CN109778214A - A kind of method in fast selective filling nanoparticle to carbon nanotubes lumen - Google Patents
A kind of method in fast selective filling nanoparticle to carbon nanotubes lumen Download PDFInfo
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- CN109778214A CN109778214A CN201711130179.2A CN201711130179A CN109778214A CN 109778214 A CN109778214 A CN 109778214A CN 201711130179 A CN201711130179 A CN 201711130179A CN 109778214 A CN109778214 A CN 109778214A
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Abstract
Method the present invention relates to composite structure of carbon nano tube field, in the fast selective filling nanoparticle to carbon nanotube hollow lumen of specially a kind of electric field power drive.The anodic alumina film for being deposited with thin layer carbon is assembled on electrolytic cell assembly, the electrolyte solution of element need to be filled in electrolytic cell injection and is inserted into electrode, applying DC voltage between two electrodes fills electrolyte rapidly in the anodised aluminium nano pore coated to carbon-coating, it takes out anodic alumina film, heat treatment, finally remove anodic alumina film template, that is, obtain the composite structure of carbon nano tube of nano-particles filled.Nanoparticle selective filling in the carbon nanotubes lumen of both ends open, be evenly distributed.This method filling process is quick, only need 0.5 second to 5 minutes；Loading controllable precise, content highest can fill up carbon nanotubes lumen.It effectively solves to fill the problems such as complex process of nanoparticle, time-consuming, a large amount of fillings are difficult in carbon nanotube at present.
Description
Technical field
The present invention relates to composite structure of carbon nano tube field, the fast selective filling of specially a kind of electric field power drive is received
Method in rice corpuscles to carbon nanotube hollow lumen.
Background technique
The hollow lumen of carbon nanotube is typical one-dimensional confinement space, due to the special electronic structure of carbon nanotube itself
And confinement effect, so that carbon nanotube inner material is obvious in terms of crystallinity, magnetism, electric property, chemical catalysis
Different from macroscopic material.It is each that carbon nanotube with novel nano structure made of its internal Nanocomposites has both two kinds of homogenous materials
From advantage, have big specific surface area, pore structure abundant, good structural stability, show excellent conductive performance,
Electrochemical catalysis activity etc., it is potential as acquisitions applications such as catalysis material or electrode materials, controllably prepare nanoparticle
The composite structure of carbon nano tube of filling is the basis of relevant rudimentary and application study.
Currently, the main method for filling nanoparticle inside carbon nanotube has physisorphtion (document, Kumiko
Ajima,Masako Yudasaka,Tatsuya Murakami,Alan Maigne,Kiyotaka Shiba,Sumio
Iijima, Molecular Pharmaceutics.2 (6): 475-480 (2005)), wet (solution) method (document, Hongkun
Zhang,Huaihe Song,Xiaohong Chen,Jisheng Zhou,J.Phys.Chem.C(116):22774-22779
(2012)), gas phase completion method (document, Narun Thamavaranukup, Henning A.Luisa Ruiz-
Gonzalez,Pedro M.F.J.Costa,Jeremy Sloan,Angus Kirkland,Malcolm L.H.Green,
Chemi.Commun. (15): 1686-1687 (2004)), nano fluid suspension direct completion method (document, Guzeliya
Korneva,Haihui Ye,Yury Gogotsi,Derek Halverson,Gary Friedman,Jean-Claude
Bradley, Konstantin G.Kornev, Nano.Lett.5 (5): 879-884 (2005)), chemical vapour deposition technique (text
It offers, Weiqiang Han, Shoushan Fan, Qunqing Li, Yongdan Hu, Science.277 (5330) 1287-1289
(1997)) etc..The range that every kind of method has its applicable, but also all there are some problems, such as: it is difficult to nanoparticle
In 100% selective filling to carbon nanotubes lumen, time-consuming for filling process, charging efficiency is not high, filling process is uncontrollable, fills out
It is single etc. to fill species.Carbon nanotubes need to be cut off and be open in oxidizing acid solution (document 1, Pan by most of work
XL,Fan ZL,Cheng W,Ding YJ,Luo HY,Bao XH.Nature Materials 6:507(2007)；Document 2,
Zhang J, Muller JO, Zheng WQ, Wang D, Su DS, Schlogl R.Nano Letters 8:2738 (2008)),
And the homogeneity for obtaining composite material is poor.
