CN112941680B - Preparation method of carbon nanotube fiber-loaded nano iron oxide composite material - Google Patents
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- CN112941680B CN112941680B CN202110122167.5A CN202110122167A CN112941680B CN 112941680 B CN112941680 B CN 112941680B CN 202110122167 A CN202110122167 A CN 202110122167A CN 112941680 B CN112941680 B CN 112941680B
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9, 10 or 18 of the Periodic System; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention discloses a preparation method of a carbon nano tube fiber loaded nano iron oxide composite material, which comprises the following steps: (1) dissolving ferrocene in an organic solvent to prepare a ferrocene solution; (2) drawing a carbon nanotube array to form a carbon nanotube film by adopting an array spinning method, twisting the carbon nanotube film to prepare carbon nanotube fibers, and spraying the ferrocene solution obtained in the step (1) on the surface of the formed carbon nanotube film in the film drawing process; (3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) in a protective atmosphere. The carbon nano tube fiber loaded nano iron oxide composite material prepared by the invention has good application prospect in the fields of capacitor preparation, catalysis, electrode material preparation and the like.
Description
Technical Field
The invention belongs to the technical field of carbon nanotube composite materials, and particularly relates to a preparation method of a carbon nanotube fiber loaded nano iron oxide composite material.
Background
The carbon nano tube has excellent mechanical, electrical and thermal properties. The preparation of the fiber into a macroscopic structure is an important means for expanding the application of the fiber. As a novel fiber material, the carbon nanotube fiber has the advantages of light weight, good conductivity, strong toughness and various functional characteristics. Nano Fe 2 O 3 It has stable chemical property, and has the advantages of light resistance, chemical corrosion resistance, no toxicity, good dispersibility, good tinting strength, and good ultraviolet absorption. Nano Fe 2 O 3 Meanwhile, the material has the properties of ferric oxide and nano materials, and is a multifunctional nano oxide material. The iron oxide has catalytic, magnetic, electrochemical properties, and the like. The obtained composite material has the high toughness and the high conductivity of the carbon nano tube fiber and the magnetic/electrochemical performance of the nano ferric oxide.
In the prior art, the nano iron oxide is mainly realized by a raw material synthesis method, and the wet preparation method comprises the following steps: precipitation, hydrothermal, forced hydrolysis, microemulsion, sol-gel, etc., and there are also dry processes: carbonyl iron or ferrocene is usually used as a raw material and is prepared by gas phase decomposition, flame thermal decomposition or laser decomposition. The synthesis process is complex in operation, low in efficiency and high in equipment requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a carbon nanotube fiber loaded nano iron oxide composite material.
The technical scheme of the invention is as follows:
a preparation method of a carbon nanotube fiber loaded nano iron oxide composite material comprises the following steps:
(1) dissolving ferrocene in an organic solvent to prepare a ferrocene solution with the concentration of 0.1-2 wt%;
(2) drawing a carbon nanotube array to form a carbon nanotube film by adopting an array spinning method, twisting the carbon nanotube film to prepare carbon nanotube fibers, and spraying the ferrocene solution obtained in the step (1) on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 29-31s under a protective atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 300-500 mA.
In a preferred embodiment of the present invention, the organic solvent is benzene, diethyl ether, petroleum ether or tetrahydrofuran.
Further preferably, the organic solvent is petroleum ether.
In a preferred embodiment of the present invention, the diameter of the carbon nanotube array is 20 to 100 mm.
Further preferably, the diameter of the carbon nanotube array is 60-80 mm.
In a preferred embodiment of the present invention, the carbon nanotube fiber has a diameter of 20 to 120 μm and a length of 5 to 20 cm.
More preferably, the diameter of the carbon nanotube fiber is 90 to 110 μm.
In a preferred embodiment of the invention, the protective atmosphere is an argon atmosphere.
In a preferred embodiment of the present invention, the time for the joule heating treatment is 30 s.
In a preferred embodiment of the present invention, the organic solvent is petroleum ether, the diameter of the carbon nanotube array is 60 to 80mm, the diameter of the carbon nanotube fiber is 90 to 110 μm, the protective atmosphere is an argon atmosphere, and the joule heat treatment time is 30 s.
The beneficial effects of the invention are:
1. the invention adopts an array spinning method, the carbon nano tube is stretched into a film, the ferrocene solution is sprayed on the surface of the film, and the obtained film is twisted to obtain the carbon nano tube fiber, and the method is simple and easy to implement.
2. The invention adopts an instantaneous Joule heating method, under the environment that high-purity argon is taken as protective gas, the obtained carbon nanotube fiber is electrified with instantaneous current, the preparation of the nano iron oxide on the surface of the carbon nanotube fiber is realized in a very short time by taking ferrocene contained in the preparation process of the carbon nanotube fiber as a raw material, and the loading of the nano iron oxide composite material on the surface of the carbon nanotube fiber can be realized in 29-31 s.
3. The invention realizes the generation of iron oxide with different granularities by adjusting different electrified currents through a joule heat treatment device.
4. The method is simple and rapid, and the iron oxide can be well loaded on the surface of the carbon nanotube fiber, so that the method is safe and efficient.
5. The carbon nano tube fiber loaded nano iron oxide composite material prepared by the invention has good application prospect in the fields of capacitor preparation, catalysis, electrode material preparation and the like.
Drawings
Fig. 1 is a schematic view of an apparatus for manufacturing carbon nanotube fibers according to an embodiment of the present invention.
