CN106082166B - A kind of metal sulfide coated single-walled carbon nano tube nano-cable and its synthetic method - Google Patents
A kind of metal sulfide coated single-walled carbon nano tube nano-cable and its synthetic method Download PDFInfo
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- CN106082166B CN106082166B CN201610404733.0A CN201610404733A CN106082166B CN 106082166 B CN106082166 B CN 106082166B CN 201610404733 A CN201610404733 A CN 201610404733A CN 106082166 B CN106082166 B CN 106082166B
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- walled carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
A kind of metal sulfide coated single-walled carbon nano tube nano-cable and its synthetic method, are related to a kind of cable and its synthetic method, using chemical vapor deposition（CVD）The mode of thermal response method is in situ to be prepared；Suppressed by graphite, catalyst, containing growth promoter of sulfur, silica flour, metal powder or metallic compound powder；Using inert atmosphere as protective atmosphere and carrier gas, graphite, catalyst, containing growth promoter of sulfur, silica flour reaction generation single-walled carbon nanotube；Containing growth promoter of sulfur and metal powder or metallic compound powder reaction generation metal sulfide, single-walled carbon nanotube and metal sulfide cluster leave raw material surface, flow to low-temperature space；In the process, metal sulfide cluster is coated on single pipe surface.The cable has excellent photoelectrochemical property, and the core body of cable only has one or a few single-walled carbon nanotube composition, is beneficial to the performance of single-walled carbon nanotube nanoscale electrical effect, embodies more excellent new kink characteristics.
Description
Technical field
The present invention relates to a kind of cable and its synthetic method, more particularly to a kind of coated single-walled carbon nanometer of metal sulfide
Pipe nano-cable and its synthetic method.
Background technology
Single-walled carbon nanotube has unique electric property, this cause its can potential application in nanoelectronic, electrically conducting transparent
Among film, conductive polymer nanometer composite material.Metal sulfide is the semiconductor with one fixed width band gap, its nanostructured
It is applied to by extensive explore among photochemical catalyst, luminescence generated by light and sensor.Vulcanized using single-walled carbon nanotube as kernel, with metal
The advantages of thing can combine both for the nano cable structure of shell, so as to show some novel properties.
Single-walled carbon nanotube sample obtained by normal conditions is typically to exist in the form of tube bank, so, several existing
The preparation method using single-walled carbon nanotube as the nano-cable of core in, single-walled carbon nanotube is divided in the solution first
Dissipate, be separated into tube bank single, then the single effective inorganic material presoma of single is coated.Due to single wall
Carbon nano-tube bundle is scattered more difficult, adds the preparation difficulty of nano-cable, therefore electric as the nanometer of core using single-walled carbon nanotube at present
Cable structure is relatively limited.In addition, the scattered of single-walled carbon nanotube usually requires to be ultrasonically treated and add surfactant, this can not keep away
The meeting exempted from introduces defect and impurity to single-walled carbon nanotube, and then influences its intrinsic property.Researcher finds and uses one-step method
The method of nano-cable of the synthesis with complete single-walled carbon nanotube kernel.Zeng You researcher is directly closed by hydrogen arc method
Into the nano cable structure of amorphous silicon oxide coated single-walled carbon nano tube, this shows that directly synthesis contains single-walled carbon nanotube
Nano-cable be feasible.
The content of the invention
It is an object of the invention to provide a kind of metal sulfide coated single-walled carbon nano tube nano-cable and its synthesis side
Method, the present invention directly synthesize metal sulfide coated single-walled carbon nano tube nano-cable, and metal sulfide is with one fixed width
The semiconductor of band gap, there is excellent photoelectrochemical property；Be advantageous to the performance of single-walled carbon nanotube nanoscale electrical effect；Should
Nano cable structure will combine the excellent specific property of two kinds of materials of shell core, embody more excellent new kink characteristics.
The purpose of the present invention is achieved through the following technical solutions：
A kind of metal sulfide coated single-walled carbon nano tube nano-cable, the cable raw material are graphite, catalyst, sulfur-bearing
Growth promoter, silica flour, metal powder or metallic compound powder, metal sulfide cluster are coated on single pipe surface, shape
Into nano-cable；Catalyst is iron, the mixing of the one or more of cobalt, nickel transition element, addition 0.01-40.0
wt.%；Addition containing growth promoter of sulfur is 0.01-30.0 wt.%；The addition of silica flour is 0-40.0 wt.%；Metal powder
Or metallic compound powder addition is 0.005-30.0 wt.%；Surplus is graphite.
A kind of metal sulfide coated single-walled carbon nano tube nano-cable synthetic method, methods described include preparing as follows
Journey：Using chemical vapor deposition（CVD）The mode of thermal response method is in situ to be prepared；By graphite, catalyst, containing growth promoter of sulfur,
Silica flour, metal powder or the compacting of metallic compound powder；Using inert atmosphere as protective atmosphere and carrier gas；At a temperature of control, stone
Ink, catalyst, containing growth promoter of sulfur, silica flour reaction generation single-walled carbon nanotube；Containing growth promoter of sulfur and metal powder or gold
Belong to compound powder reaction generation metal sulfide；Under the carrier gas effect of inert atmosphere, single-walled carbon nanotube and metal sulfide
Cluster leaves raw material surface, flows to low-temperature space；In the process, metal sulfide cluster is coated on single pipe surface,
It is prepared into nano-cable.
A kind of described metal sulfide coated single-walled carbon nano tube nano-cable synthetic method, the inert atmosphere are
Ar、N2、He、H2One or several mixing of atmosphere, flow is 5-2000 ml/min.
A kind of described metal sulfide coated single-walled carbon nano tube nano-cable synthetic method, the heating rate are 2-
50 °C/min, between reaction temperature is 600-1300 °C, the reaction time is 0.1-10 h.