In addition, using the anodised aluminium for being deposited with carbon-coating as template, chemical vapour deposition technique is respectively adopted inventor's early period
The nanoparticulate selectives such as silicon particle, iron oxide are filled into (Chinese invention in carbon nanotube hollow lumen with liquid-phase impregnation process
Patent application 1, Hou Pengxiang, Yu Wanjing, Li Shisheng, Liu Chang, Cheng Huiming, ferric oxide particles selective filling are hollow in carbon nanotubes
Intraluminal method, patent No. ZL200810229969.0；Chinese invention patent application 2, Liu Chang, Yu Wanjing, Hou Pengxiang, Cheng Hui
It is bright, a kind of silicon nanoparticle filling carbon nano-pipe compound and its preparation method and application, the patent No.
ZL201210566788.3)；There are still filling process complexity, filling time length, filling species are limited for both methods, it is difficult to
The deficiencies of obtaining high fill-ratio (peak filling rate is weight ratio 70%).
The critical issue of urgent need to resolve is at present: how to develop a kind of economy, quickly and effectively fill method, realizes and exist
Nanoparticle type and the unrestricted controllable filling of loading in carbon nanotube.
Summary of the invention
The purpose of the present invention is to provide a kind of fast selectives of electric field power drive to fill nanoparticle to carbon nanotube
Method in hollow lumen, solves current fill process complexity, and filling process time-consuming, poor controllability, a large amount of filling difficulties etc. are asked
Topic.
The technical scheme is that
Method in a kind of fast selective filling nanoparticle to carbon nanotubes lumen, will be deposited with the anode of thin layer carbon
Alumina wafer is assembled on electrolytic cell assembly, and the electrolysis groove body of electrolytic cell assembly is separated into two independent electrolysis by assembly
Electrode is inserted into each electrolytic cell in pond respectively, need to fill the electrolyte solution of element in electrolytic cell injection, apply between two electrodes
Add 1~50V DC voltage, fills nanoparticle 0.5 second to 5 minutes, after removing anodic alumina film and being heat-treated, removal
Anodic alumina film obtains the composite structure of carbon nano tube of nano-particles filled；Wherein, it is 20 that anodic alumina film, which has aperture,
The perforation nano pore of~100nm.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, electrolytic cell assembly includes electrolysis
Electrode I, electrode II, sealing rubber strip I, sealing rubber strip II, assembly setting is arranged in groove body and assembly, electrolysis groove body
Organic glass piece I, rubber gasket I, rubber gasket II, organic glass piece II, anodic alumina film, specific structure are as follows:
Assembly is inserted into the groove of electrolysis groove body from top to bottom, is electrolysed groove body by organic glass piece I, rubber gasket
I, anodic alumina film, rubber gasket II, organic glass piece II assembly be separated into two electrolytic cells: electrolytic cell I, electrolytic cell
II, sealing rubber strip I is set at assembly and I cooperation of electrolytic cell, sealing rubber strip is set at assembly and II cooperation of electrolytic cell
II, electrode I is inserted in electrolytic cell I, inserts electrode II in electrolytic cell II；After assembling, the filling device of nano particle is formed；
The anodic alumina film of carbon-coating cladding is clipped in the rubber gasket I of center opening, among rubber gasket II, carbon-coating
The anodic alumina film of cladding is identical as shape, the size of rubber gasket I, II center opening of rubber gasket, carbon-coating cladding
Anodic alumina film the center opening of rubber gasket I, rubber gasket II, organic glass piece I, organic glass is completely covered
Piece II is clamped in rubber gasket I, II outside of rubber gasket, the side pair corresponding with rubber gasket II of organic glass piece II
Claim setting fixed pin, open up pilot hole corresponding with fixed pin on rubber gasket I, rubber gasket II and organic glass piece I,
Organic glass piece I, rubber gasket I, rubber gasket II, organic glass piece II are cooperated by fixed pin and pilot hole, are formed
