CN1147427C - Process for synthesizing nm carbon tubes containing nm metal wires - Google Patents
Process for synthesizing nm carbon tubes containing nm metal wiresInfo
- Publication number
- CN1147427C CN1147427C CNB991206584A CN99120658A CN1147427C CN 1147427 C CN1147427 C CN 1147427C CN B991206584 A CNB991206584 A CN B991206584A CN 99120658 A CN99120658 A CN 99120658A CN 1147427 C CN1147427 C CN 1147427C
- Authority
- CN
- China
- Prior art keywords
- anode
- carbon nanotube
- hydrochloric acid
- electrochemical deposition
- multiaperture pellumina
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002184 metal Substances 0.000 title claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims description 5
- 229910052799 carbon Inorganic materials 0.000 title abstract description 6
- 230000002194 synthesizing effect Effects 0.000 title description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 41
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 41
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000004070 electrodeposition Methods 0.000 claims abstract description 24
- -1 paratoluenesulfonic acid ammonium salt Chemical class 0.000 claims abstract description 18
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 12
- 239000004332 silver Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000010189 synthetic method Methods 0.000 claims abstract description 12
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 3
- 150000003839 salts Chemical class 0.000 claims abstract 2
- 238000001354 calcination Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 10
- 239000002070 nanowire Substances 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000009713 electroplating Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 27
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- 239000012298 atmosphere Substances 0.000 description 14
- 229910001873 dinitrogen Inorganic materials 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 230000035484 reaction time Effects 0.000 description 9
- CODVACFVSVNQPY-UHFFFAOYSA-N [Co].[C] Chemical compound [Co].[C] CODVACFVSVNQPY-UHFFFAOYSA-N 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 4
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005087 graphitization Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
Images
Abstract
The present invention relates to a synthetic method of carbon nanometer tubes containing iron group metal nanometer wires. In the synthetic method, a porous alumina film with an anode is immersed into the mixed solution of aniline, paratoluenesulfonic acid ammonium salt, ammonium metavanadate and hydrochloric acid to make polymerization reaction under a nitrogen atmosphere; then, silver slurry is coated on the porous alumina film with an anode to be baked as a cathode of electrochemical deposition reaction; the iron group metal nanometer wires which need to be deposited are used as anodes; iron group metal salt is allocated into electroplating solution for making electrochemical deposition; finally, the carbon nanometer tubes containing the iron group metal nanometer wires are obtained by burning in 600 to 1000 DEG C under an argon atmosphere. The length of the carbon nanotubes is 50 mu m, and the diameter is 30 to 150 nm.
Description
Technical field
The present invention relates to comprise the synthetic method of metal nanometer line carbon nanotube.
Background technology
Carbon nanotube has caused material supply section scholars' very big interest since 1991 are synthesized.So far existing several different methods attempts inserting metal or other metallic compounds to obtain nano composite material in carbon nanotube.People such as P.M.Ajayan utilize wicking action that liquid lead is inserted in the carbon nanotube, and people such as S.C.Tsang provide a kind of wet-chemical technique synthetic a series of metal oxide compounds in carbon nanotube.Human arc discharge methods such as C.Guerret-Plecourt are synthetic 15 kinds of metals and/or other compounds in carbon nanotube.People such as nearest B.K.Pradhan adopt MOCVD method synthetic metal nanometer line in alumina formwork.All these methods all are first synthesizing carbon nanotubes, insert metal or other compounds again in carbon nanotube.Earlier synthetic carbon pipe, its graphitization temperature is higher, generally all more than 1200 ℃.
Summary of the invention
The object of the present invention is to provide a kind of easy graphitization temperature in the synthetic method that comprises the metal nanometer line carbon nanotube below 1200 ℃.
