CN105158158B - A kind of method for the optic visualization for realizing low-dimension nano material - Google Patents
A kind of method for the optic visualization for realizing low-dimension nano material Download PDFInfo
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Abstract
The invention discloses a kind of method for the optic visualization for realizing low-dimension nano material, by the way that the one or more markers that can be distilled/volatilize are deposited in nano material.It the described method comprises the following steps：Marker is placed in container, marker is heated in atmospheric environment；Substrate containing low-dimension nano material is placed in above marker, marker is made to be deposited in nano material, removes substrate, utilizes optical microphotograph sem observation.The marker is the organo-metallic compound selected from sublimed sulfur, inorganic ammonium salt, carbamide, ammonium persulfate, paraffin or aliphatic acid it is one or more.Method provided by the invention is compared with prior art, method is simple, and strong applicability, controllability are strong, and low-dimension nano material is without any pretreatment, the positioning of nano material under ordinary optical microscope can be realized, significantly facilitate the laboratory research of nano material and industrial production and application；Used marker can be removed controllably, and nano material is not polluted and destroyed, and not influence its follow-up use.
Description
Technical field
Realize what low-dimension nano material was directly observed under ordinary optical microscope or even under naked eyes the present invention relates to a kind of
Method belongs to the characterization technique field of nano material.
Background technology
Nano material refers at least one-dimensional in nanoscale range (1-100nm) or by their works in microstructure
For the material that basic unit is formed, rapidly developed since last century the eighties.Nano material has unique structure
With the properties such as excellent power, electricity, thermal and magnetic, light, have in fields such as nanometer electronic device, biosensor, optical devices wide
Application prospect.Monodimension nanometer material mainly has nano wire, nanotube, nanobelt, nanometer rods etc.；Two-dimension nano materials are mainly received
Rice film, such as graphene.The development of nano material promotes and perfect corresponding characterization technique, as scanning electron microscope,
Transmission electron microscope, atomic force microscope, scanning tunneling microscope, Raman spectrum, X-ray diffraction, photoelectron spectroscopy, atom
Absorption spectrum and calorifics characterization technique etc..These methods effectively characterize the structure and property of nano material, for nanometer material
The research and application of material play important function.
With going deep into for research, the accurate positionin of nano material (especially monodimension nanometer material) and controllable behaviour how are realized
It is vertical to become a problem urgently to be resolved hurrily.The size of nano material is small, can be real using high-resolution instruments such as electron microscopes
The positioning of existing nano material, but there are visual field is small, condition is harsh, take the shortcomings of, it is difficult to controllably be manipulated to it.In addition,
Raman characterization is carried out to monodimension nanometer material needs the locator material first in scanning electron microscope, then pass through Raman spectrum
Face sweeps function (Mapping) and confirms position, then just carries out Raman test, and whole process takes time and effort.
Light microscope have it is cheap, visual field is open, simple and convenient advantage, can be in atmospheric environment to nanometer
Material is manipulated.The size of nano material is small, if the diameter of carbon nanotube only has several nanometers, and conventional light microscope
Resolution ratio is 200nm, can not observe such nano material.Researcher once attempted to realize nano material by loading substance
Observation under ordinary optical microscope.For example, (Huang S H, the Qian Y, et such as Huang SM
Al.J.Am.Chem.Soc.2008,130,11860-11861) realize that single wall carbon is received by way of electrochemical deposition Argent grain
The optic visualization of mitron, but carry out in the liquid phase, and need to do electrode on the carbon nanotubes；(the Zhang R such as Zhang R F
F, Zhang Y Y, et al.Nat.Commun., 2013,4,1727) realize that carbon is received by chemical vapor deposition titanium dioxide etc.
The optical observation of mitron, but this method scope of application is very narrow, it is only effective to hanging carbon nanotube, and in practical application mainly
The carbon nanotube of substrate surface, in addition titanium dioxide be not easy to remove, affect subsequent characterizations and the application of material；Wang J T etc.
(Wang J T, Li T Y, et al.Nano Lett.2014,14,3527-3533) realizes base using the method for water recovery
The optic visualization of carbon nanotube on bottom, but easily evaporated since minute water is dropped under normal temperature environment, the visualization time is short, and
This method is only applicable to the carbon nanotube of substrate surface, invalid to hanging carbon nanotube.Chinese patent CN 101191794A are proposed
A kind of preparation method of the biological sensor based on one-dimensional nano structure, but need to be surface-treated nanostructured,
And fluorescence microscope is used using the fluorescence of excitation, method and apparatus is complex, does not also mention this method to two
The applicability of dimension nano material.CN102564951 disclose a kind of optic visualization for realizing monodimension nanometer material and/or effectively
The method of label, by marker titanium oxide, silica, tin oxide, vanadium oxide, zirconium oxide, bismuth oxide, niobium oxide, zinc oxide and
One or more in silver oxide are supported on monodimension nanometer material.But above-mentioned marker can only realize the light of hanging nano material
Visualization is learned, but the mark substance used has certain toxicity, there is no visualization/label effect to the nano material of substrate surface
Fruit, and marker cannot be removed by mode of heating, can influence further applying for nano material.
In conclusion so far, it is (suitable to substrate surface and hanging nano material there are no a kind of strong applicability
With), controllability is strong, free of contamination labeling method, to realize that nano material is straight even under naked eyes under ordinary optical microscope
Observation is connect, so as to the positioning of aided nano material, manipulation, carries out other characterizations (such as Raman Characterization) and device structure
It builds；In addition, the marker should be able to be controllably removed, avoid polluting nano material, it is follow-up so as to not influence it
It uses.The development of this method constructing and producing in batches to the characterization of nano material and manipulation, nano material base electron device
Etc. being of great significance.
