
Integument be same step the step of remove.Introduce first below how to be formed on one-dimensional material one wrap up section and with parcel
The adjacent naked section of section.
In a preferred embodiment of the invention, the step of parcel section and naked section are formed on one-dimensional material and heating
One-dimensional material is until the step of reaching thermally-stabilised poised state includes：Lapping is coated on one-dimensional material；With first
Laser irradiates wrapped one-dimensional material to heat which so that at the hot spot of first laser and its one segment distance of surrounding
Interior lapping is volatilized out because being heated from one-dimensional material, until it reaches thermally-stabilised poised state.Thus, in one-dimensional material because
Lapping volatilizees and is exposed to the part in surrounding and forms naked section, adjoins with the side of naked section in one-dimensional material
The part for remaining with lapping forms parcel section.
The invention provides one kind reversibly allows one-dimensional material visible method flow under an optical microscope, including：
1) one-dimensional material of certain configuration is placed in a kind of environment for including volatile substances precursor, herein one
Dimension material configuration is for vacantly and across slit.Specifically, configuration can be single-root carbon nano-tube growth in situ be across hundred it is micro-
The hanging single SWCN configuration of meter level insertion slit.In other unshowned embodiments, one-dimensional material configuration
Can be attached on substrate.
2) change the environmental variables such as the temperature of surrounding so that volatile substances are condensed on one-dimensional material, formed different
Matter structure and it is thicker, until within its size reaches the limit of resolution of optical microscope.As shown in Figure 2-5, reduce surrounding
106 temperature, the volatile substances precursor in surrounding are deposited on one-dimensional material 105, formation volatile substances-one-dimensional
The cable shape heterojunction structure of material, until within the size of one-dimensional material 105 reaches the limit of resolution of optical microscope, due to easy
Volatile substance and surrounding have the property of different reflections or scattered light, it is achieved thereby that right under optical microscope 101
The observation (referring to Fig. 2) of small one-dimensional material pattern.
When the supercool environment of surrounding is broken, the volatile substances for being condensed in one-dimensional material surface depart from, one-dimensional material sheet
Body recovers former pattern once again, does not affect the characteristic of one-dimensional material itself.So condense repeatedly reversibly to enter with volatilization
OK, also referred to as one-dimensional material method reversibly visualization under an optical microscope, the reversibly visualization method bag
Include but be not limited to visualization, simply can wrap up and invisible under an optical microscope.
The presoma of the above-mentioned lapping being previously mentioned is the gaseous form of volatile material of being heated.Parcel one-dimensional material
The volatile material that is heated can be rendered as solid-state.Still optionally further, presoma can be vapor, wrap up receiving for one-dimensional material
The volatile material of heat is that, by the ice sheet of steam coagulation, surrounding refers to the air ambient containing vapor.It is heated volatile
The precursor of material can also be the such as gaseous form of form of carbon dioxide, liquid form (Organic substance such as in water etc.) and free
The change of the material is produced after the ionic speciess (inorganic ion such as in water etc.) and chemical reaction that constitute which in the solution
Learn reactant.Organic substance wherein in the former vapor, carbon dioxide and water can be physically deposited due to the reduction of temperature
On one-dimensional material, Organic substance of ice, dry ice and solidification etc. is formed, then both can cause chemically because of environmental factorss change
Generate in the environment and be deposited on one-dimensional material, or ride in
Salt of precipitation etc.).
As shown in figure 3, present invention also offers using one-dimensional material side reversibly visualization under an optical microscope
Method is come the system that measures one-dimensional material thermal conductivity.The thermal conductivity measurement system includes a sample preparation module, and a physical dimension is obtained
Delivery block, a visualization or parcel one-dimensional material module, laser irradiation melt evaporation module, and a Raman spectrum characteristic peak position is obtained
Take and temperature computation module, one melts linear measure longimetry module and a computing module.