The technical scheme of synthetic method of the present invention is as follows:
A kind of synthetic method that comprises Ferrious material nano wire carbon nanotube, it is made up of the following step:
A. under nitrogen atmosphere, the immersion of anode multiaperture pellumina is contained in the mixing solutions of aniline, paratoluenesulfonic acid sodium salt, ammonium meta-vanadate and hydrochloric acid, at room temperature carry out polyreaction;
B. anode porous pellumina after the step a polyreaction is simultaneously coated silver slurry, oven dry, as the negative electrode of electrochemical deposition reaction, with required sedimentary Ferrious material, iron, cobalt, nickel, wire becomes electroplate liquid to carry out electrochemical deposition Ferrious material hydrochloric acid as anode;
C. the pellumina that step b is deposited metal is under argon atmospher, and in 600-1000 ℃ of temperature range, the normal pressure calcination promptly gets and comprises Ferrious material nano wire carbon nanotube.
To contain the mixing solutions of aniline, paratoluenesulfonic acid sodium salt, ammonium meta-vanadate and hydrochloric acid can be isopyknic hydrochloric acid soln that contains aniline and the hydrochloric acid soln mixed preparing that contains paratoluenesulfonic acid sodium salt and ammonium meta-vanadate to step a in the above-mentioned synthetic method.The hydrochloric acid soln that contains aniline is that concentration is the 1M hydrochloric acid soln of 0.3-0.6M aniline, and the hydrochloric acid soln that contains paratoluenesulfonic acid sodium salt and ammonium meta-vanadate is the 1M hydrochloric acid soln that concentration is respectively 0.5-0.8M paratoluenesulfonic acid sodium salt and 0.12-0.14M ammonium meta-vanadate.
To comprise nickel nano wire carbon nanotube electroplate liquid can be (NH to step b for synthetic in the above-mentioned synthetic method
4)
2SO
47H
2O270-300g/L, NiCl
26H
2O40-60g/LH
3BO
3The solution that 35-40g/L forms; To comprise cobalt nanowire carbon nanotube electroplate liquid can be CoSO for synthetic
47H
2O250-266g/LH
3BO
3The solution that 40-50g/L forms; To comprise Fe nanowire carbon nanotube plating bath can be FeSO for synthetic
47H
2O120-140g/L, H
3BO
345-50g/L, the solution that xitix 1g/L forms.
Simple synthetic method of the present invention, graphitization temperature are below 1200 ℃, and the Ferrious material nano wire carbon nanotube that comprises that synthesizes is about 50 μ m, and diameter 30-150nm is determined by anode porous alumina membrane pore size.
Description of drawings
Fig. 1 be embodiment 1 comprise nickel nano wire carbon nanotube with the molten electron scanning micrograph that goes behind the anode multiaperture pellumina of NaOH, a is a sectional drawing; B is a vertical view.
Fig. 2 be embodiment 1 comprise molten Raman spectrogram behind the anode multiaperture pellumina, the thing phase of alleged occurrence carbon of going of nickel nano wire carbon nanotube.
Fig. 3 be embodiment 1 comprise the molten x-ray diffraction pattern that goes behind the anode multiaperture pellumina of nickel nano wire carbon nanotube, the thing phase of alleged occurrence nickel.
Fig. 4 be embodiment 1 comprise the molten magnetic hysteresis loop figure that goes behind the anode multiaperture pellumina of nickel nano wire carbon nanotube part, anode porous alumina membrane plane and externally-applied magnetic field direction are 0 °, coercive force is respectively 92.19O when 45 ° and 90 °
e, 158.3O
eAnd 149.2O
e
Fig. 5 be embodiment 2 comprise the molten magnetic hysteresis loop figure that goes behind the anode multiaperture pellumina of nickel nano wire carbon nanotube part, anode porous alumina membrane plane becomes 0 ° with the externally-applied magnetic field direction, coercive force is respectively 86.85O when 45 ° and 90 °
e, 126.5O
eAnd 125.5O
e
Embodiment
Further specify the present invention by the following examples.
Example 1: comprise the nickel carbon nanotube.
--with the aperture is that 20nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Ni wire as anode, with (NH as the negative electrode of electrochemical deposition reaction
4)
2SO
47H
2O270g/l, NiCl
26H
2O40g/l, H
3BO
340g/l solution carried out electrochemical deposition 10 hours as the electroplate liquid of Ni;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, and then under Ar atmosphere, the temperature rise rate of 5 ℃/min was 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 20nm is a template institute synthetic nickel coat carbon nanotube.
Example 2: comprise the nickel carbon nanotube.