Invention content
In view of the above problems, the present invention is directed to by by the one or more substances that can be distilled/volatilize in nano material
Deposition, realizes under ordinary optical microscope the method that low-dimension nano material is observed under even naked eyes, the low-dimension nano material without
Any pretreatment is needed, microscope used is conventional light microscope, without any special accessory.This method makes the sight of nano material
It examines without the characterization methods such as fluorescence microscope and traditional expensive electron microscope, realizes and received under ordinary optical microscope
The positioning of rice material, and can aided nano material structure and properties characterization and nano material base electron device construct,
This will significantly facilitate the laboratory research of nano material and industrial production and application.In addition, mark substance of the present invention
It can controllably be removed, nano material is not polluted and destroyed, do not influence its follow-up use.
A kind of realization low-dimension nano material provided by the invention is directly observed under ordinary optical microscope or even under naked eyes
Method, include the following steps：
1) marker 1 is placed in container, marker is heated in atmospheric environment, heating temperature is 20 DEG C of (room temperatures) -200
℃；Or marker 2 is used, which obtained by two kinds of substance reactions.A kind of marker presoma is placed in container,
It is slow added into another marker presoma, injection rate 1ml/min-600ml/min, the step condition is according to before two kinds
Depending on driving precursor reactant condition, according to the difference of forerunner's precursor reactant, heating, vacuum or lower pressure can be related to.
2) substrate containing nano material is placed in above marker, places 1s-60min, remove substrate, shown using optics
Micro mirror is observed.
3) nano material for loading marker is placed in heating unit, places 30s-24h, heating temperature is 20 DEG C of (rooms
Temperature) -450 DEG C, it can realize the controllable removal of marker.
In the above method, the step 1) container concretely beaker, culture dish, conical flask, three-necked flask, reagent bottle.
In the above method, warm table, baking oven, batch-type furnace, tube furnace may be used in the step 1) heating unit.
In the above method, concretely 70 DEG C, 90 DEG C, 100 DEG C or 120 DEG C of the step 1) heating temperature.
In the above method, the step 1) injection rate concretely 30ml/min, 60ml/min, 120ml/min or
240ml/min。
In the above method, the step 2) substrate concretely silicon, silica/silicon, quartz, glass, sapphire (three oxygen
Change two aluminium), molybdenum, copper, gold, silver, platinum, nickel, polyethylene terephthalate (PET), dimethyl silicone polymer (PDMS).
In the above method, the step 2) load time concretely 1min, 3min, 5min, 10min or 30min.
The marker 1 is the simple substance such as sublimed sulfur, the organo-metallic compounds such as ferrocene, cobaltocene, dicyclopentadienyl nickel, sulfuric acid
The inorganic ammonium salts such as ammonium, ammonium nitrate, ammonium acetate, ammonium chloride, the organic compounds such as carbamide, ammonium persulfate, paraffin, stearic acid, palm fibre
The aliphatic acid such as palmitic acid acid, lauric acid, resin acid (rosin), the marker 2 can be formed by following two kinds of substance reactions, including nitre
Sour and ammonium hydroxide, hydrochloric acid and ammonium hydroxide, acetic acid and ammonium hydroxide, hydrochloric acid and ammonium hydrogen carbonate, sulfuric acid and ammonium hydrogen carbonate, nitric acid and ammonium hydrogen carbonate,
Sodium hydroxide and ammonium hydrogen carbonate etc., more than marker can be used alone, can also two or more use simultaneously.
In the above method, the marker can be particle or drop, and shape can be spherical, sheet, rodlike etc., size
It can be 30nm-100 μm, the marker of the size has stronger light scattering effect, can be square in ordinary optical microscope
Just it recognizes.
In the above method, the nano material can be nano wire, nanotube, nanometer rods, nanobelt, nano wire and nanometer
Film, nano coating.
In the above method, the nano material concretely zinc oxide nanowire, zinc oxide nano mitron, silicon nanowires, oxygen
Change zinc nanobelt, nanowires of gold, nano silver wire, copper nano-wire, carbon nanotube, graphene, boron nitride, molybdenum disulfide, curing
Tungsten, two selenizing molybdenums, two tungsten selenides, stannic disulfide；
In the above method, the pattern of the nano material can be agglomerate shape, array-like or single, can be vacant state
Or in substrate surface, shape can be hexagon, triangle, quadrangle, pentagon, petal, snowflake shape, circle and random
Shape etc., the number of plies can be individual layer, bilayer or multilayer.
In the above method, warm table, baking oven, batch-type furnace, tube furnace may be used in heating unit described in step 3).
In the above method, the step 3) heating temperature concretely room temperature (20 DEG C), 100 DEG C, 120 DEG C or 150 DEG C.
In the above method, step 3) the removal marker time concretely 1min, 5min, 15min or for 24 hours.This hair
The low-dimension nano material method for visualizing of bright offer can directly observe nano material by ordinary optical microscope, to hanging
Nano material and the nano material of substrate surface are effective.This method is easy to operate, of low cost, adaptation is extensive, can assist receiving
The characterization of rice material and manipulation, it can also be used to preparation of the constructing of aided nano device, composite material and composite construction etc., and institute
There is hypotoxicity with marker, can controllably be removed, do not polluted, do not influence the follow-up use of nano material.