Sample preparation module, can be used to realize tested one-dimensional material is grown with certain configuration or is placed on certain substrate
On 104.It is preferred that the one-dimensional material of certain configuration is placed in using the device (commercial Linkam THMS600 thermal stations) shown in Fig. 1
Change the environmental variables such as the temperature of surrounding in including the environment of volatile substances precursor and conveniently.Can be added using micro-
One-dimensional material is placed on substrate by work mode with certain configuration, it would however also be possible to employ one-dimensional material is grown in substrate by situ synthesis
On.Specifically, the method growth CNT of chemical vapor deposition can be adopted, because growth conditionss are adapted to offline mode life
Long, carbon pipe flies up and leaps rear and receives substrate, when temperature is reduced, after carbon pipe 105 has dropped to hundred microns of insertion slits
On the reception substrate of side, the attachment of two ends carbon pipe is formed on a substrate 104 and there is the configuration of hanging section centre.
Physical dimension acquisition module, for obtaining the physical dimension of measured object, including the cross-sectional area A of measured object and transversal
Face circumferential periphery P.The substrate and various microscopes that physical dimension acquisition module can be adhered to by one-dimensional material (includes electronic display
Micro mirror and atomic force microscope etc.) realizing its measurement function.Can be using observing under transmission electron microscope or scanning electron microscope
To, or determined using modes such as AFM, STM or step instruments.For carbon nanotube-sample, it is possible to use electronic diffraction is matched somebody with somebody
Close high resolution electron microscopy directly to observe, determine the chirality of SWCN, then table look-up and obtain the cross-sectional area and girth of carbon pipe.
If the cross section of measured object is filled circles, diameter of a circle d is measured, round cross-sectional area is obtained for A=0.25 π d2, P=π
d.If the cross section of measured object is annulus, round outside diameter d and wall thickness b are measured, cross-sectional area is obtained for A=π b (d-b), P
=π d.In one particular embodiment of the present invention, measured object is SWCN, and its cross section can be understood as very thin wall
Annular, does electronic diffraction to hanging CNT by TEM, according to diffraction pattern, calculates related data, and consulting literatures can
To obtain the chirality of carbon pipe, such as the present embodiment find for (21,4), and then table look-up that can to obtain the diameter d of carbon pipe be 1.82nm,
Its wall thickness b is approximately constant 0.34nm, obtains cross-sectional area for A=0.34 π d, P=π d.
Visualization or parcel one-dimensional material into heterojunction structure module, in one-dimensional material surface attachment volatile substances,
Until degree visible under an optical microscope or that material attachment parcel situation can be characterized under an electron microscope.This module
Can realize visualization, but it is also possible to be not up to visible level, only volatile substances need to be wrapped up on surface.At one of the present invention
In specific embodiment, as shown in figure 1, sample is placed on a thermal station 102, surrounding 106 is closing and aqueous steaming
The air of gas, thermal station 102 can provide -100 DEG C of stable air environment.Thermal station temperature starts to reduce, when as little as -87 DEG C
When, the volatile substances presoma vapor in surrounding 106 reduces reaching saturation because of temperature, is rapidly condensed into ice
103, it is attached on CNT 105, forms the construction of cable, until ice sheet is thickening, being finally issued in optical microscope 101 can
Take effect fruit.
Poised state to be reached, needs the one-dimensional material to being coated with integument to heat.Evaporation is melted in laser irradiation
Module, as illustrated in figures 4-5, for irradiating heterojunction structure using high power laser light, causes one-dimensional material 105 to be heated, and then will
Heat transfer causes volatile substances 103 to disappear to surrounding volatile substances 103.In a preferred embodiment of the invention,
It is irradiated parallel to axial resistivity using the 514nm laser polarization directions projected in optical microscope 101, causes carbon to be received
Mitron 105 is heated, and then melts the ice sheet 103 of outside parcel.Laser-irradiated domain week is shown as under optical microscope 101
Enclose that CNT is invisible again, as shown in figure 5, forming the naked section 107 of one-dimensional material.
