CN1300713A - Process for synthesizing nm carbon tubes containing nm metal wires - Google Patents
Process for synthesizing nm carbon tubes containing nm metal wires Download PDFInfo
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- CN1300713A CN1300713A CN99120658.4A CN99120658A CN1300713A CN 1300713 A CN1300713 A CN 1300713A CN 99120658 A CN99120658 A CN 99120658A CN 1300713 A CN1300713 A CN 1300713A
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- hydrochloric acid
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- carbon nanotube
- aniline
- vanadate
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- 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 14
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 title abstract description 5
- 230000002194 synthesizing effect Effects 0.000 title abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 72
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 239000002002 slurry Substances 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
- 239000002041 carbon nanotube Substances 0.000 claims description 42
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 42
- 238000004070 electrodeposition Methods 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 20
- -1 paratoluenesulfonic acid sodium salt Chemical class 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 19
- 238000010189 synthetic method Methods 0.000 claims description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 11
- 239000004332 silver Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000002070 nanowire Substances 0.000 claims description 9
- 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
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000012528 membrane Substances 0.000 abstract description 6
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- GDCXBZMWKSBSJG-UHFFFAOYSA-N azane;4-methylbenzenesulfonic acid Chemical compound [NH4+].CC1=CC=C(S([O-])(=O)=O)C=C1 GDCXBZMWKSBSJG-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000009713 electroplating Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 27
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 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
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 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
- 230000008021 deposition Effects 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
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Abstract
A process for synthesizing nm carbon tubes containing nm-class metal wires includes polymerizing reaction by dipping anodized porous alumina membrane in the mixed solution containing aniline, ammonium p-toluenesulfonate, ammonium metavanadate and hydrochloric acid in nitrogen atmosphere, coating silve slurry on one surface of said anodized porous alumina membrane, baking, electrochemical depositing where said membrane is used as cathode, Fe-series metal wire as anode and Fe-series metal salt is used to prepare electroplating liquid, and burning at 600-1000 deg.C in argon atmosphere. Obtained nm-class carbon tube is 50 microns in length and 30-150 nm in diameter.
Description
The present invention relates to comprise the synthetic method of metal nanometer line carbon nanotube.
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 ℃.
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 porous alumina 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 deposition is had 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
2O 270-300g/L, NiCl
26H
2O 40-60g/L H
3BO
3The solution that 35-40g/L forms; To comprise cobalt nanowire carbon nanotube electroplate liquid can be CoSO for synthetic
47H
2O 250-266g/LH
3BO
3The solution that 40-50g/L forms; To comprise Fe nanowire carbon nanotube plating bath can be FeSO for synthetic
47H
2O 120-140g/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 ferrous metal 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
Further specify the present invention by the following examples.
Example 1 comprises 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
2O 40g/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 comprises 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
2O 40g/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 a template institute synthetic nickel coat carbon nanotube.
Example 3 comprises 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
2O 60g/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 comprises 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 comprises 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 comprises 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 comprises 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 comprises 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 comprises 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 (6)
1. synthetic method that comprises Ferrious material nano wire 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 carries out polyreaction,
B. with the anode multiaperture pellumina after the step a polyreaction-and coat silver slurry, oven dry, as the negative electrode of electrochemical deposition reaction, as anode, Ferrious material salt is made into electroplate liquid carries out electrochemical deposition with required sedimentary Ferrious material silk,
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. synthetic method according to claim 1, the aniline that contains that it is characterized in that step a, paratoluenesulfonic acid sodium salt, the mixing solutions of ammonium meta-vanadate and hydrochloric acid are that isopyknic hydrochloric acid soln that contains aniline forms with the hydrochloric acid soln mixed preparing that contains paratoluenesulfonic acid sodium salt and ammonium meta-vanadate.
3. synthetic method according to claim 2, the hydrochloric acid soln that it is characterized in that 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 that concentration is the 1M hydrochloric acid soln of 0.5-0.8M paratoluenesulfonic acid sodium salt and 0.12-0.14M ammonium meta-vanadate.
4. synthetic method according to claim 1 is characterized in that synthetic comprising nickel nano wire carbon nanotube, and its electroplate liquid is (NH
4)
2SO
47H
2O 270-300g/l, NiCl
26H
2O 40-60g/l, H
3BO
3The solution that 35-40g/l forms.
5. method according to claim 1 is characterized in that synthetic containing the cobalt nanowire carbon nanotube, and its electroplate liquid is CoSO
47H
2O 250-266g/l, H
3BO
3The solution that 40-50g/l forms.
6. synthetic method according to claim 1 is characterized in that synthetic comprising the Fe nanowire carbon nanotube, and its electroplate liquid is FeSO
47H
2O 120-140g/l, H
3BO
345-50g/l, the solution that xitix 1g/l forms.
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| CNB991206584A CN1147427C (en) | 1999-12-22 | 1999-12-22 | Process for synthesizing nm carbon tubes containing nm metal wires |
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| CNB991206584A CN1147427C (en) | 1999-12-22 | 1999-12-22 | Process for synthesizing nm carbon tubes containing nm metal wires |
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| CN103342352A (en) * | 2013-07-24 | 2013-10-09 | 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 |
| CN104528867A (en) * | 2014-12-25 | 2015-04-22 | 东华大学 | Preparation method for environment-friendly advanced water treatment agent by combining carbon nano tube and ferric vanadate |
| CN104846411A (en) * | 2015-04-27 | 2015-08-19 | 北京航空航天大学 | Method for preparing flowerlike nanometer cobalt by using anodised aluminum template, and product of same |
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1999
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102205957A (en) * | 2011-04-07 | 2011-10-05 | 上海大学 | Method for generating carbon chain in multi-wall carbon nanotube |
| CN102205957B (en) * | 2011-04-07 | 2012-10-31 | 上海大学 | Method for generating carbon chain in multi-wall carbon nanotube |
| CN103342352A (en) * | 2013-07-24 | 2013-10-09 | 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 |
| CN104528867A (en) * | 2014-12-25 | 2015-04-22 | 东华大学 | Preparation method for environment-friendly advanced water treatment agent by combining carbon nano tube and ferric vanadate |
| 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 |
| CN104846411A (en) * | 2015-04-27 | 2015-08-19 | 北京航空航天大学 | Method for preparing flowerlike nanometer cobalt by using anodised aluminum template, and product of same |
| 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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| CN1147427C (en) | 2004-04-28 |
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