Description of the drawings
Fig. 1 is simple process figure in the embodiment of the present invention 1, and the optical microphotograph sem observation of nano material can be two by A, B
Approach is realized.Wherein 1 is the substrate for growing or being dispersed with nano material, and 2 be the container for containing marker 1, and 3 is in markers 2
Presoma, 4 be another presoma in marker 2, and 5 be precursor gas/liquid velocity controller, and 6 be light microscope.
Fig. 2 is the morphology characterization after single nanomaterial loadings marker (sublimed sulfur), nanometer material therein in embodiment 1
Expect for carbon nanotube.Wherein Fig. 2 (a) (b) is respectively the light microscope light field of carbon nanotube in substrate and details in a play not acted out on stage, but told through dialogues photo, wherein
The striped of horizontal direction corresponds to carbon nanotube.Fig. 2 (c) is electron scanning micrograph, and Fig. 2 (d) shines for atomic force microscope
Piece.
Fig. 3 is carbon nanotube loaded marker (sublimed sulfur) optical photograph and the Raman table afterwards of substrate surface in embodiment 1
Sign, wherein Fig. 3 (a) are light microscope photograph via bright field, and wherein the carbon nanotube indicated by arrow is to carry out Raman Characterization
Carbon nanotube, Fig. 3 (b) be carbon nanotube corresponding to arrow Raman spectrogram.
Fig. 4 is the morphology characterization of hanging carbon nanotube loaded marker (sublimed sulfur) in embodiment 2, wherein Fig. 4 (a) (b)
For light microscope photograph via bright field, Fig. 4 (c) is Optical microscope dark field photo, and Fig. 4 (d) is electron scanning micrograph, is schemed
4 (e) is to manipulate photo to the controllable of the carbon nanotube under light microscope.
Fig. 5 is the optical visible of the carbon nanotube loaded marker (sublimed sulfur) on different base surface in embodiment 3,4,5
Change as a result, wherein Fig. 5 (a) (b) is respectively the light microscope light field of pure silicon substrate surface carbon nanotube and details in a play not acted out on stage, but told through dialogues photo, Fig. 5
(c) it is the light microscope photograph via bright field of quartz substrate surface single-walled carbon nanotube, Fig. 5 (d) is polyethylene terephthalate
The optical microscope photograph of ester (PET) substrate surface carbon nanotube.
Fig. 6 is the optics that different solid marker matter realize hanging carbon nanotube in embodiment 10,11,12,13,14,15
Micro- sem observation, wherein Fig. 6 (a)-(f) are respectively that vacantly carbon nanotube loaded chloride solid, ammonium nitrate solid, ammonium acetate are solid
Body, ammonium sulfate solids, carbamide, ferrocene optical microscope photograph.
Fig. 7 is the light that two kinds of presomas mark substance obtained by the reaction realizes hanging carbon nanotube in embodiment 16,17,18
Micro- sem observation is learned, wherein Fig. 7 (a)-(c) is respectively hanging carbon nanotube loaded hydrochloric acid and ammonium chloride, the nitric acid of ammonium hydroxide reaction
The optical microscope photograph of the ammonium acetate of ammonium nitrate, acetic acid and ammonium hydroxide reaction with ammonium hydroxide reaction.
Fig. 8 is that the mark substance (sublimed sulfur) that the different loads time obtains in embodiment 2 realizes the light of hanging carbon nanotube
Microscope photo is learned, wherein Fig. 8 (a) load times are 1min, and (b) load time is 5min, and (c) load time is 10min,
(d) load time is 20min, and the different loads time can control the size of load marker, so as to regulate and control effect of visualization.
Fig. 9 is that different markers realize hanging and substrate surface nano material optics in embodiment 19,20,21,22,23
The optical microscope photograph of microscope photo, wherein Fig. 9 (a) (b) for hanging carbon nanotube loaded paraffin, the load temperature of the two
It is different；Fig. 9 (c) is hanging carbon nanotube loaded stearic optical microscope photograph；Fig. 9 (d) is hanging carbon nanotube loaded
The optical microscope photograph of palmitic acid；Fig. 9 (e) is hanging carbon nanotube loaded lauric optical microscope photograph；Fig. 9 (f)
Optical microscope photograph for hanging carbon nanotube loaded resin acid；Fig. 9 (g) is the carbon nanotube loaded ammonium sulfate of substrate surface
Optical microscope photograph；Fig. 9 (h) is the optical microscope photograph of the carbon nanotube loaded resin acid of substrate surface；Fig. 9 (i) is base
The carbon nanotube loaded lauric optical microscope photograph of bottom surface.
Figure 10 is the basic characterization of single nanomaterial loadings marker (sublimed sulfur) in embodiment 24,25,26, wherein scheming
10 (a) (b) are respectively the optical microscope photograph of zinc oxide nanowire and copper nano-wire for loading sublimed sulfur, and Figure 10 (c) is silver
The electron scanning micrograph of nano wire, Figure 10 (d) are the optical microscope photograph for the nano silver wire for loading sublimed sulfur.
