CN101513997B - Method for synthesizing nano cable structure of silica-coated single-walled carbon nano tube - Google Patents
Method for synthesizing nano cable structure of silica-coated single-walled carbon nano tube Download PDFInfo
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- CN101513997B CN101513997B CN2008100104448A CN200810010444A CN101513997B CN 101513997 B CN101513997 B CN 101513997B CN 2008100104448 A CN2008100104448 A CN 2008100104448A CN 200810010444 A CN200810010444 A CN 200810010444A CN 101513997 B CN101513997 B CN 101513997B
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Abstract
The invention relates to synthesis technology of nano cable, and in particular provides a preparation method for synthesizing the nano cable structure of the amorphous silica-coated single-walled carbon nano tube by an arc discharge method. The preparation method comprises the following steps: adopting a cathode and anode DC arc discharge mode to realize in-situ preparation; the anode is a consumptive anode formed by pressing graphite, silicon powder, catalyst and growth promoter; after arc starting discharge, carrying out coevaporation of raw materials including the graphite, the silicon powder, the catalyst and the growth promoter; and completing in-situ synthesis of the nano cable structure of one or more silica-coated single-walled carbon nano tubes. Silica has the characteristics of good thermal stability, high dielectric constant, small drain current and high compressive strength, and the like. and is an ideal material of insulation layers used in nano devices such as the nano cable and a field effect transistor; in addition, a core body of the developed nano cable consists of one or more single-walled carbon nano tubes, which is favorable for bringing into playing the nano size effect of the single-walled carbon nano tube and improving the performances such as efficiency and sensitivity of a fabricated nano device.
Description
Technical field
The present invention relates to the synthetic technology of nano-cable, the preparation method of the synthetic amorphous silicon oxide coated single-walled carbon nano tube nano cable structure of a kind of arc discharge method original position is provided especially.
Background technology
Along with the quick microminiaturization and the Highgrade integration of electron device, the unitary research of package technique and related device from bottom to top receives very big concern.Wherein carbon nanotube-based nano-cable is because of having particular structure feature, excellent physicochemical property and good practicality, as good stability, easily handle, can make up field-effect transistor and logical circuit etc., so caused scientist's very big research enthusiasm.
The main preparation methods of having reported carbon nanotube-based nano-cable is: be immersed in the outer shell precursor solution after carbon nanotube is disperseed, thermal treatment that process is suitable or chemical treatment realize the coating of carbon pipe again.It is better that this method prepares the effect of multi-walled carbon nano-tubes base nano-cable.And Single Walled Carbon Nanotube is assembled bunchy usually under the effect of Van der Waals force, does not also have good way to make its homodisperse at present.So utilize nano-cable core body that above method prepares usually by the tube bank that comprises many Single Walled Carbon Nanotube, this has limited the performance of Single Walled Carbon Nanotube nanoscale effect and the application in nano-device thereof.There is scientist on silicon substrate, to prepare isolating single Single Walled Carbon Nanotube, obtains nano-cable at its surface selectivity deposition coating layer afterwards.This method has been avoided the scattering problem of Single Walled Carbon Nanotube, but owing to be to deposit outer material at the upper surface that carries carbon pipe substrate, the nanostructure that obtains not is proper coaxial nano cable; And the chemical process that this method relates to can produce certain influence to the electronic structure of carbon pipe; In addition, the nanostructure deposition that obtains on substrate, to its move, the difficulty of operation such as assembling is bigger.
Summary of the invention
The arc discharge method that the purpose of this invention is to provide a kind of direct synthetic silica coated single-walled carbon nano tube nano cable structure.Silicon oxide has characteristics such as Heat stability is good, specific inductivity height, leakage current are little, compressive strength height, is the ideal material of insulation layer in the nano-devices such as nano-cable and field effect transistor; In addition, the core body of the nano-cable of developing only is made of one or a few Single Walled Carbon Nanotube, will help the performance of Single Walled Carbon Nanotube nanoscale effect and improve the efficient of constructed nano-device and performance such as sensitivity.