Thermally-stabilised poised state is obtained during naked section 107 is formed, or forms naked section
Continue irradiation afterwards, so as to obtain the thermally-stabilised poised state of one-dimensional material.When one-dimensional material reach thermally-stabilised poised state it is necessary to
Select the position at the first and second reference points and the temperature under thermally-stabilised poised state.When the position of the first and second reference points
When putting selection difference, calculation relational expression is also differed.In one embodiment of the invention, the position at the first and second reference points
It is by by naked section and the parcel each self-corresponding one-dimensional stable thermic vibrating screen of section to put with the calculated relationship of temperatureIt is associated to set up.Preferably, according to one-dimensional material in parcel section and naked section
The differentiability of the temperature at abutment points is associating.As the first and second reference points position and temperature as naked section a stability maintenance
Two boundary conditions of state thermic vibrating screen, the position of the first reference point and temperature are used as the one-dimensional stable thermal diffusion side for wrapping up section
One in two boundary conditions of journey.Another base in two boundary conditions of the one-dimensional stable thermic vibrating screen of parcel section
Set in the temperature that one-dimensional material temperature at infinity is surrounding.
In one particular embodiment of the present invention, volatilization transition temperature of the temperature of the first reference point for lapping.
The temperature value can pass through consulting literatures or experiment determines.Second reference point is wrapped in one-dimensional material direction for the hot spot of first laser
Wrap up in the edge of section side.
In an exemplary embodiments of the present invention, the method bag of the temperature on one-dimensional material at the second reference point is obtained
Include：In the case where thermally-stabilised poised state and first laser are irradiated, the first Raman spectral peaks at the second reference point are measured
Peak position, obtains one-dimensional material the second Raman spectral peaks peak position at ambient temperature；According to the first and second Raman spectrums
Peak-to-peak position, obtains temperature value of second reference point under thermally-stabilised poised state or the temperature increase relative to surrounding.
Certainly, the invention is not limited in by the way of Raman spectrum, it would however also be possible to employ other modes are obtaining the second reference point
Temperature value or the temperature increase relative to surrounding under thermally-stabilised poised state.Preferably, obtain the second Raman light
The step of spectral peak peak position, includes：One-dimensional material is cooled to the temperature of surrounding, Zhi Houyong first from thermally-stabilised poised state
Second laser irradiates the naked section of one-dimensional material, to obtain the second Raman spectral peaks peak position.Wherein, the power of second laser is less than
The power of first laser, and the power selection of second laser is not into as much as possible to one-dimensional material generation heats.
Specifically, obtained and temperature computation module using Raman spectrum characteristic peak position.As shown in figure 3, for obtaining Gao Gong
Exist to calculate laser spot edge with the Raman spectrum characteristic peak difference on the frequency without illuminated point during heating effect when rate laser irradiates
The lift-off value Δ T of temperature when being irradiated with a laserH.Preferably, the measurement of Raman spectrum characteristic peak should cause in high power laser
Volatile substances volatilization is carried out after reaching stable dynamic equilibrium with condensation again, and melting process and raman spectroscopy measurement process institute
Should be equally with laser power.For different one-dimensional materials, the raman characteristic peak for being detected is different.
In one particular embodiment of the present invention, the one-dimensional material for being adopted for single-root carbon nano-tube, raman characteristic peak
What is chosen is the G moulds of carbon pipe, and volatile substances are ice.Because the ice of carbon nano tube surface can stretch carbon pipe, and then can affect carbon
The G moulds of nanotube, so after high power laser light irradiates 10 minutes, surface ice sheet no longer changes, and is now continuing with Gao Gong
Rate laser irradiation collection carbon pipe G mould peak positions ωH, it is 1588.6cm in the present embodiment-1, laser is turned off, laser power is turned down, is made
Which becomes low power laser, irradiates carbon pipe Raman spectrum G mould peak positions ω that the collection of carbon pipe cools down later againL, this enforcement
It is 1589.0cm in example-1.Avoided when one-dimensional material Raman spectrum characteristic peak is gathered using low power laser heating effect as far as possible
Should exist.Collection above is all that repeatedly measurement ensures precision.Consulting literatures know single carbon pipe in T0When peak position red shift
Percentage ratio, αT0=(d ω/dT) T0/ωT0, it is α at -100 DEG C or so-100℃=8 × 10-6/ K, calculates according to formula because swashing
Light irradiation causes illuminated temperature to rise a height of Δ TH=Δ ω/αT0/ωT=(1589.0-1588.6)/(8 × 10-6)/
1588.6=32K.