Figure 11 is that the carbon nanotube loaded marker of nano material (sublimed sulfur) is realized under light microscope in embodiment 27
Observation removes controllable observation of the marker so as to fulfill nano material by mode of heating.Figure 11 (a) (c) is load marker
Nano material optical microscope photograph, Figure 11 (b) (d) is that the light microscope after heating removal marker at same position shines
Piece.As it can be seen that marker can effectively remove.Figure 12 is the carbon nanotube loaded marker of nano material (sublimed sulfur) in embodiment 27
Realize that optic visualization realizes visual comparison with nanomaterial loadings titanium dioxide in embodiment 28.Figure 12 (a) is load
The nano material of the nano material optical microscope photograph of marker sublimed sulfur, substrate surface and overhanging portion is visible；Figure 12
(b) the nano material optical microscope photograph of carried titanium dioxide particle, only overhanging portion nano material are visible；Figure 12 (c) is
The optical microscope photograph of substrate surface nanomaterial loadings marker (sublimed sulfur)；Figure 12 (d) is mode of heating removal label
The optical microscope photograph of corresponding position after object sublimed sulfur；Figure 12 (e) is substrate surface nanomaterial loadings titanium dioxide granule
Optical microscope photograph, it is seen that titanium dioxide does not have effect of visualization to substrate surface nano material.
Figure 13 is the observation that titanium dioxide realizes under hanging nano material carbon nanotube light microscope in embodiment 28.Figure
13 (a) (c) are the hanging nano material optical microscope photograph of carried titanium dioxide；Figure 13 (b) (d) is optical microphotograph after heating
Mirror photo, it is seen that hanging carbon nanotube is under an optical microscope still as it can be seen that illustrate that titanium dioxide is not easy to remove.
Figure 14 is that the carbon nanotube loaded marker of nano material (sublimed sulfur) realizes optic visualization and reality in embodiment 27
Apply the comparison that stannic oxide in example 29 realizes carbon nanotube optic visualization.Figure 14 (a) is hanging carbon nanotube loaded sublimed sulfur
Optical microscope photograph, the carbon nanotube of overhanging portion and substrate surface is visible；Figure 14 (b) is hanging carbon nanotube loaded
The carbon nanotube of the optical microscope photograph of stannic oxide, only overhanging portion is visible；After Figure 14 (c) is heat treatment, carbon nanometer
Pipe is still able to differentiate in light microscope, illustrates that stannic oxide is not easy to remove；Figure 14 (d) is hanging carbon nanotube loaded two
The optical microscope photograph of tin oxide, Figure 14 (e) are the optical microscope photograph of same position after heat treatment, it is seen then that dioxy
Change tin to be difficult to remove by mode of heating.
Figure 15 is that marker (sublimed sulfur) realizes base before and after the visualization of substrate surface nano material carbon nanotube in embodiment 1
The influence of this property.Figure 15 (a) is the result of Raman characterization before and after load marker, it is seen that does not influence the Raman of material
Matter；Figure 15 (b) be load marker before and heating removal marker after (embodiment 27) transfer characteristic curve as a result, threshold value is electric
Pressure does not change, it is seen that does not influence the electrical properties of material.
Figure 16 is the characterization result of graphene nano material load marker (sublimed sulfur) in embodiment 30, wherein Figure 16
(a) (b) is respectively to load the light microscope light field of graphene of sublimed sulfur and details in a play not acted out on stage, but told through dialogues photo, and Figure 16 (c) is corresponding region
Electron scanning micrograph.
Specific embodiment
Using material, reagent etc. in following embodiments, unless otherwise instructed, obtain from commercial channels；Used in it
Microscope is commercially available ordinary optical microscope, does not add any special accessory.
Embodiment 1, the optic visualization that single-root carbon nano-tube in silica/silicon substrate is realized using sublimed sulfur
Concrete technology flow process as shown in Figure 1, get out the overlength carbon nano pipe being grown in silica/silicon substrate first
Then sublimed sulfur is heated to 120 DEG C by horizontal array by warm table, after temperature stabilization, by the substrate with carbon nanotube
It is upside down in above sublimed sulfur, is removed after 5min, you can utilize optical microphotograph sem observation.
The optical photograph of sublimed sulfur load carbon nanotube prepared in the present embodiment is as shown in Fig. 2, by optical photograph, sweep
Electron micrograph and atomic force microscopy are retouched it is found that sublimed sulfur effectively loads on the carbon nanotubes, and realizes
The optic visualization of carbon nanotube in silica/silicon substrate.
The carbon nanotube of sublimed sulfur is loaded in the present embodiment can realize optic visualization, facilitate the close of statistics carbon nanotube
It spends and single-root carbon nano-tube is accurately positioned, the growth conditions of carbon nanotube is instructed to adjust, can also facilitate auxiliary carbon nanometer
The Raman characterization of pipe, as shown in Figure 3.
Property comparison in the present embodiment before and after load sublimed sulfur is as shown in figure 15, and Raman and electrical properties do not change.
Embodiment 2, the optic visualization that hanging carbon nanotube is realized using sublimed sulfur
Concrete technology flow process is with embodiment 1, substrate grown carbon nanotube of the selection with slit in the present embodiment, in slit
Place's carbon nanotube is in vacant state, and hanging carbon nanotube contributes to subsequent controllable manipulation.Growth there is into hanging carbon nanometer
The substrate of pipe is placed in above 120 DEG C of sublimed sulfurs, and load time 5min removes sample i.e. observable.
The sublimed sulfur prepared in the present embodiment loads the optical photograph of hanging carbon nanotube as shown in figure 4, being shone by optics
Piece, electron scanning micrograph realize hanging carbon nanotube it is found that sublimed sulfur is effectively supported in hanging carbon nanotube
Optic visualization.
The hanging carbon nanotube of load sublimed sulfur manufactured in the present embodiment is under an optical microscope it is observed that thus
It can realize the controllable manipulation to carbon nanotube, detailed process is shown in Fig. 4.It as shown in Figure 4, can be effective by loading sublimed sulfur
It realizes the optic visualization of hanging carbon nanotube, and it is positioned, realize controllable manipulate.