Technical scheme of the present invention is:
The invention provides a kind of arc discharge method of direct synthetic silica coated single-walled carbon nano tube nano cable structure, adopt the mode of cathode and anode arc-over under pressure atmosphere; Negative electrode is a graphite rod that diameter is 10mm, the sacrificial anode of anode for forming by graphite, silica flour, catalyzer, growth stimulant compacting, in the anode material: one or more mixing of catalyzer chosen from Fe, cobalt, nickel, add-on are 1.0-10.0at.%; Iron sulphide is cooked growth stimulant, and add-on is 0.1-4.0at.%; The add-on of silica flour is 2at.%-7at.%; Surplus is a graphite; Buffer gas 50-500Torr hydrogen; Galvanic current 30-200A; After playing arc discharge, raw material coevaporations such as graphite, silica flour, catalyzer, growth stimulant, carbon atom is separated out on the surface of catalyzer, structural rearrangement forms CNT (carbon nano-tube) (growth stimulant plays and enlarges the effect that CNT (carbon nano-tube) continues growth temperature range); Meanwhile, Siliciumatom is by dioxygen oxidation residual in the cavity, and for reducing surface energy, the silicon oxide of generation has promptly formed the construction of cable of silica-coated single-walled CNT (carbon nano-tube) attached to the surface of carbon pipe.
In the arc discharge method of nano cable structure of silica-coated single-walled carbon nano tube of the present invention, in the anode material, the granularity of silica flour is 200 orders; The granularity of graphite is 200 orders; The granularity of catalyzer is iron 100 orders, cobalt 100 orders, nickel 100 orders; The granularity of growth stimulant is 200 orders.
In the arc discharge method of nano cable structure of silica-coated single-walled carbon nano tube of the present invention, become 20～90 ° angle between described negative electrode and anode, negative electrode and positive interpolar shortest distance are 0.5～2mm.
Negative electrode adopts graphite rod or other conductive carbon material among the present invention.
The nano cable structure of silica-coated single-walled carbon nano tube and the technical parameter scope that adopt the present invention to obtain are: cable core is Single Walled Carbon Nanotube (a 1-5 root); The coating of cable is the SiO of amorphous state
X(
X≤ 2); Cable size is 20～100nm, and length is that tens nanometer is to tens of microns.
The arc discharge method of nano cable structure of silica-coated single-walled carbon nano tube of the present invention has following advantage:
(1) the present invention is raw material coevaporations such as graphite, silica flour, catalyzer, and original position, growth and the silicon oxide of finishing carbon nanotube synchronously coat, and technological process is simple;
(2) the present invention has avoided physical and chemical processes such as purifying, ultra-sonic dispersion, electrochemical deposition, organic medium bonding to the structure of Single Walled Carbon Nanotube and the influence of electrical property;
(3) nano-cable that obtains of the present invention is discrete, and manipulative capability is strong.
Description of drawings
Fig. 1. the stereoscan photograph (a) and (b) of institute's synthetic silica coated single-walled carbon nano tube nano-cable and transmission electron microscope photo (c), (d), (e) among the embodiment one.
Fig. 2. the stereoscan photograph (a) and (b) of institute's synthetic silica coated single-walled carbon nano tube nano-cable among the embodiment two.
Fig. 3. the stereoscan photograph (a) and (b) of institute's synthetic silica coated single-walled carbon nano tube nano-cable among the embodiment three.
Embodiment
Embodiment one
The powder mix of the iron sulphide growth stimulant of graphite, 2.0at.% silica flour, 2.0at.% catalyzer (mol ratio: Fe: Co: Ni=1: 1: 5) and 0.1at.% is put into anode graphite disk hole and compacting, negative electrode is a graphite rod, charge into 100Torr hydrogen in the reactor, striking current is the 120A direct current, the shortest distance of two interpolar maintenance～2mm and～30 ° of angles.The products therefrom characterization result as shown in Figure 1.This preparation condition length of the nano-cable of growth down is several to tens microns, and diameter is about 20nm, and the radical of cable core Single Walled Carbon Nanotube is between 1-5, and the outer shell of cable is continuous, and the coating of cable is the SiO of amorphous state
X(
X≤ 2).
Embodiment two
The powder mix of the iron sulphide growth stimulant of graphite, 5.0at.% silica flour, 4.0at.% catalyzer (mol ratio: Fe: Co: Ni=1: 1.5: 5) and 4.0at.% is put into anode graphite disk hole and compacting, negative electrode is a graphite rod, charge into 500Torr hydrogen in the reactor, striking current is the 200A direct current, the shortest distance of two interpolar maintenance～2mm and～40 ° of angles.The products therefrom characterization result as shown in Figure 2.This preparation condition length of the nano-cable of growth down is tens microns, and diameter is between 20-50nm.The cable jacket layer is discontinuous, as seen exposes the Single Walled Carbon Nanotube of core, cable core be Single Walled Carbon Nanotube between the 1-5 root, the coating of cable is the SiO of amorphous state
X(
X≤ 2).