After naked section 107 is formed on one-dimensional material, in addition it is also necessary to measure its length.Naked section 107 be exactly it is heated after melt
The region of change, the i.e. length of invisible area under an optical microscope.As shown in 4-5, melting linear measure longimetry module is used to obtain
Heterojunction structure after laser irradiation around invisible area 107 under the optical microscope that disappears and stay of volatile substances 103
Length, for causing temperature elevated temperature to refer to mark because of the axial heat conduction of one-dimensional material as away from illuminated laser spot
It is accurate.Measurement module can be obtained using optical microscope measuring, it is also possible to by sample on the premise of guarantee volatile substances are constant
Product are put in scanning electron microscope (SEM), more accurately measure the length of naked section 107 in the secure execution mode (sem, it might even be possible to according to
The pattern of volatile substances 103 instead releases position and the temperature of the first reference point by additive method, namely according to these to temperature
The sensitive phenomenon of degree, simulates the distribution of temperature.In the present embodiment, ice sheet thawing can be directly observed under an optical microscope
Region is the length of naked section 107, is calculated according to scale, is 4 microns, deducts laser facula about 2 micro- in the present embodiment
Rice, obtains xM=1 μm.
Computing module is for the second reference point temperature increase according to the one-dimensional material, physical dimension of one-dimensional material, different
Data that thawing length of matter structure etc. has been measured and experimental system parameter are calculating the thermal conductivity of one-dimensional material.It is based on
Theory be one-dimensional stable thermic vibrating screen and potentially include one-dimensional material each point temperature should meet can be micro- property.
As shown in figures 1 to 6, the present invention describes naked respectively with reference to two one-dimensional stable thermic vibrating screens by taking single carbon pipe as an example
Dew section 107 and parcel section 103.As shown in figure 4, because naked section 107 is right with parcel 103 sample of section in the sample of one-dimensional material
Title property, we are only taken as object of study.
For the naked section 107 of carbon pipe, according to one-dimensional stable thermic vibrating screen, on CNT, the temperature of optional position is full
Foot：
It is that carbon pipe naked section and ice are wrapped up at section boundary to take the first reference point, the position XMTemperature be TM；Take second
Reference point is T in the temperature of laser irradiation light spot edge point for carbon pipeH, the point is that the another of the first reference point is different from naked section
One reference point.This equation analytic solutions can be obtained for T (x)=ae using the two boundary conditionsmx+be-mx+T0.WhereinΔTH=TH-T0, Δ TM=TM-T0。
And for have ice parcel one section 103, equally using boundary condition：The first reference point is taken for carbon pipe naked section and ice
Position X at parcel section boundaryMThe temperature of (in this formula, zero is set to this point, namely x=0 herein) is TM.And because
The temperature of carbon pipe can be reduced to room temperature (usually more than ten micron) in smaller distance, so and having T (∞)=T0.Bag
Wrap up in section and equally meet another one-dimensional stable thermic vibrating screenAccording to two above-mentioned sides
Boundary's condition can obtain second equation analytic solutions for T (x)=Δ TMe-m'x+T0, wherein
In nature, the temperature of material the function of position should be met can micro- condition (namely approach from left and right two ends, temperature
Angle value is identical in same point, and the first derivative of temperature is identical in same point), i.e., the Temperature Distribution of same object should can be micro-
Point.Due to temperature to the function of position except be not in notch cuttype jump (the total boundary condition of both the above equation), also
Must be fulfilled for first derivative should left and right it is equal, so having
This equation is simplified, the calculated relationship of position and temperature at the first and second reference points is as follows：
Wherein,ΔTH=TH-T0,ΔTM=TM-T0。