Assembly.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, two electrodes: electrode I, electricity
Pole II is inert electrode, and when being powered, electrode plays electric action, without reacting with electrolyte.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, two electrolytic cells are interior using same
Kind or xenogenesis electrolyte solution, when holding not electrolyte solution of the same race in two electrolytic cells, two kinds of electrolysis of selection as needed
Liquid and direction of an electric field realize nanoparticle direct rapid synthesis in carbon nanotube hollow lumen.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, the anodic oxidation of carbon-coating cladding
Aluminium flake uses other sheets, via material with similar structure to replace, and realizes nanoparticle in various nanotubes or porous material
Expect the Fast Filling in nano pore.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, heat treatment condition is according to needed for
Depending on grain structure, atmosphere is one or more of air, argon gas, nitrogen, hydrogen gaseous mixture, and temperature is 50~1000
℃。
The fast selective fills the method in nanoparticle to carbon nanotubes lumen, the nanoparticle in carbon nanotube
Concentration, application voltage time accuracy controlling of the sub- content by electrolyte solution, nanoparticle content is within the scope of 0.5~95wt%
Controllable precise.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, nanoparticle contain quantitative change with it
Change and different-shape is presented, exists in granular form when content is lower, the segment dislocation nanometer of carbon nanotube is filled up when content is higher
Stick.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, nanoparticle content exist
When 75wt% or less, exist in granular form.
Method in the fast selective filling nanoparticle to carbon nanotubes lumen, since anodised aluminium is to carbon
The physical isolation effect of nanometer pipe outer wall, nanoparticle 100% are filled in the hollow lumen of carbon nanotube.
Design philosophy of the invention is:
In order to realize high-content of the nano particle in carbon nanotube hollow lumen, controllable filling, pass through design electrolytic cell
Structure, so that negative ions can only be by the anodised aluminium duct that carbon-coating coats to opposite under electric field power drive in electrolyte
Direction is mobile, and negative ions combine in nano pore, and substance not soluble in water directly generates nano particle；It is dissolved in the substance of water
High concentration salt solutions are then formed in nano pore, are uniformly filled in nano pore, then postmenstruation heat treatment can be obtained
The nano particle of even filling.
The invention has the advantages and beneficial effects that:
1, the present invention provides the method quickly, being controllably filled in nano particle in carbon nanotube hollow lumen, receives in carbon
Selective filling nano particle in the hollow lumen of mitron, filling process only need 0.5 second~5 minutes, greatly improve timeliness, solution
Certainly other methods filling process generally requires a few hours to a couple of days, the process difficulties that time-consuming.
2, the present invention provides controllable fill method of a variety of nanoparticles in carbon nanotube hollow lumen, greatly abundant
The carbon nano tube compound material of the structure.
3, the present invention, which provides the controllable fill method of nano-particle content, only needs short time DC charging in electrolytic cell,
Achieve that content in the controllable filling of the unrestricted nanoparticle of 0.5~95wt%, type.The nanoparticle that this method is filled
Son is evenly distributed, content controllable precise, and the type and loading of nanoparticle are unrestricted.Loading is by concentration of electrolyte, application
The conditions such as voltage time accurately control, and especially have significant advantage in terms of a large amount of fillings, can fill up the hollow tube of carbon nanotube
Chamber.
4, the method for the present invention simple process, filling process are not required to expensive device, be it is a kind of it is economical, simple, efficiently in carbon
The method of filling nanoparticle in nanotube.
