CN101745434B - Method for selectively filling ferric oxide particles in hollow cavity of carbon nanotube - Google Patents
Method for selectively filling ferric oxide particles in hollow cavity of carbon nanotube Download PDFInfo
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- CN101745434B CN101745434B CN2008102299690A CN200810229969A CN101745434B CN 101745434 B CN101745434 B CN 101745434B CN 2008102299690 A CN2008102299690 A CN 2008102299690A CN 200810229969 A CN200810229969 A CN 200810229969A CN 101745434 B CN101745434 B CN 101745434B
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000002245 particle Substances 0.000 title claims abstract description 58
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000011049 filling Methods 0.000 title abstract description 15
- 239000002041 carbon nanotube Substances 0.000 title abstract description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 title abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 15
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000009514 concussion Effects 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000009415 formwork Methods 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 150000001722 carbon compounds Chemical class 0.000 abstract 2
- 239000003054 catalyst Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 9
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 7
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 239000011232 storage material Substances 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000003863 metallic catalyst Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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Abstract
The invention relates to the selectively filling of ferric oxide particles in the hollow cavity of a carbon nanotube, in particular to a method for selectively filling ferric oxide particles in the hollow cavity of a carbon nanotube, with accurate and controllable ferric oxide particle filling amount and size, and the application of a filling compound. An anodic alumina membrane with a regular pore structure is taken as a template, and a carbon layer is evenly deposited on the template by a chemical vaporous deposition method, and then an anodic alumina membrane/carbon compound is obtained; the compound is put in a ferric nitrate solution and then is ultrasonically shaken at room temperature; the anodic alumina membrane/carbon compound is taken out and then is treated under the protective atmosphere after being dried; ferric nitrate is decomposed into ferric oxide; then the anodic alumina template is removed; and finally, a carbon nanotube that the ferric oxide particles are selectively filled in the hollow cavity of the carbon nanotube is obtained. The ferric oxide particles are selectively filled in the hollow cavity of the carbon nanotube, the content by weight of the ferric oxide particles is between 5 percent and 70 percent and is accurate, even and controllable, and the sizes of the ferric oxide particles are between 1nm and 10nm and is controllable.
Description
Technical field
The present invention relates to ferric oxide particles and fill, be specially the accurately controlled method of a kind of ferric oxide particles selectivity filling, ferric oxide particles loading and size in CNT hollow tube chamber and the purposes of filled composite in the intraluminal selectivity of CNT hollow.
Background technology
The modern humans is faced with problems such as the energy, environmental pollution, and the solution of these problems all needs to depend in large quantities catalytic process.Carrier is being played the part of important role in catalytic process, it is as the skeleton of supported catalyst, it mainly acts on and increases active surface and suitable hole is provided, the activated centre is provided, improves the thermal conductivity and the heat endurance of catalyst, improves the mechanical strength of catalyst and performance (between carrier and catalyst activity component chemical action taking place) etc.
CNT can regard that certain crooked and space topological structure of forming takes place Graphene hexagon grid as, the hollow tube chamber that have that chemical stability is good, heat shock resistance, electric conductivity uniqueness, intensity height, specific area are big, has nanoscale, with excellent properties such as biocompatible is good.Because the arrangement mode of guest molecule and related physical chemical process may be totally different in macroscopical plane in the confinement effect, the accurate one dimension hollow of CNT tube chamber, so CNT also can be used as unique " nanochemistry test tube ".Owing to have said structure and performance characteristics, CNT is considered to a kind of desirable catalyst carrier material.
Recent result of study shows, because the space confinement effect, the catalytic activity and the life-span that are filled in the intraluminal catalyst granules of CNT hollow obviously are better than the outer catalyst granules of tube wall.But it is up to the present, very limited to multiple-wall carbon nanotube both at home and abroad as the research report of catalyst carrier material.Existing in CNT hollow tube chamber the approach of catalyst filling particle be CNT to be cut off in oxidizing acid solution and opening (document 1, Pan 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.NanoLetters 8:2738 (2008)).The subject matter of this method is: catalyst particle can't selectivity be filled in the hollow tube chamber amount of uncontrollable filler particles and size.CNT as catalyst carrier is a lack of alignment, and the opening of CNT is to obtain by acidification simultaneously, and this just makes its aperture opening ratio and draw ratio be difficult to control; In addition, though most of metallic catalyst is filled in the hollow tube chamber of CNT, but still 20% the catalyst deposit of having an appointment is at outer surface, and the content of catalyst granules is less simultaneously.This both had been unfavorable for the raising of catalyst activity, also was unfavorable for furtheing investigate the confinement enhancing mechanism of the accurate one dimension hollow of CNT tube chamber to metallic catalyst.