Wherein, T0Temperature (being -100 DEG C herein) for surrounding, TMFor the temperature at the first reference point.ΔTMReally
It is fixed, can pass through to change the temperature of surrounding, up to the matter melts evaporation for causing remaining around one-dimensional material or directly
Distillation reaches critical point, so that it is determined that raise because being irradiated with a laser temperature, heat travels to material along one-dimensional material can be with
There is the critical point for melting distillation, namely the equivalent temperature of material disappearance marginal point.XMTo be located, the second reference point is being chosen as
The coordinate of the first reference point, T in the case of zeroHFor the temperature at the second reference point, g for one-dimensional material naked section with
(herein, consulting literatures are known that as g ≈ 0.1MW/ (m heat exchange coefficient between surrounding2K)), g ' is one-dimensional material
Material and wrap up the heat exchange coefficient between its lapping, herein g' represent carbon pipe and wrap up it ice between heat exchange series
(consulting literatures are known that as g' ≈ 1.6MW/ (m number2·K)).P is one-dimensional material (i.e. carbon pipe) girth in the circumferential, should
Data can be obtained by consulting literatures.Cross-sectional areas of the A for one-dimensional material, to be determined axial thermal conductivities of the κ for one-dimensional material
Rate.
Thus have found axial thermal conductivity κ to be determined of one-dimensional material therewith between pre-test value necessarily satisfying for pass
It is formula, thermal conductivity κ is lain in m.In the present embodiment, bring into data be calculated equation above normal solution be 2617W/ (m
K)。
In an exemplary embodiments of the present invention, using visualization method (it is including but not limited to visualization, can simply
Parcel and it is invisible under an optical microscope) measurement one-dimensional material thermal conductivity the step of include：
Step S101, the one-dimensional material of certain configuration is prepared on certain substrate.Wherein it is possible to use micro Process mode
One-dimensional material is placed on substrate with certain configuration, or growth in situ is on substrate.In an exemplary embodiments of the present invention
In, using chemical gaseous phase depositing process on a kind of homemade substrate growth in situ single-root carbon nano-tube, be formed with hundred microns hang
The one-dimensional material sample of empty configuration.
Step S102, the physical dimension of the one-dimensional material needed for obtaining.
Step S103, the substrate containing measured object is placed in a kind of environment for including volatile substances precursor, and
Reduce the temperature to T0So that volatile substances are condensed on one-dimensional material, cause one-dimensional material-volatile substances to form hetero-junctions
Structure and it is thicker.Specifically, sample is positioned on a thermal station, is around the air ring containing vapor of closing
Border, during thermal station temperature is reduced to -100 DEG C of setting, steam coagulation on the carbon nanotubes, forms cable knot
Structure, until ice sheet is thickening finally to reach visual effects under an optical microscope.Volatile substances are wrapped up on one-dimensional material surface, can
It is visualization to realize, but necessarily, as long as wrapping up volatile substances on surface.
Step S104, positions one-dimensional material under an optical microscope, and using high power laser light irradiation heterojunction structure, (cable is tied
Structure) central authorities, cause one-dimensional material to be heated, and then transfer heat to volatile substances around, cause volatile substances to volatilize,
Expose exposed one-dimensional material, and no longer increase until melting length stabilisation, reach thermally-stabilised poised state.
Step S105, when high power laser light irradiation is stable, one-dimensional material Raman spectral peaks peak position during collection high temperature (the
One Raman spectral peaks peak position), it is after reducing laser power until can ignore to one-dimensional material heats, one-dimensional during collection low temperature
Material Raman spectral peaks peak position (the second Raman spectral peaks peak position), and calculate the later one-dimensional material temperature rising Δ of laser irradiation
TH.For different one-dimensional materials, the raman characteristic peak for being detected is different.