5, the carbon nanotube of the nano-particles filled of the method for the present invention preparation can be used as nano-reactor and be used for on-spot study,
It can be used as electrochemical energy storage materials or catalysis material etc..
Detailed description of the invention
Fig. 1 is electrolytic cell assembly schematic diagram used in the present invention；Wherein, (a), (b), (c) are respectively to be assembled with electrode
With main view, left view, the top view of the electrolysis groove body of sealing rubber strip；(d), (e), (f) be respectively organic glass piece and
Main view, left view after the exploded view of rubber seal pad assembly, combination；(g) after for assembly and electrolysis groove body assembling
Device left view.In figure, 1 electrolysis groove body；2 electrodes I；3 electrodes II；4 sealing rubber strips I；5 sealing rubber strips II；6 is organic
Sheet glass I；7 rubber gaskets I；8 rubber gaskets II；9 organic glass pieces II；10 anodic alumina films；11 pilot holes；12 is solid
Rationed marketing；13 assemblys；14 grooves；A electrolytic cell I；B electrolytic cell II.
Fig. 2 is the electron micrograph of nickel nano particle filling carbon nano-pipe prepared by embodiment 1；Wherein, (a) is to sweep
Retouch electromicroscopic photograph；It (b) is transmission electron microscope photo.
Fig. 3 is the electron micrograph of ferric oxide nano particles filling carbon nano-pipe prepared by embodiment 2；Wherein, (a)
For stereoscan photograph；It (b) is transmission electron microscope photo.
Fig. 4 is the electron micrograph of chlorination Silver nanorod filling carbon nano-pipe prepared by embodiment 4；Wherein, (a) is
Stereoscan photograph；It (b) is transmission electron microscope photo.
Specific embodiment
As shown in Figure 1, electrolytic cell assembly includes being electrolysed groove body 1 and assembly 13, the electrolysis setting of groove body 1 electrode I 2,
Organic sheet glass I 6, rubber gasket I 7, rubber is arranged in electrode II 3, sealing rubber strip I 4, sealing rubber strip II 5, assembly 13
Gasket II 8, organic glass piece II 9, anodic alumina film 10, specific structure is as follows:
Assembly 13 is inserted into the groove 14 of electrolysis groove body 1 from top to bottom, is electrolysed groove body 1 by organic glass piece I 6, rubber
Glue gasket I 7, anodic alumina film 10, rubber gasket II 8, organic glass piece II 9 assembly 13 be separated into two electrolysis
Pond: sealing rubber strip I 4, assembly 13 and electrolysis are set at I A of electrolytic cell, II B of electrolytic cell, assembly 13 and I A cooperation of electrolytic cell
Sealing rubber strip II 5 is set at II B cooperation of pond, inserts electrode I 2 (inert electrode) in I A of electrolytic cell, electricity is inserted in II B of electrolytic cell
Pole II 3 (inert electrode).Electrolytic cell assembly after assembling, the filling device as nano particle.
The anodic alumina film 10 of carbon-coating cladding is clipped in the rubber gasket I 7 of center opening, among rubber gasket II 8,
The anodic alumina film 10 of carbon-coating cladding is identical as shape, the size of rubber gasket I 7, II 8 center opening of rubber gasket,
The center opening of rubber gasket I 7, rubber gasket II 8, organic glass is completely covered in the anodic alumina film 10 of carbon-coating cladding
Piece I 6, organic glass piece II 9 are clamped in rubber gasket I 7, II 8 outside of rubber gasket, and organic glass piece II 9 and rubber are close
The corresponding side of packing II 8 is symmetrical arranged fixed pin 12, on rubber gasket I 7, rubber gasket II 8 and organic glass piece I 6
Open up pilot hole 11 corresponding with fixed pin 12, organic glass piece I 6, rubber gasket I 7, rubber gasket II 8, organic glass
Piece II 9 is cooperated by fixed pin 12 and pilot hole 11, forms assembly 13.