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Ni wire as anode, with (NH as the negative electrode of electrochemical deposition reaction
4)
2SO
47H
2O270g/l, NiCl
26H
2O40g/l, H
3BO
340g/l solution carried out electrochemical deposition 10 hours as the electroplate liquid of Ni;
--the temperature rise rate by 5 ℃/min, 250 ℃ of calcinations 30 minutes, continue the temperature rise rate with 5 ℃/min, then 600 ℃ of temperature section calcinations 30 minutes;
--naturally cool to room temperature.The anode multiaperture pellumina that gets 100nm is that template institute synthetic nickel coat carbon is received
Example 3: comprise the nickel carbon nanotube.
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Ni wire as anode, with (NH as the negative electrode of electrochemical deposition reaction
4)
2SO
47H
2O300g/l, NiCl
26H
2O60g/l, H
3BO
335g/l solution carries out electrochemical deposition about 10 hours as the electroplate liquid of Ni;
--the temperature rise rate by 5 ℃/min, 250 ℃ of calcinations 30 minutes, continue the temperature rise rate with 5 ℃/min, then 650 ℃ of temperature section calcinations 30 minutes;
--naturally cool to room temperature.The anode multiaperture pellumina that gets 100nm is that template institute synthetic comprises the nickel carbon nanotube.
Example 4: comprise the cobalt carbon nanotube.
--with the aperture is that 20nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Co wire as anode, with CoSO as the negative electrode of electrochemical deposition reaction
47H
2O266g/l, H
3BO
340g/l, solution carried out electrochemical deposition 20 hours as the electroplate liquid of Co;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 20nm is a template institute synthetic bag cobalt carbon nanotube.
Example 5: comprise the cobalt carbon nanotube.
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Co wire as anode, with CoSO as the negative electrode of electrochemical deposition reaction
47H
2O266g/l, H
3BO
340g/l solution carried out electrochemical deposition 20 hours as the electroplate liquid of Co;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 100nm is a template institute synthetic bag cobalt carbon nanotube.
Example 6: comprise the cobalt carbon nanotube.
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Co wire as anode, with CoSO as the negative electrode of electrochemical deposition reaction
47H
2O250g/l, H
3BO
350g/l solution carried out electrochemical deposition 20 hours as the electroplate liquid of Co;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 100nm is a template institute synthetic bag cobalt carbon nanotube.
Example 7: comprise the iron carbon nanotube.
--with the aperture is that the immersion of 20nm anode multiaperture pellumina contains 0.3M aniline, and 1M hydrochloric acid 10ml solution and 0.5M paratoluenesulfonic acid sodium salt in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Fe wire as anode, with FeSO as the negative electrode of electrochemical deposition reaction
47H
2O140g/l, H
3BO
350g/l, xitix 1g/l, solution carried out electrochemical deposition 20 hours as the electroplate liquid of Fe;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 20nm is a template institute synthetic iron clad carbon nanotube.
Example 8: comprise the iron carbon nanotube
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.6M aniline, 1M hydrochloric acid 10ml solution with contain the 0.8M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.14M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Fe wire as anode, with FeSO as the negative electrode of electrochemical deposition reaction
47H
2O140g/l, H
3BO
350g/l, xitix 1g/l, solution carried out electrochemical deposition 20 hours as the electroplate liquid of Fe;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 900 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 100nm is a template institute synthetic iron clad carbon nanotube.
Example 9: comprise the iron carbon nanotube.
--with the aperture is that 100nm anode multiaperture pellumina immerses and to contain 0.3M aniline, 1M hydrochloric acid 10ml solution with contain the 0.5M paratoluenesulfonic acid sodium salt, in the mixing solutions that 0.12M ammonium meta-vanadate and 1M hydrochloric acid soln 10ml are formed, carry out polyreaction at ambient temperature.This is reflected at before the reaction and leads to nitrogen in the reaction process all the time, to remove air, this is reflected under the condition of nitrogen gas carries out.Reaction times was about about 1.5 hours;
--the anode multiaperture pellumina after the above-mentioned polyreaction is simultaneously coated the silver slurry, under infrared lamp, dry,, use the Fe wire as anode, with FeSO as the negative electrode of electrochemical deposition reaction
47H
2O120g/l, H
3BO
345g/l, xitix 1g/l solution carried out electrochemical deposition 20 hours as the electroplate liquid of Fe;
--by the temperature rise rate of 5 ℃/min, 250 ℃ of calcinations 30 minutes, again under Ar atmosphere 650 ℃ of temperature section calcinations 30 minutes;
--under Ar atmosphere, normal pressure is cooled to room temperature.The anode multiaperture pellumina that gets 100nm is a template institute synthetic iron clad carbon nanotube.