Step S106, measures the length of exposed one-dimensional material out, and the edge with laser facula is calculated as zero
Go out one-dimensional material light spot edge to heterojunction structure edge apart from XM。
Step S107, according to one-dimensional material be irradiated with a laser the temperature increase of hot spot marginal position, one-dimensional material it is several
What size, thawing length of heterojunction structure etc. has measured the data that obtain and experimental system parameter to calculate one-dimensional material
Thermal conductivity.
Wherein, because substrate can affect the heat transfer of one-dimensional material and its intrinsic properties, and TEM may bring irradiation to damage
Wound etc., in order to reduce the impact of substrate and TEM, the invention provides a kind of be beneficial to TEM structural characterizations and the detection of optics calorifics
The carbon pipe of growth in situ receives the preparation method of substrate, including：
Step S201, (optics calorifics is special on 100 silicon chips of double polishings to make hundred micrometer slits using ultraviolet photolithographic method
With) respectively there are three 5 μm of narrow slit patterns up and down, and narrow slit contains the convenient positioning of projection (slit areas is covered with photoresist
Firmly).
Step S202, plates 5 μm silicon nitride layers in photoetching one side using PECVD methods, and carries out photoresist lift off, namely
Slit areas define groove.
Step S203, using positive and negative alignment methods, in silicon chip reverse side photoetching grade rectangular patterns so that wrap rectangular area
Wrap up in width slit above-mentioned.(rectangular area covers with photoresist).
Step S204, plates 5 μm silicon nitride layers in photoetching one side using PECVD methods, and carries out photoresist lift off, namely
Rectangular area defines groove.
Step S205, carries out 90 DEG C of backflow water-baths in Tetramethylammonium hydroxide (TMAH) solution, etches silicon and do not affect
Silicon nitride, more than 10 hours, forms the narrow slit structure of insertion.
Employ the reception substrate of method of the present invention preparation, the electron beam that can be allowed in TEM by narrow insertion slit,
High-power electron beam is avoided for the bombardment destruction of the hanging carbon pipe of length；Also because slit is narrower, rocking for carbon pipe is reduced, side
Just electron diffraction pattern photo and high-resolution TEM pictures are shot.
Present invention also offers a kind of method by measured object CNT growth in situ on above-mentioned self-control substrate, bag
Include：
Step S301, hemoglobin solutions of the concentration for 5mg/ml are spun on oxide layer as catalyst precursor
Silicon chip on, and be heated in air ambient 800 DEG C anneal 20 minutes, be cooled to room temperature, as catalyst slide glass.
The catalyst slide glass prepared in step S301 adjacent carbon pipe is received substrate, and while is put in a stone by step S302
On English plate, push in 950 DEG C of bodies of heater.It is passed through hydrogen so that the ferric oxide particles on catalyst slide glass are fully reduced into ferrum.
Step S303, according to the volume ratio 2 of hydrogen and methane:1 mixed gas that hydrogen and methane are passed through in body of heater, and
So that carbon nano tube growth 20 minutes, CNT can fly up, flies over and drop to carbon pipe and receive on substrate.The present invention is using upper
Trip catalyst substrate, the configuration of accepted downstream substrate allow the CNT of preparation to fly to downstream, directly across slit, form single
The hanging carbon nanotube-sample configuration of root.Room temperature is finally down to, the reception substrate containing CNT is taken out.
By one-dimensional CNT growth in situ on homemade substrate, as homemade substrate is that wide slot coordinates narrow slit
Design, wide slot be used for optically and thermally test, with large span not receive both sides substrate effect the characteristics of；Narrow slit is used for
Electron beam passes through, and with the quality of materials for preventing beam bombardment irradiation from affecting the test of optics calorifics, and avoids beam bombardment
That what is brought rocks；There is on narrow slit locator protrusions, facilitate the position matching of optical microscope and ultramicroscope, improve reality
Test efficiency.
So far, although those skilled in the art will appreciate that detailed herein illustrate and describe multiple showing for the present invention
Example property embodiment, but, without departing from the spirit and scope of the present invention, still can be direct according to present disclosure
It is determined that or deriving many other variations or modifications for meeting the principle of the invention.Therefore, the scope of the present invention is understood that and recognizes
It is set to and covers all these other variations or modifications.