In the specific implementation process, the quick, selective filling to carbon nanometer by nanoparticle of electric field power drive of the present invention
The anodic alumina film that carbon-coating coats is assembled on electrolytic cell assembly by the method in pipe hollow lumen, and injection need to fill element
Electrolyte solution and be inserted into electrode, apply 1~50V DC voltage between two electrodes and remove anodic oxygen after 0.5 second to 5 minutes
Change aluminium flake, certain atmosphere and at a temperature of handle, last removal anodic alumina film template, the carbon for obtaining nano-particles filled receives
Mitron composite construction, nanoparticle are evenly distributed, content controllable precise within the scope of 0.5~95wt%.
After two electrolytic cells inject electrolyte, the anodic alumina film tow sides of sheet-like carbon layer cladding are connect with electrolyte
Touching, but since interfacial tension acts on, electrolyte cannot be introduced into its nano pore.Adhere to the positive and negative ion of two electrolytic cells separately outside
Under electric field driven, enters in the nano pore of the anodic alumina film of carbon-coating cladding with solution, be precipitated in nano pore insoluble
In the nano particle (such as: silver chloride particle) or high concentration salt solutions (such as: iron nitrate solution) of aqueous solution, external electric field is driven
Dynamic negative ions move in the nano pore of the anodic alumina film of (and can only) carbon-coating cladding.The anode of carbon-coating cladding
Alumina wafer can be replaced with other similar structural material, and similar structures material refers to that the perforation with regularly arranged size uniformity is received
In the form of sheets or membranaceous material or composite material, duct direction is perpendicular to sheet or film material surface for metre hole road, macroscopic view.
For the anodic alumina film of carbon-coating cladding not as electrode, the electrochemical redox for being not involved in external electric field driving is anti-
It answers, is different from electrochemical deposition.Carbon-coating cladding anodic alumina film have aperture be 20~100nm perforation nano pore,
Thickness is unrestricted.
In addition, filling device concretely different shapes and forms, drive as long as not departing from electric field force used in the present invention
The technological means that dynamic electrolyte solution overcomes material interface tension to enter nano pore belongs to the technology scope that the present invention protects.
In the following, the present invention is described in further detail by embodiment:
Embodiment 1
As shown in Figure 1, the anodic alumina film 10 that carbon-coating coats is assembled on electrolytic cell assembly, anodic alumina film 10
It is clipped in the middle by rubber gasket I 7, rubber gasket II 8, and rubber gasket I 7, II 8 center of rubber gasket is completely covered
Rectangular hole, organic glass piece I 6, organic glass piece II 9 be clamped in rubber gasket I 7, the outside of rubber gasket II 8,
Organic glass piece I 6, rubber gasket I 7, anodic alumina film 10, rubber gasket II 8, II 9 sequence of organic glass piece assemble
Assembly 13 is constituted together, sees Fig. 1 (d) and Fig. 1 (e).Assembly 13 is then inserted into the recessed of electrolysis groove body 1 from top to bottom
Slot 14, the filling device after assembling are shown in Fig. 1 (f).Electrolysis groove body 1 is by organic glass piece I 6, rubber gasket I 7, anode at this time
Alumina wafer 10, rubber gasket II 8, organic glass piece II 9 assembly 13 be separated into two electrolytic cells: I A of electrolytic cell, electrolysis
II B of pond, is shown in Fig. 1 (c).Be injected separately into 0.25 mole of every liter of nickel nitrate solution in I A of electrolytic cell, II B of electrolytic cell, electrode I 2,
Apply 10V DC voltage 0.5s between II 3 liang of electrodes of electrode, removes at 10,350 DEG C of anodic alumina film of carbon-coating cladding in hydrogen
It handles 2 hours, then is soaked in 5 moles of every liter of sodium hydroxide solutions at 30 DEG C under the gaseous mixture of gas/argon gas (volume ratio 1/3)
Processing 40 hours removes anodic alumina film template, i.e. the acquisition uniform filling carbon nano-pipe composite material of nickel nano particle.Such as figure
Shown in 2 (a)-(b), nanoparticle is elemental nickel in hollow lumen, mass content~8%, and diameter is distributed as 1~5 nanometer, concentrates
It is distributed in 1~2 nanometer.