Claims (3)
1. synthetic method that comprises the metal nanometer line carbon nanotube is characterized in that being made up of the following step:
A. under nitrogen atmosphere, the immersion of anode multiaperture pellumina is contained aniline, paratoluenesulfonic acid sodium salt, in the mixing solutions of ammonium meta-vanadate and hydrochloric acid, at room temperature carry out polyreaction, above-mentioned mixing solutions is to be that the 1M hydrochloric acid soln of aniline of 0.3～0.6M and the 1M hydrochloric acid soln mixed preparing that concentration is 0.5～0.8M paratoluenesulfonic acid sodium salt and 0.12～0.14M ammonium meta-vanadate form by isopyknic concentration;
B. the anode multiaperture pellumina after the step a polyreaction is simultaneously coated the silver slurry, oven dry, the negative electrode as the electrochemical deposition reaction as anode, is made into required sedimentary Ferrious material silk electroplate liquid with Ferrious material salt and carries out electrochemical deposition;
C. the anode multiaperture pellumina that step b is deposited metal is under argon atmospher, and in 600-1000 ℃ of temperature range, the normal pressure calcination promptly gets and comprises Ferrious material nano wire carbon nanotube.
2. method according to claim 1 is characterized in that synthetic containing the cobalt nanowire carbon nanotube, and its electroplate liquid is CoSO
47H
2O250-266g/l, H
3BO
3The solution that 40-50g/l forms.
3. synthetic method according to claim 1 is characterized in that synthetic comprising the Fe nanowire carbon nanotube, and its electroplate liquid is FeSO
47H
2O120-140g/l, H
3BO
345-50/gl, the solution that xitix 1g/l forms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB991206584A CN1147427C (en) | 1999-12-22 | 1999-12-22 | Process for synthesizing nm carbon tubes containing nm metal wires |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB991206584A CN1147427C (en) | 1999-12-22 | 1999-12-22 | Process for synthesizing nm carbon tubes containing nm metal wires |
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|---|---|
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| CN1147427C true CN1147427C (en) | 2004-04-28 |
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| CNB991206584A Expired - Fee Related CN1147427C (en) | 1999-12-22 | 1999-12-22 | Process for synthesizing nm carbon tubes containing nm metal wires |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165469B (en) * | 2006-10-19 | 2012-11-14 | 河南师范大学 | Protein coated silver sulfide nano line preparation method |
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|---|---|---|---|---|
| CN100390046C (en) * | 2004-12-17 | 2008-05-28 | 清华大学 | Synthesis method of iron nanotube array |
| CN102650077A (en) * | 2011-02-24 | 2012-08-29 | 中国科学院合肥物质科学研究院 | Chitosan-finishing iron nanowire, method for producing same and application thereof |
| CN102205957B (en) * | 2011-04-07 | 2012-10-31 | 上海大学 | Method for generating carbon chain in multi-wall carbon nanotube |
| CN103342352B (en) * | 2013-07-24 | 2015-01-14 | 中国科学院合肥物质科学研究院 | Carbon nano bottle containing nickel nano particles and method for preparing carbon nano bottle |
| CN104528867B (en) * | 2014-12-25 | 2016-04-06 | 东华大学 | A kind of preparation method of carbon nanotube compound ferric vandate green deep water conditioner |
| CN104846411B (en) * | 2015-04-27 | 2017-08-25 | 北京航空航天大学 | The method and its product of flower-like nanometer metal cobalt are prepared using anodic oxidation aluminium formwork |
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1999
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101165469B (en) * | 2006-10-19 | 2012-11-14 | 河南师范大学 | Protein coated silver sulfide nano line preparation method |
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| CN1300713A (en) | 2001-06-27 |
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