Embodiment 3, the optic visualization that pure silicon substrate carbon nanotube is realized using sublimed sulfur
Concrete technology flow process gets out the overlength carbon nano pipe horizontal array being grown in pure silicon substrate first with embodiment 1
Row, are then heated to 120 DEG C by warm table by sublimed sulfur, and after temperature stabilization, the pure silicon substrate with carbon nanotube is fallen
It puts above sublimed sulfur, is removed after 5min, you can utilize optical microphotograph sem observation.
The optical photograph of sublimed sulfur load carbon nanotube prepared in the present embodiment is as shown in figure 5, can by optical photograph
Know, sublimed sulfur effectively loads on the carbon nanotubes, and realizes the optic visualization of carbon nanotube in pure silicon substrate.
Embodiment 4, the optic visualization that quartz substrate carbon nanotube is realized using sublimed sulfur
Concrete technology flow process is ready to grow single-walled carbon nanotube horizontal array on a quartz substrate first with embodiment 1
Row, are then heated to 120 DEG C by warm table by sublimed sulfur, and after temperature stabilization, the quartz substrate with carbon nanotube is fallen
It puts above sublimed sulfur, is removed after 5min, you can utilize optical microphotograph sem observation.
The optical photograph of sublimed sulfur load carbon nanotube prepared in the present embodiment is as shown in figure 5, can by optical photograph
Know, sublimed sulfur effectively loads on the carbon nanotubes, and realizes the optic visualization of single-walled carbon nanotube in quartz substrate.
Embodiment 5, the optical visible that polyethylene terephthalate (PET) substrate carbon nanotube is realized using sublimed sulfur
Change
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 120 DEG C of sublimed sulfurs, load time 5min, after removing under an optical microscope to carbon nanotube into
Row is controllable to be manipulated, and carbon nanotube is transferred on PET substrate.Treat that sublimed sulfur volatilization is complete, in optics
Carbon nanotube is not observed in microscope, sublimed sulfur is heated to 120 DEG C using warm table at this time, after temperature stabilization, will be had
The PET substrate of carbon nanotube is upside down in above sublimed sulfur, is removed after 5min, you can shown using optics
Micro mirror is observed.
The optical photograph of sublimed sulfur load carbon nanotube is as shown in figure 5, by optical photograph it is found that distillation in the present embodiment
Sulphur effectively loads on the carbon nanotubes, and the optics for realizing the upper carbon nanotube of PET substrate can
Depending on change.
Embodiment 6, the optic visualization that dimethyl silicone polymer (PDMS) substrate carbon nanotube is realized using sublimed sulfur
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 120 DEG C of sublimed sulfurs, load time 5min, after removing under an optical microscope to carbon nanotube into
Row is controllable to be manipulated, and carbon nanotube is transferred in dimethyl silicone polymer substrate.Treat that sublimed sulfur volatilization is complete, in light microscope
In do not observe carbon nanotube, sublimed sulfur is heated to 120 DEG C using warm table at this time, after temperature stabilization after, will have carbon nanometer
The dimethyl silicone polymer substrate of pipe is upside down in above sublimed sulfur, is removed after 5min, you can utilize optical microphotograph sem observation.
Embodiment 7, the optic visualization that substrate of glass carbon nanotube is realized using sublimed sulfur
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 120 DEG C of sublimed sulfurs, load time 5min, after removing under an optical microscope to carbon nanotube into
Row is controllable to be manipulated, and carbon nanotube is transferred in substrate of glass.It treats that sublimed sulfur volatilization is complete, is to observe not in light microscope
Carbon nanotube is arrived, sublimed sulfur is heated to 120 DEG C using warm table at this time, after temperature stabilization, there will be the glass of carbon nanotube
Glass substrate is upside down in above sublimed sulfur, is removed after 5min, you can utilize optical microphotograph sem observation.
Embodiment 8, the optic visualization that molybdenum base bottom carbon nanotube is realized using sublimed sulfur
Concrete technology flow process selects molybdenum sheet substrate grown carbon nanotube, growth is had carbon nanotube first with embodiment 2
Substrate is placed in above 120 DEG C of sublimed sulfurs, load time 5min, i.e. using being observed under light microscope after removing.
Embodiment 9 realizes agglomerate shape or the optic visualization of orthogonal array carbon nanotube using sublimed sulfur
Agglomerate shape or orthogonal array carbon nanotube are dispersed in water first, add in surfactant aid dispersion, ultrasound
30min uniformly disperses carbon nanotube.Carbon nanotube is dispersed in substrate by way of spin coating, 60 DEG C of dry 1h.Then
Sublimed sulfur is heated to 120 DEG C by warm table, after temperature stabilization, the substrate for being dispersed with carbon nanotube is upside down in sublimed sulfur
Top is removed after 5min, you can utilize optical microphotograph sem observation.
Embodiment 10, the optic visualization that hanging carbon nanotube is realized using ammonium chloride
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 150 DEG C of ammonium chlorides, and load time 10min is observed under an optical microscope after removing.
Chloride solid loads the optical photograph of hanging carbon nanotube as shown in fig. 6, passing through optical photograph in the present embodiment
It is found that sal-ammoniac solid effectively loads the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 11, the optic visualization that hanging carbon nanotube is realized using ammonium nitrate
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 100 DEG C of ammonium nitrate, and load time 10min is observed under an optical microscope after removing.