Embodiment 2
The anodic alumina film 10 that carbon-coating coats is assembled on electrolytic cell assembly, method is the same as embodiment 1.In electrolytic cell I
A, it is injected separately into 0.4 mole of every liter of iron nitrate solution in II B of electrolytic cell, it is straight applies 20V between II 3 liang of electrode I 2, electrode electrodes
Galvanic electricity presses 25s, removes the anodic alumina film 10 of carbon-coating cladding, dries in 80 DEG C, is warming up to 400 DEG C under nitrogen protection simultaneously again
Constant temperature is handled 5 hours, is finally placed in 25 DEG C of processing, 36 hours removal anodic alumina film moulds in 5 moles of every liter of sodium hydroxide solutions
Plate obtains the composite material of ferric oxide nano particles filling carbon nano-pipe.As shown in Fig. 3 (a)-(b), nanometer in hollow lumen
Particle is iron oxide, mass content~20%, and ferric oxide nano particles diameter is distributed as 10~25 nanometers, integrated distribution in 15~
20 nanometers.
Embodiment 3
The anodic alumina film that carbon-coating coats is assembled on electrolytic cell assembly, method is the same as embodiment 1.I A of electrolytic cell,
It is injected separately into 0.01 mole of every liter of silver nitrate solution and 0.01 mole of every liter of hydrochloric acid solution in II B of electrolytic cell, is sun with electrode I 2
Pole, electrode II 3 be cathode, applies 30V DC voltage 1 minute between two electrodes, remove carbon-coating coat anodic alumina film, in
25 DEG C of processing, 32 hours removal anodised aluminiums in hydrofluoric acid obtain the composite wood of silver chloride nanoparticles filling carbon nano-pipe
Material.Nanoparticle is silver chlorate in hollow lumen, and mass content~35%, silver chloride nanoparticles diameter is distributed as 15~30 and receives
Rice, integrated distribution is in 25~30 nanometers.
Embodiment 4
The anodic alumina film that carbon-coating coats is assembled on electrolytic cell assembly, method is the same as embodiment 1.I A of electrolytic cell,
It is injected separately into 0.05 mole of every liter of silver nitrate solution and 0.05 mole of every liter of hydrochloric acid solution in II B of electrolytic cell, is sun with electrode I 2
Pole, electrode II 3 be cathode, applies 15V DC voltage 5 minutes between two electrodes, remove carbon-coating coat anodic alumina film, in
25 DEG C of processing, 48 hours removal anodised aluminiums in hydrofluoric acid obtain the composite wood of chlorination Silver nanorod filling carbon nano-pipe
Material.It is chlorination Silver nanorod, mass content~92% in hollow lumen as shown in Fig. 4 (a)-(b).
Embodiment the result shows that, the present invention propose electric field power drive quick, controllable filling carbon nano-pipe hollow lumen in
Method, by using Novel electrolytic slot device, so that the positive and negative ion in solution is only capable of passing through anode under electric field power drive
Aluminium oxide nano duct is moved round about, realizes variety classes, different shape (nano particle or nanometer rods) substance in carbon
Controllable filling in nanotube hollow lumen, for pushing nano particle/nanometer rods filling carbon nano-pipe in electrochemical catalysis material
Material, energy storage material, in-situ nano reactor field basic and applied research have great importance.