Summary of the invention
The object of the present invention is to provide a kind of the complete selectivity of ferric oxide particles to be filled in the intraluminal method of CNT hollow, and propose its purposes.Solved at present and can't catalyst particle be filled in the hollow tube chamber selectivity amount of uncontrollable filler particles and the problem of size.
Technical scheme of the present invention is:
A kind of ferric oxide particles fully optionally is filled in the intraluminal method of CNT hollow, the ferric oxide particles weight content is accurate homogeneous and controllable between 5-70%, the ferric oxide particles size is controlled in the 1-10 nanometer, and the size of CNT that is filled with ferric oxide particles is evenly accurately controlled.
The described ferric oxide particles preparation method that selectivity is filled in CNT hollow tube chamber, be template, be that carbon source, inert gas are carrier gas, chemical vapour deposition technique uniform deposition charcoal layer on template with anodic alumina films, obtain the compound of anodic alumina films/carbon with little molecule organic molecule with regular pore structure.Compound is put into iron nitrate solution; the concentration of iron nitrate solution is 5-35wt%; ultrasonic concussion is 0.5-3 hour under the room temperature; take out the compound of anodic alumina films/carbon; at 60-140 ℃ of dry 2-6 hour; 350-500 ℃ of processing (1-5 hour) resolved into iron oxide with ferric nitrate under protective atmosphere again, removes anodic oxidation aluminium formwork then, obtains the ferric oxide particles CNT that selectivity is filled in CNT hollow tube chamber at last.
Described anodic oxidation aluminium formwork is the preparation of sulfuric acid or Oxalic Acid Method, and its aperture is the 10-100 nanometer, and length is 50 nanometers-200 micron, a both ends open or an end opening.
Described little molecule organic molecule is acetylene, ethene or propylene, and described inert gas is argon gas or nitrogen, and the vapour deposition temperature is 600-900 ℃, and heating rate is 5-30 ℃/min, and 0.5-5 hour vapour deposition time, the carbon-source gas volumetric concentration is 1-20%.
The described purposes that is filled with the CNT of ferric oxide particles in the hollow tube chamber is meant: can be used as nano catalysis reaction device and energy storage material.
Among the present invention, the thickness of chemical vapour deposition technique uniform deposition charcoal layer on template is the 2-20 nanometer.
Advantage of the present invention is:
1, the present invention can prepare the complete selectivity of ferric oxide particles and is filled in the intraluminal CNT of hollow, has solved present ferric oxide particles and can't 100% be filled in nano-sized carbon hollow tube chamber, and ferric oxide particles content and size such as can't accurately control at problem.
2, the CNT of the iron oxide filling of the present invention's preparation, can be by optimizing the accurately content and the size of control iron oxide such as iron nitrate concentration, ultrasonic time, heating rate, the weight content of iron oxide is between 5-70%, and the ferric oxide particles size is controlled in the 1-10 nanometer.
3, the multiple-wall carbon nanotube of the iron oxide selectivity filling of the inventive method preparation can be used as nano catalysis reaction device and energy storage material.
Description of drawings
Fig. 1. the even selectivity of ferric oxide particles is filled in the intraluminal transmission electron microscope photo of CNT hollow.
Fig. 2. the even selectivity of ferric oxide particles is filled in the intraluminal stereoscan photograph of CNT hollow.
The specific embodiment
Below by embodiment in detail the present invention is described in detail.
At the 3wt% oxalic acid aqueous solution, negative electrode adopts aluminium flake, and anode adopts aluminium flake, and anodic oxidation prepares the anodic alumina films of an end opening under 20 ℃, 40V condition.600 ℃ of chemical vapour deposition (CVD)s of carrying out acetylene gas 0.5 hour, carrier gas was an argon gas after the anodic alumina films drying, and flow is 300ml/min, and heating rate is 5 ℃/min, and the acetylene gas volumetric concentration is 1.5%, and the thickness of deposit carbon layer is 2 nanometers.The post-depositional anodic alumina films of carbon is placed in the iron nitrate solution that concentration is 30wt%, and ultrasonic concussion was taken out after 2 hours, after the clean surface at 140 ℃, air drying 6 hours, the speed with 5 ℃/min is elevated to 350 ℃ under argon atmospher then, constant temperature 3 hours.Remove anodic alumina films behind the cool to room temperature, just obtained the ferric oxide particles complete filling at the intraluminal CNT of hollow, as shown in Figure 1.The content of iron oxide is about 70wt%, and particle size distribution is concentrated to be distributed in about 5 nanometers between the 3-10 nanometer.