Ammonium nitrate solid loads the optical photograph of hanging carbon nanotube as shown in fig. 6, passing through optical photograph in the present embodiment
It is found that ammonium nitrate solid effectively loads the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 12, the optic visualization that hanging carbon nanotube is realized using ammonium acetate
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 80 DEG C of ammonium acetates, and load time 10min is observed under an optical microscope after removing.
The optical photograph of the hanging carbon nanotube of ammonium acetate solid supported is as shown in fig. 6, pass through optical photograph in the present embodiment
It is found that ammonium acetate solid effectively loads the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 13, the optic visualization that hanging carbon nanotube is realized using ammonium sulfate
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 120 DEG C of ammonium sulfate, and load time 5min is observed under an optical microscope after removing.
Ammonium sulfate solids load the optical photograph of hanging carbon nanotube as shown in fig. 6, passing through optical photograph in the present embodiment
It is found that ammonium sulfate solids effectively load the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 14, the optic visualization that hanging carbon nanotube is realized using carbamide
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 70 DEG C of carbamides, and load time 15min is observed under an optical microscope after removing.
In the present embodiment carbamide load the optical photograph of hanging carbon nanotube as shown in fig. 6, by optical photograph it is found that
Carbamide solid effectively loads the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 15, the optic visualization that hanging carbon nanotube is realized using ferrocene
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 100 DEG C of ferrocene, and load time 1min is observed under an optical microscope after removing.
The optical photograph of the hanging carbon nanotube of ferrocene solid supported is as shown in fig. 6, pass through optical photograph in the present embodiment
It is found that ferrocene solid effectively loads the optic visualization on the carbon nanotubes, realizing hanging carbon nanotube.
Embodiment 16, the optic visualization that hanging carbon nanotube is realized using hydrochloric acid and ammonium hydroxide
Then concrete technology flow process is measured a certain amount of as shown in Figure 1, select the substrate grown carbon nanotube with slit first
Hydrochloric acid solution is placed it in beaker, and it is molten that by syringe ammonia spirit is injected into hydrochloric acid with given pace (120ml/min)
In liquid, the substrate that growth has hanging carbon nanotube is placed in above beaker, the white cigarette for reacting generation is ammonium chloride, and ammonium chloride loads
In hanging carbon nanotube, observed under an optical microscope after being removed after 30s.
Hydrochloric acid and ammonium hydroxide reaction generate optical photograph such as Fig. 7 institutes that ammonium chloride loads hanging carbon nanotube in the present embodiment
Show, by optical photograph it is found that hydrochloric acid and ammonium hydroxide reaction product can effectively load on the carbon nanotubes, realize hanging carbon
The optic visualization of nanotube.
Embodiment 17, the optic visualization that hanging carbon nanotube is realized using nitric acid and ammonium hydroxide
Concrete technology flow process first selects the substrate grown carbon nanotube with slit, then measures a certain amount of with embodiment 14
Salpeter solution is placed it in beaker, and it is molten that by syringe ammonia spirit is injected into nitric acid with given pace (120ml/min)
In liquid, the substrate that growth has hanging carbon nanotube is placed in above beaker, the white cigarette for reacting generation is ammonium nitrate, and ammonium nitrate loads
In hanging carbon nanotube, observed under an optical microscope after being removed after 30s.
Nitric acid and ammonium hydroxide reaction generate optical photograph such as Fig. 7 institutes that ammonium nitrate loads hanging carbon nanotube in the present embodiment
Show, by optical photograph it is found that nitric acid and ammonium hydroxide reaction product can effectively load on the carbon nanotubes, realize hanging carbon
The optic visualization of nanotube.
Embodiment 18, the optic visualization that hanging carbon nanotube is realized using acetic acid and ammonium hydroxide
Concrete technology flow process first selects the substrate grown carbon nanotube with slit, then measures a certain amount of with embodiment 14
Acetic acid solution is placed it in beaker, and it is molten that by syringe ammonia spirit is injected into acetic acid with given pace (120ml/min)
In liquid, the substrate that growth has hanging carbon nanotube is placed in above beaker, the white cigarette for reacting generation is ammonium acetate, and ammonium acetate is in water
Middle solubility is high, can form ammonium acetate solution and be supported in hanging carbon nanotube, in light microscope after being removed after 1min
Lower observation.
Acetic acid and ammonium hydroxide reaction generate optical photograph such as Fig. 7 institutes that ammonium acetate loads hanging carbon nanotube in the present embodiment
Show, by optical photograph it is found that acetic acid and ammonium hydroxide reaction product can effectively load on the carbon nanotubes, realize hanging carbon
The optic visualization of nanotube.
Embodiment 19, the optic visualization that carbon nanotube in hanging and substrate is realized using paraffin
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 150 DEG C of paraffin, and load time 10min is observed under an optical microscope after removing.
The paraffin prepared in the present embodiment loads optical microscope photograph such as Fig. 9 institutes of carbon nanotube in hanging and substrate
Show, by optical photograph it is found that paraffin effectively loads the light on the carbon nanotubes, realizing carbon nanotube in hanging and substrate
Learn visualization.
Embodiment 20, the optic visualization that carbon nanotube in hanging and substrate is realized using stearic acid
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 100 DEG C of stearic acid, and load time 10min is observed under an optical microscope after removing.
The stearic acid prepared in the present embodiment loads optical microscope photograph such as Fig. 9 institutes of carbon nanotube in hanging and substrate
Show, by optical photograph it is found that stearic acid effectively loads on the carbon nanotubes, realize carbon nanotube in hanging and substrate
Optic visualization.