Claims (16)
1. the local locating method of one-dimensional material, for positioning to the local of the one-dimensional material under an observation condition,
So as to the subsequent operation needed for carrying out to the local of the one-dimensional material, wherein, the one-dimensional material is from the sight
It is not directly visible under the conditions of survey；Methods described includes step：
An integument is formed on the surface of the one-dimensional material along the one-dimensional material, so that the one-dimensional material and thereon
The integument it is visible under the observation condition on the whole；Wherein, the integument is by can remove from the one-dimensional material
Lapping formed；
The integument at the local for by the way of LASER HEATING positioning the need of the one-dimensional material is removed, so as to
Parcel section and the naked section corresponding to the local are formed on the one-dimensional material, wherein, at the parcel section, described one
Dimension material keeps being wrapped up by the integument, so that the parcel section is visible under the observation condition；Described exposed
It is at section, invisible under the observation condition during the one-dimensional material is directly exposed to surrounding；Can thus, it is possible to utilize
The parcel section seen is positioned to the sightless naked section as telltale mark.
2. local locating method according to claim 1, it is characterised in that also include：
The one-dimensional material is placed in the depositional environment of the presoma containing the lapping；With
Regulate and control the parameter of the depositional environment, so that the presoma physically or is chemically deposited on the one-dimensional material
Surface, to form the integument.
3. local locating method according to claim 2, it is characterised in that the presoma of the lapping is institute
The gaseous form of lapping is stated, the parameter for regulating and controlling depositional environment includes reducing the temperature of the depositional environment, so that described
Presoma is condensed in liquid or solid-state form on the surface of the one-dimensional material.
4. local locating method according to claim 2, it is characterised in that the lapping is the volatilization material that is easily heated
Material；Methods described also includes：
The local that the need of the one-dimensional material are positioned is heated, to remove the integument at the local.
5. local locating method according to claim 4, it is characterised in that the lapping is ice or dry ice.
6. local locating method according to claim 3, it is characterised in that the depositional environment is by the lapping
The solution that formed of the presoma.
7. local locating method according to claim 6, it is characterised in that the presoma is to be distributed in the solution
Organic substance or the ion to be free in the solution.
8. local locating method according to claim 6, it is characterised in that the lapping is volatile material.
9. local locating method according to claim 8, it is characterised in that the lapping is the volatilization material that is easily heated
Material；Methods described also includes：
The local that the need of the one-dimensional material are positioned is heated, to remove the integument at the local.
10. the local locating method according to any one of claim 1-9, it is characterised in that the one-dimensional material is
Dimension nano material, the observation condition are the one-dimensional material to be observed with optical microscope.
11. local locating methods according to any one of claim 1-9, it is characterised in that also include：
After the local to the one-dimensional material carries out positioning action, the integument in the parcel section is removed.
12. local locating methods according to any one of claim 1-9, it is characterised in that the subsequent operation includes
Determine the thermal conductivity of the one-dimensional material.
13. local locating methods according to claim 12, it is characterised in that the measure of the thermal conductivity includes：
The one-dimensional material is heated until reaching thermally-stabilised poised state；
Obtain position at the first reference point and the second reference point on the one-dimensional material and in the thermally-stabilised poised state
Under temperature；Wherein, first reference point is the abutment points of the parcel section and the adjoiner of the naked section；Described second
Reference point is different from another reference point of the abutment points selected from the naked section；
According to first reference point and the position at the second reference point and temperature and based on the thermal conductivity for pre-building with
The calculated relationship of position and temperature at first reference point and the second reference point is calculating to obtain the thermal conductivity.
14. local locating methods according to claim 13, it is characterised in that the heating one-dimensional material is until reach which
To the step of thermally-stabilised poised state with the local by the one-dimensional material at the integument remove the step of be same
One step.
15. local locating methods according to claim 7, it is characterised in that the ion is salt ion.
16. local locating methods according to claim 7 or 15, it is characterised in that the solution is aqueous solution.
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