Embodiment 2.
The anodised aluminium membrane preparation method is with embodiment 1.700 ℃ of chemical vapour deposition (CVD)s of carrying out acetylene gas 5 hours, carrier gas was a nitrogen after the anodic alumina films drying, and flow is 300ml/min, and heating rate is 5 ℃/min, and the acetylene gas volumetric concentration is 5%, and the thickness of deposit carbon layer is 20 nanometers.The post-depositional anodic alumina films of carbon is placed in the iron nitrate solution that concentration is 25wt%, and ultrasonic concussion was taken out after 0.5 hour, after the clean surface at 60 ℃, vacuum drying 2 hours, the speed with 30 ℃/min is elevated to 350 ℃ under argon atmospher then, constant temperature 1 hour.Remove anodic alumina films behind the cool to room temperature, just obtained the CNT of ferric oxide particles complete filling at the hollow tube chamber.As shown in Figure 2, there is not ferric oxide particles in the outside of CNT.The content of iron oxide is about 20wt%, and particle size distribution is concentrated to be distributed in about 3 nanometers between the 1-8 nanometer.
Embodiment 3.
At the 10wt% aqueous sulfuric acid, negative electrode adopts aluminium flake, and anode adopts aluminium flake, and anodic oxidation prepares the anodic alumina films of an end opening under 10 ℃, 20V condition.600 ℃ of chemical vapour deposition (CVD)s of carrying out acetylene gas 0.5 hour, carrier gas was an argon gas after the anodic alumina films drying, and flow is 200ml/min, and heating rate is 5 ℃/min, and the acetylene gas volumetric concentration is 5%, and the thickness of deposit carbon layer is 5 nanometers.The post-depositional anodic alumina films of carbon is placed in the iron nitrate solution that concentration is 25wt%, ultrasonic concussion was taken out after 3 hours, and at 140 ℃, drying is 3 hours under the air atmosphere after the clean surface, speed with 10 ℃/min is elevated to 350 ℃ under argon atmospher then, constant temperature 3 hours.Remove anodic alumina films behind the cool to room temperature, just obtained the CNT of ferric oxide particles complete filling at the hollow tube chamber, the content of iron oxide is about 5wt%, and average particle size particle size is about 4 nanometers.
Embodiment 4.
The anodised aluminium membrane preparation method is with embodiment 3, different is anodic alumina films is 800 ℃ of chemical vapour deposition (CVD)s of carrying out ethylene gas 3 hours after the both ends open anodic alumina films drying through post-processed, carrier gas is an argon gas, flow is 300ml/min, heating rate is 10 ℃/min, the ethylene gas volumetric concentration is 1.5%, and the thickness of deposit carbon layer is 10 nanometers.The post-depositional anodic alumina films of carbon is placed in the iron nitrate solution that concentration is 10wt%, and ultrasonic concussion was taken out after 2 hours, and 140 ℃ of air dryings 2 hours, the speed with 5 ℃/min was elevated to 450 ℃ under argon atmospher then, constant temperature 1 hour after the clean surface.Remove anodic alumina films behind the cool to room temperature, just obtained the CNT of ferric oxide particles complete filling at the hollow tube chamber, the content of iron oxide is 20wt%, and average particle size particle size is about 8 nanometers.
Embodiment 5.
The anodised aluminium membrane preparation method is with embodiment 4.900 ℃ of chemical vapour deposition (CVD)s of carrying out propylene gas 2 hours, carrier gas was a nitrogen after the anodic alumina films drying, and flow is 300ml/min, and heating rate is 5 ℃/min, and the propylene gas volumetric concentration is 1.5%, and the thickness of deposit carbon layer is 11 nanometers.The post-depositional anodic alumina films of carbon is placed in the iron nitrate solution that concentration is 25wt%, and ultrasonic concussion was taken out after 0.5 hour, and 60 ℃ of vacuum drying 6 hours, the speed with 20 ℃/min was elevated to 500 ℃ under argon atmospher then, constant temperature 3 hours after the clean surface.Remove anodic alumina films behind the cool to room temperature, just obtained the CNT of ferric oxide particles complete filling at the hollow tube chamber, the content of iron oxide is about 40wt%, and average particle size particle size is about 10 nanometers.