Embodiment three
The powder mix of the iron sulphide growth stimulant of graphite, 7.0at.% silica flour, 10.0at.% catalyzer (mol ratio: Fe: Co: Ni=1: 2: 5) and 1.0at.% is put into anode graphite disk hole and compacting, negative electrode is a graphite rod, charge into 50Torr hydrogen in the reactor, striking current is the 30A direct current, the shortest distance of two interpolar maintenance～2mm and～60 ° of angles.The products therefrom characterization result as shown in Figure 3.This preparation condition length of the nano-cable of growth down is several microns, diameter 50-100nm, and have bifurcation along diametric(al) usually, be dendroid more, cable core be Single Walled Carbon Nanotube between the 1-5 root, the coating of cable is the SiO of amorphous state
X(
X≤ 2).
Experiment shows that the catalyzer among the present invention can adopt one or more mixing of transition elements such as iron, cobalt, nickel.
Claims (2)
1. the synthetic method of a nano cable structure of silica-coated single-walled carbon nano tube is characterized in that: adopt the mode in-situ preparing of cathode and anode direct current arc discharge, negative electrode is a graphite rod that diameter is 10mm; The sacrificial anode of anode for forming by graphite, silica flour, catalyzer, growth stimulant compacting, in the anode material: one or more mixing of catalyzer chosen from Fe, cobalt, nickel, add-on are 1.0-10.0at.%; Iron sulphide is cooked growth stimulant, and add-on is 0.1-4.0at.%; The add-on of silica flour is 2at.%-7at.%; Surplus is a graphite; Buffer gas is a 50-500Torr hydrogen, and galvanic current is 30-200A, after the arc discharge, and graphite, silica flour, catalyzer, growth stimulant raw material coevaporation, original position synthesizes silicon oxide and coats one or a few Single Walled Carbon Nanotube nano cable structure.
2. according to the described preparation method of claim 1, it is characterized in that: become 20～90 ° angle between described negative electrode and anode, negative electrode and positive interpolar shortest distance are 0.5～2mm.
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| CN2008100104448A CN101513997B (en) | 2008-02-20 | 2008-02-20 | Method for synthesizing nano cable structure of silica-coated single-walled carbon nano tube |
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| CN101513997B true CN101513997B (en) | 2011-04-20 |
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| CN102530917A (en) * | 2012-01-09 | 2012-07-04 | 中国科学院金属研究所 | Method for preparing carbon nanotube structure with sharp end socket |
| CN105836749A (en) * | 2016-04-01 | 2016-08-10 | 山东容奈材料设计有限公司 | Modification method for white carbon black and application of modified white carbon black |
| CN106082166B (en) * | 2016-06-12 | 2018-01-16 | 沈阳化工大学 | A kind of metal sulfide coated single-walled carbon nano tube nano-cable and its synthetic method |
| EP4009400B1 (en) | 2019-09-30 | 2024-01-31 | Lg Energy Solution, Ltd. | Composite anode active material, preparation method therefor, and anode comprising same |
| CN112538596A (en) * | 2020-05-08 | 2021-03-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nano tube-metal composite conductor and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020031465A1 (en) * | 1998-07-21 | 2002-03-14 | Yahachi Saito | Production of carbon nanotube |
| CN1463918A (en) * | 2002-06-06 | 2003-12-31 | 中国科学院金属研究所 | Process for preparing single wall nano carbon tube |
| CN1743265A (en) * | 2004-08-31 | 2006-03-08 | 中国科学院金属研究所 | A kind of low-cost preparation method of double-wall carbon nano-tube |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020031465A1 (en) * | 1998-07-21 | 2002-03-14 | Yahachi Saito | Production of carbon nanotube |
| CN1463918A (en) * | 2002-06-06 | 2003-12-31 | 中国科学院金属研究所 | Process for preparing single wall nano carbon tube |
| CN1743265A (en) * | 2004-08-31 | 2006-03-08 | 中国科学院金属研究所 | A kind of low-cost preparation method of double-wall carbon nano-tube |
Non-Patent Citations (1)
| Title |
|---|
| 张爱霞等.一维碳化硅纳米材料的研究进展.《材料导报》.2006,第20卷106-108. * |
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