Claims (10)
1. a kind of method in fast selective filling nanoparticle to carbon nanotubes lumen, which is characterized in that will be deposited with thin
The anodic alumina film of layer carbon is assembled on electrolytic cell assembly, and the electrolysis groove body of electrolytic cell assembly is separated into two by assembly
A independent electrolytic cell, is inserted into electrode in each electrolytic cell respectively, need to fill the electrolyte solution of element in electrolytic cell injection, in
Apply 1~50V DC voltage between two electrodes, fills nanoparticle 0.5 second to 5 minutes, remove anodic alumina film and carry out heat
After processing, anodic alumina film is removed, the composite structure of carbon nano tube of nano-particles filled is obtained；Wherein, anodic alumina film
The perforation nano pore for being 20~100nm with aperture.
2. the method in fast selective filling nanoparticle to carbon nanotubes lumen described in accordance with the claim 1, feature
Be, electrolytic cell assembly includes electrolysis groove body and assembly, electrolysis groove body setting electrode I, electrode II, sealing rubber strip I,
Organic sheet glass I, rubber gasket I, rubber gasket II, organic glass piece II, anode is arranged in sealing rubber strip II, assembly
Alumina wafer, specific structure are as follows:
Assembly is inserted into the groove of electrolysis groove body from top to bottom, and electrolysis groove body is by organic glass piece I, rubber gasket I, sun
Pole alumina wafer, rubber gasket II, organic glass piece II assembly be separated into two electrolytic cells: electrolytic cell I, electrolytic cell II,
Sealing rubber strip I is set at assembly and I cooperation of electrolytic cell, sealing rubber strip II is set at assembly and II cooperation of electrolytic cell,
Electrode I is inserted in electrolytic cell I, inserts electrode II in electrolytic cell II；After assembling, the filling device of nano particle is formed；
The anodic alumina film of carbon-coating cladding is clipped in the rubber gasket I of center opening, among rubber gasket II, carbon-coating cladding
Anodic alumina film it is identical as shape, the size of rubber gasket I, II center opening of rubber gasket, carbon-coating cladding sun
The center opening of rubber gasket I, rubber gasket II, organic glass piece I, organic glass piece II is completely covered in pole alumina wafer
It is clamped in rubber gasket I, II outside of rubber gasket, the side corresponding with rubber gasket II of organic glass piece II is symmetrically set
Fixed pin is set, pilot hole corresponding with fixed pin is opened up on rubber gasket I, rubber gasket II and organic glass piece I, it is organic
Sheet glass I, rubber gasket I, rubber gasket II, organic glass piece II are cooperated by fixed pin and pilot hole, form combination
Body.
3. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is that two electrodes: electrode I, electrode II are inert electrode, and when being powered, electrode plays electric action, without sending out with electrolyte
Raw reaction.
4. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is, of the same race or xenogenesis electrolyte solution is used in two electrolytic cells, molten when holding electrolyte not of the same race in two electrolytic cells
When liquid, two kinds of electrolyte and direction of an electric field are selected as needed, realize that nanoparticle is directly fast in carbon nanotube hollow lumen
Speed synthesis.
5. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is that the anodic alumina film of carbon-coating cladding uses other sheets, via material with similar structure to replace, and realizes nanometer
Fast Filling of the particle in various nanotubes or porous material nano pore.
6. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is that for heat treatment condition depending on required grain structure, atmosphere is one or both of air, argon gas, nitrogen, hydrogen
The above gaseous mixture, temperature are 50~1000 DEG C.
7. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is, the nanoparticle content in carbon nanotube by electrolyte solution concentration, apply voltage time accuracy controlling, nanoparticle
Sub- content controllable precise within the scope of 0.5~95wt%.
8. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2, special
Sign is that different-shape is presented with its changes of contents in nanoparticle, exists in granular form when content is lower, fills out when content is higher
The segment dislocation nanometer rods of full carbon nanotube.
9. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 8, feature
It is, nanoparticle content exists in granular form in 75wt% or less.
10. the method in fast selective filling nanoparticle to carbon nanotubes lumen according to claim 1 or 2,
It is characterized in that, since physical isolation of the anodised aluminium to carbon nanotube outer wall acts on, nanoparticle 100% is filled in carbon nanometer
In the hollow lumen of pipe.
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