Embodiment result shows, the present invention can be by optimizing anodic alumina films preparation condition, chemical vapor deposition conditions, the filling condition of ferric oxide particles optionally ferric oxide particles is filled in the controlled CNT hollow tube chamber of structure, and the content of ferric oxide particles and size are accurately controlled, this structure and size can be accurately controlled and the catalyst granules selectivity be filled in the intraluminal nano-sized carbon of hollow and can be used as nano catalysis reaction device and energy storage material.
Claims (5)
1. a ferric oxide particles selectivity is filled in the intraluminal method of CNT hollow, it is characterized in that: with the anodic alumina films with regular pore structure is template, by chemical vapour deposition technique uniform deposition charcoal layer on template, obtain the compound of anodic alumina films/carbon; Compound is put into iron nitrate solution; the concentration of iron nitrate solution is 5-35wt%; ultrasonic concussion is 0.5-3 hour under the room temperature; take out the compound of anodic alumina films/carbon; at 60-140 ℃ of dry 2-6 hour, again under protective atmosphere 350-500 ℃ handled 1-5 hour, ferric nitrate is resolved into iron oxide; remove anodic oxidation aluminium formwork then, obtain the ferric oxide particles CNT that selectivity is filled in CNT hollow tube chamber at last.
2. be filled in the intraluminal method of CNT hollow according to the described ferric oxide particles selectivity of claim 1, it is characterized in that: the ferric oxide particles selectivity is filled in CNT hollow tube chamber, the ferric oxide particles weight content is accurate homogeneous and controllable between 5-70%, the ferric oxide particles size is controlled in the 1-10 nanometer, and the size of CNT that is filled with ferric oxide particles is evenly accurately controlled.
3. be filled in the intraluminal method of CNT hollow according to the described ferric oxide particles selectivity of claim 1, it is characterized in that: described anodic alumina films adopts oxalic acid or sulfuric acid process preparation.
4. be filled in the intraluminal method of CNT hollow according to the described ferric oxide particles selectivity of claim 1, it is characterized in that: described drying mode is vacuum drying or at air drying.
5. be filled in the intraluminal method of CNT hollow according to the described ferric oxide particles selectivity of claim 1, it is characterized in that: described protective atmosphere is argon gas or nitrogen.
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CN102274976B (en) * | 2011-05-16 | 2013-05-29 | 云南师范大学 | Method for preparing nanomaterials by using anodized aluminum oxide template |
CN102263257B (en) * | 2011-06-28 | 2013-08-07 | 中国科学院金属研究所 | High energy flexible electrode material and preparation method thereof and application thereof in storage battery |
CN102386042B (en) * | 2011-12-04 | 2014-05-28 | 中国航天科技集团公司第五研究院第五一〇研究所 | Preparation method of carbon nanotube field emission cathode |
GB2500611A (en) * | 2012-03-26 | 2013-10-02 | Cambridge Entpr Ltd | Powder comprising carbon nanostructures and method of preparation |
CN103022451B (en) * | 2012-12-24 | 2015-03-25 | 中国科学院金属研究所 | Nano silicon particles filled carbon nano tube compound as well as preparation method and application thereof |
CN109778214B (en) * | 2017-11-15 | 2020-11-13 | 中国科学院金属研究所 | Method for rapidly and selectively filling nano particles into carbon nano tube cavity |
CN109698342B (en) * | 2018-12-28 | 2022-08-19 | 廊坊绿色工业技术服务中心 | Metal oxide-ordered carbon nanotube composite material and preparation method and application thereof |
WO2021223251A1 (en) * | 2020-05-06 | 2021-11-11 | 青岛理工大学 | Metal oxide nano-confined catalytic film for catalytic treatment of wastewater and method for preparation thereof |
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CN1670251A (en) * | 2005-03-01 | 2005-09-21 | 东华大学 | Method for preparing magnetic compound material of ferric oxide cladded carbon nanotube |
CN1743387A (en) * | 2005-04-07 | 2006-03-08 | 东华大学 | Method for preparing carbon nanotube magnetic compositematerial modified by iron oxide red |
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