Advantages of the present invention is with effect：
1. the present invention by graphite, catalyst, containing growth promoter of sulfur, metal powder（Or metallic compound powder）Steamed altogether Deng raw material
Hair, original position, the growth of single-walled carbon nanotube and the cladding of metal sulfide are synchronously completed, technical process is simple；
2. present invention, avoiding physical and chemical processes such as purifying, ultrasonic disperse, electrochemical deposition, organic media bondings to list
The structure of wall carbon nano tube and the influence of electrical property；
3. the nano-cable that the present invention obtains is discrete, navigability is strong.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of synthesized metal sulfide coated single-walled carbon nano tube nano-cable in embodiment one
（a）、（b）With transmission electron microscope photo（c）、（d）.
Fig. 2 is the stereoscan photograph of synthesized metal sulfide coated single-walled carbon nano tube nano-cable in embodiment two
（a）、（b）.
Fig. 3 is the stereoscan photograph of synthesized metal sulfide coated single-walled carbon nano tube nano-cable in embodiment three
（a）、（b）.
Embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment one
The mixed-powder of graphite, 5.0 wt.% catalyst, 2.0 wt.% growth promoters and 0.2 wt.% zinc powders is suppressed
Into a round material, it is put in porcelain boat, is placed in the center flat-temperature zone of chemical vapor deposition stove.Using argon gas as protective atmosphere and load
Gas, flow are 50 ml/min.1000 °C are risen to 10 °C/min heating rate, is incubated 1 h, then Temperature fall.Gained produces
Thing characterization result is as shown in Figure 1.The length of the nano-cable grown under this preparation condition is several to tens microns, and diameter is about
For 120 nm, for the radical of cable core SWNT between 1-5, the outer shell of cable is continuous, the external coating of cable
For polycrystalline zinc sulphide.
Embodiment two
By graphite, 10.0 wt.% catalyst, 4.0 wt.% growth promoters, 1.0 wt.% silica flours and 1.0 wt.% zinc
The mixed-powder of powder is pressed into a round material, is put in porcelain boat, is placed in the center flat-temperature zone of chemical vapor deposition stove.With helium
Gas is protective atmosphere and carrier gas, and flow is 100 ml/min.900 °C are risen to 10 °C/min heating rate, is incubated 0.5 h,
Then Temperature fall.Products therefrom characterization result is as shown in Figure 2.The length of the nano-cable grown under this preparation condition is several
Individual to tens microns, diameter is about 200 nm, and the radical of cable core SWNT is between 1-5, the outer shell of cable
It is made up of multiple nanocrystals, the external coating of cable is polycrystalline zinc sulphide.
Embodiment three
By graphite, 20.0 wt.% catalyst, 8.0 at.% growth promoters, 2.0 wt.% silica flours and 2.0 wt.% oxygen
The mixed-powder for changing zinc powder is pressed into a round material, is put in porcelain boat, is placed in the center flat-temperature zone of chemical vapor deposition stove.
Using nitrogen as protective atmosphere and carrier gas, flow is 120 ml/min.1000 °C are risen to 10 °C/min heating rate, insulation
1.2 h, then Temperature fall.Products therefrom characterization result is as shown in Figure 3.The length of the nano-cable grown under this preparation condition
Spend for tens microns, diameter is about 400 nm, and the radical of cable core SWNT is between 1-5, the outer shell of cable
Continuously, the external coating of cable is polycrystalline zinc sulphide.
Claims (1)
1. a kind of metal sulfide coated single-walled carbon nano tube nano-cable synthetic method, it is characterised in that methods described includes
Following preparation process：Using chemical vapor deposition（CVD）The mode of thermal response method is in situ to be prepared；By graphite, catalyst, sulfur-bearing life
Long accelerator, silica flour, metal powder or the compacting of metallic compound powder；Using inert atmosphere as protective atmosphere and carrier gas；Controlling
At a temperature of, graphite, catalyst, containing growth promoter of sulfur, silica flour reaction generation single-walled carbon nanotube；Containing growth promoter of sulfur and gold
Belong to powder or metallic compound powder reaction generation metal sulfide；Under the carrier gas effect of inert atmosphere, single-walled carbon nanotube and gold
Category sulfide cluster leaves raw material surface, flows to low-temperature space；In the process, metal sulfide cluster is coated on single
Pipe surface, it is prepared into nano-cable；
The inert atmosphere is Ar, N2、He、H2One or several mixing of atmosphere, flow is 5-2000 ml/min；
Heating rate is 2-50 DEG C/min, and between reaction temperature is 600-1300 DEG C, the reaction time is 0.1-10 h；
The catalyst is iron, the mixing of the one or more of cobalt, nickel transition element, addition 0.01-40.0
wt.%；Addition containing growth promoter of sulfur is 0.01-30.0 wt.%；The addition of silica flour is 0-40.0 wt.%；Metal powder
Or metallic compound powder addition is 0.005-30.0 wt.%；Surplus is graphite.
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| AUPQ065099A0 (en) * | 1999-05-28 | 1999-06-24 | Commonwealth Scientific And Industrial Research Organisation | Substrate-supported aligned carbon nanotube films |
| CN100455508C (en) * | 2007-03-29 | 2009-01-28 | 浙江大学 | Method for producing Nano carbon tube clad by metallic sulfide |
| CN100549106C (en) * | 2007-10-23 | 2009-10-14 | 浙江大学 | A kind of method for preparing nano ZnS coated carbon nano-tube |
| CN101513997B (en) * | 2008-02-20 | 2011-04-20 | 中国科学院金属研究所 | Method for synthesizing nano cable structure of silica-coated single-walled carbon nano tube |
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