Embodiment 21, the optic visualization that carbon nanotube in hanging and substrate is realized using palmitic acid
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 100 DEG C of palmitic acids, and load time 10min is observed under an optical microscope after removing.
The palmitic acid prepared in the present embodiment loads optical microscope photograph such as Fig. 9 institutes of carbon nanotube in hanging and substrate
Show, by optical photograph it is found that palmitic acid effectively loads on the carbon nanotubes, realize carbon nanotube in hanging and substrate
Optic visualization.
Embodiment 22, the optic visualization that carbon nanotube in hanging and substrate is realized using lauric acid
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 80 DEG C of lauric acid, and load time 10min is observed under an optical microscope after removing.
The lauric acid prepared in the present embodiment loads optical microscope photograph such as Fig. 9 institutes of carbon nanotube in hanging and substrate
Show, by optical photograph it is found that lauric acid effectively loads on the carbon nanotubes, realize carbon nanotube in hanging and substrate
Optic visualization.
Embodiment 23, the optic visualization that carbon nanotube in hanging and substrate is realized using resin acid
Concrete technology flow process selects the substrate grown carbon nanotube with slit, growth is had hanging carbon first with embodiment 2
The substrate of nanotube is placed in above 120 DEG C of resin acids, and load time 10min is observed under an optical microscope after removing.
The resin acid prepared in the present embodiment loads optical microscope photograph such as Fig. 9 institutes of carbon nanotube in hanging and substrate
Show, by optical photograph it is found that resin acid effectively loads on the carbon nanotubes, realize carbon nanotube in hanging and substrate
Optic visualization.
Embodiment 24, the optic visualization that zinc oxide nanowire is realized using sublimed sulfur
Concrete technology flow process prepares zinc oxide nanowire, obtained zinc-oxide nano by hydro-thermal method first with embodiment 1
Line is dissolved in ethanol solution, and ultrasonic disperse recycles the mode of spin coating to be dispersed in silica/silicon substrate, then passes through warm table
Sublimed sulfur is heated to 120 DEG C, after temperature stabilization, the substrate for being dispersed with zinc oxide is upside down in above sublimed sulfur, after 5min
It removes, you can utilize optical microphotograph sem observation.
The optical photograph of sublimed sulfur load zinc oxide nanowire prepared in the present embodiment is as shown in Figure 10, is shone by optics
Piece realizes the optic visualization of zinc oxide nanowire it is found that sublimed sulfur is effectively supported on zinc oxide nanowire.
Embodiment 25, the optic visualization that copper nano-wire is realized using sublimed sulfur
Concrete technology flow process gets out copper nano-wire, it is molten that obtained copper nano-wire is dissolved in n-hexane first with embodiment 1
Liquid, ultrasonic disperse recycle the mode of spin coating to be dispersed in silica/silicon substrate, are then heated sublimed sulfur by warm table
To 120 DEG C, after temperature stabilization, the substrate for being dispersed with copper nano-wire is upside down in above sublimed sulfur, is removed after 5min, you can profit
It is observed with light microscope.
The optical photograph of sublimed sulfur load copper nano-wire prepared in the present embodiment is as shown in Figure 10, can by optical photograph
Know, sublimed sulfur is effectively supported on copper nano-wire, realizes the optic visualization of copper nano-wire.
Embodiment 26, the optic visualization that nano silver wire is realized using sublimed sulfur
Concrete technology flow process gets out nano silver wire, it is molten that obtained nano silver wire is dissolved in isopropanol first with embodiment 1
Liquid, ultrasonic disperse recycle the mode of spin coating to be dispersed in silica/silicon substrate, are then heated sublimed sulfur by warm table
To 120 DEG C, after temperature stabilization, the substrate for being dispersed with nano silver wire is upside down in above sublimed sulfur, is removed after 5min, you can profit
It is observed with light microscope.
The optical photograph of sublimed sulfur load nano silver wire prepared in the present embodiment is as shown in Figure 10, can by optical photograph
Know, sublimed sulfur is effectively supported on nano silver wire, realizes the optic visualization of nano silver wire.
Embodiment 27, realized using sublimed sulfur hanging carbon nanotube optic visualization and marker removal
The same Examples 1 and 2 of concrete technology flow process, selection silica/silicon substrate and the base with slit in the present embodiment
Bottom grows carbon nanotube respectively, and carbon nanotube is in vacant state at slit, hanging carbon nanotube contribute to it is subsequent can
Control manipulates.The substrate of the carbon nanotube of substrate surface and hanging carbon nanotube is respectively placed in above 120 DEG C of sublimed sulfurs, during load
Between 5min, remove sample i.e. observable.The sample that loading has marker sublimed sulfur is placed in 120 DEG C of thermal station, heats 15min, takes
Lower sample, that is, observable.
In the present embodiment after substrate surface and hanging carbon nanotube loaded sublimed sulfur after optical photograph and distillation removal of sulphur
Optical photograph it is as shown in figure 11, it is seen that sublimed sulfur can be efficiently removed.
Embodiment 28, the optic visualization for preparing titanium dioxide granule realization carbon nanotube as presoma using titanium tetrachloride
Specific implementation process such as CN102564951A embodiments 1.Heating removal titanium dioxide uses temperature as 120 DEG C, when
Between be 15min.
Carried titanium dioxide realizes that the optic visualization of hanging carbon nanotube and titanium dioxide heating do not remove in the present embodiment
As shown in Figures 12 and 13, titanium dioxide can realize the optic visualization of hanging CNT to the optical photograph gone, but not have to CNT in substrate
It is effective.Fail to remove titanium dioxide by mode of heating, further applying for nano material can be influenced.
Embodiment 29, the optic visualization for preparing stannic oxide particle realization carbon nanotube as presoma using butter of tin
Specific implementation process such as CN102564951A embodiments 2.Heating removal stannic oxide uses temperature as 120 DEG C, when
Between be 15min.
Stannic oxide realizes that the optical microphotograph Microscopic observation of hanging carbon nanotube and stannic oxide heat not in the present embodiment
The optical photograph of removing is as shown in figure 14, and stannic oxide can realize the optic visualization of hanging CNT, but not have to CNT in substrate
Effect.Fail to remove stannic oxide by mode of heating, illustrate that this method controllability is poor, and the presence of stannic oxide can influence
Nano material is further applied.
Embodiment 30, the optic visualization that graphene on copper-based bottom is realized using sublimed sulfur
Concrete technology flow process gets out the graphene sample being grown on copper-based bottom, then by adding first with embodiment 1
Sublimed sulfur is heated to 120 DEG C by thermal station, and after temperature stabilization, the copper sheet substrate with graphene is upside down in above sublimed sulfur,
It is removed after 5min, you can utilize optical microphotograph sem observation.
The optical photograph of sublimed sulfur load graphene prepared in the present embodiment is as shown in figure 16, can by optical photograph
Know, sublimed sulfur is effectively supported on graphene, realizes the optic visualization of graphene.
Claims (9)
1. a kind of method for the optic visualization for realizing low-dimension nano material, passes through the one or more marks that will can be distilled/volatilize
Note object deposits in nano material, which is characterized in that the described method comprises the following steps：
1) marker is placed in container, marker is heated in atmospheric environment, heating temperature is 20 DEG C -200 DEG C；
2) substrate containing low-dimension nano material is placed in above marker, places 1s-60min, make marker in nano material
Upper deposition, removes substrate, utilizes optical microphotograph sem observation；
3) marker being deposited in nano material can effectively remove, and heating temperature is 20 DEG C -450 DEG C, and heating time is
30s-24h；
The marker is selected from sublimed sulfur, organo-metallic compound, inorganic ammonium salt, carbamide, ammonium persulfate, paraffin or fat
Sour is one or more；
The inorganic ammonium salt is ammonium sulfate, ammonium nitrate, ammonium acetate or ammonium chloride.
2. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, organic gold
Category compound is ferrocene, cobaltocene or dicyclopentadienyl nickel, and the aliphatic acid is stearic acid, palmitic acid, lauric acid or resin acid.
3. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, the marker by
Following two kinds of markers forerunner's precursor reactants form, and specifically a kind of marker precursor is placed in container, are slow added into another
A kind of marker presoma, injection rate 1ml/min-600ml/min, marker presoma include nitric acid and ammonium hydroxide, hydrochloric acid
With ammonium hydroxide, acetic acid and ammonium hydroxide, hydrochloric acid and ammonium hydrogen carbonate, sulfuric acid and ammonium hydrogen carbonate, nitric acid and ammonium hydrogen carbonate, sodium hydroxide and carbonic acid
Hydrogen ammonium, more than marker can be used alone, but also two or more are used simultaneously.
4. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, the low-dimensional are received
Rice material is nano wire, nanotube, nanometer rods, nanobelt, nano wire, nano thin-film or nano coating.
5. a kind of method of optic visualization for realizing low-dimension nano material according to claim 4, the low-dimensional are received
Rice material is zinc oxide nanowire, zinc oxide nano mitron, silicon nanowires, zinc oxide nano-belt, nanowires of gold, nano silver wire, copper
Nano wire, carbon nanotube, graphene, boron nitride, molybdenum disulfide, tungsten disulfide, two selenizing molybdenums, two tungsten selenides or stannic disulfide.
6. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, the marker
For particle or drop, size is 30nm-100 μm.
7. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, the heating temperature
Degree is specially 70 DEG C, 90 DEG C, 100 DEG C or 120 DEG C.
8. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, described in step 2)
Substrate is selected from silicon, silica/silicon, quartz, glass, sapphire, molybdenum, copper, gold, silver, platinum, nickel, polyethylene terephthalate
Ester (PET) or dimethyl silicone polymer (PDMS).
9. a kind of method of optic visualization for realizing low-dimension nano material according to claim 1, during the placement
Between be specially 3min, 5min, 10min or 30min.
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| CN102564951A (en) * | 2012-02-08 | 2012-07-11 | 清华大学 | Method for realizing optic visualization and/or effective marking on one-dimensional nanometer material |
| CN104359941A (en) * | 2014-11-24 | 2015-02-18 | 中国科学院物理研究所 | Local positioning method of one-dimensional material |
| CN104483310A (en) * | 2014-12-03 | 2015-04-01 | 济南大学 | Construction method of visual self-energized glucose biosensor |
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| CN102564951A (en) * | 2012-02-08 | 2012-07-11 | 清华大学 | Method for realizing optic visualization and/or effective marking on one-dimensional nanometer material |
| CN104359941A (en) * | 2014-11-24 | 2015-02-18 | 中国科学院物理研究所 | Local positioning method of one-dimensional material |
| CN104483310A (en) * | 2014-12-03 | 2015-04-01 | 济南大学 | Construction method of visual self-energized glucose biosensor |
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