FIG. 2 is a surface topography of carbon nanotube fibers obtained by joule heating under different current conditions in an embodiment of the present invention.
FIG. 3 is a diagram illustrating a heating object of carbon nanotube fibers during an instantaneous Joule heating process in an embodiment of the present invention.
Fig. 4 is an EDS diagram of the carbon nanotube fiber surface iron oxide-loaded composite material prepared in example 1 of the present invention.
Fig. 5 is an XPS chart of the iron oxide composite material loaded on the surface of the carbon nanotube fiber prepared in example 1 of the present invention.
FIG. 6 is a cyclic voltammogram of an electrode in which carbon nanotube fibers without iron oxide composite (a) and a non-carbon nanotube fiber surface iron oxide composite material prepared in example 1 of the present invention (b) are supported, wherein the scanning speeds are 0.5v/s, 0.2v/s, 0.1v/s, and 0.05 v/s.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
The apparatus for Joule heat treatment in the following examples and comparative examples was made with reference to CN 208297264U and set up.
Example 1
(1) Dissolving ferrocene in petroleum ether to prepare a ferrocene solution with the concentration of 1 wt%;
(2) as shown in fig. 1, a carbon nanotube array with a diameter of 80mm is firstly drawn to form a carbon nanotube film by an array spinning method, then the carbon nanotube film is twisted to prepare a carbon nanotube fiber with a diameter of 100 μm, and the ferrocene solution obtained in the step (1) is sprayed on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 30s in a high-purity argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 500mA, and thus obtaining the carbon nanotube fiber.
As shown in fig. 2, the carbon nanotube fiber-loaded nano iron oxide composite material prepared in this embodiment can emit brighter light, and the brightness varies with the current. As can be seen from fig. 3, the surface elements of the obtained carbon nanotube fiber-supported nano iron oxide composite material are distributed as carbon, oxygen, and iron. As can be seen from fig. 4 and 5, the spherical particles on the surface are iron oxide. As shown in fig. 6, under a potential window of-0.8 v to 0.6v, the carbon nanotube fibers before and after the joule heat treatment are respectively scanned at different rates of 0.5v/s to 0.2v/s to 0.1v/s to 0.05v/s, and as can be seen from the cyclic voltammetry curve, the carbon nanotube fiber-loaded nano iron oxide composite material prepared by the embodiment has excellent mechanical and electrical properties, and can be expanded in the application fields of capacitors, electrode materials and the like.
Example 2
(1) Dissolving ferrocene in petroleum ether to prepare a ferrocene solution with the concentration of 0.5 wt%;
(2) as shown in fig. 1, a carbon nanotube array with a diameter of 60mm is firstly drawn to form a carbon nanotube film by an array spinning method, then the carbon nanotube film is twisted to prepare a carbon nanotube fiber with a diameter of 110 μm, and the ferrocene solution obtained in the step (1) is sprayed on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 30s in a high-purity argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 300 mA.
As shown in fig. 2, the surface of the carbon nanotube fiber-supported nano iron oxide composite material prepared in this example is substantially free of large iron oxide composites, but the surface of the carbon nanotube fiber has very small particles, which can be determined as iron oxide crystal grains, and the particles gradually become larger as the current intensity increases.
Comparative example 1
(1) Dissolving ferrocene in petroleum ether to prepare a ferrocene solution with the concentration of 1.2 wt%;
(2) as shown in fig. 1, a carbon nanotube array with a diameter of 60mm is firstly drawn to form a carbon nanotube film by an array spinning method, then the carbon nanotube film is twisted to prepare carbon nanotube fibers with a diameter of 90 μm, and the ferrocene solution obtained in the step (1) is sprayed on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 30s in a high-purity argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 700 mA.
As shown in fig. 2, the surface of the product prepared in this comparative example was damaged, and iron oxide could not be loaded well, and the surface iron oxide particles were less.
Comparative example 2
(1) Dissolving ferrocene in petroleum ether to prepare a ferrocene solution with the concentration of 0.05 wt%;
(2) as shown in fig. 1, a carbon nanotube array with a diameter of 80mm is firstly drawn to form a carbon nanotube film by an array spinning method, then the carbon nanotube film is twisted to prepare a carbon nanotube fiber with a diameter of 100 μm, and the ferrocene solution obtained in the step (1) is sprayed on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 30s in a high-purity argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 500 mA.
The surface of the product prepared in this comparative example was substantially free of iron oxide complexes due to the low concentration of ferrocene.
Comparative example 3
(1) Dissolving ferrocene in petroleum ether to prepare a ferrocene solution with the concentration of 2.5 wt%;
(2) as shown in fig. 1, a carbon nanotube array with a diameter of 80mm is firstly drawn to form a carbon nanotube film by an array spinning method, then the carbon nanotube film is twisted to prepare a carbon nanotube fiber with a diameter of 100 μm, and the ferrocene solution obtained in the step (1) is sprayed on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 30s in a high-purity argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 500mA, and thus obtaining the carbon nanotube fiber.
The product prepared by the comparative example has a surface that is substantially free of nano iron oxide particles and has a composite with a certain thickness due to the excessively high concentration of ferrocene.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, and all equivalent variations and modifications made within the scope of the present invention and the content of the description should be included in the scope of the present invention.
Claims (6)
1. A preparation method of a carbon nanotube fiber loaded nano iron oxide composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) dissolving ferrocene in an organic solvent to prepare a ferrocene solution with the concentration of 0.1-2wt%, wherein the organic solvent is benzene, diethyl ether, petroleum ether or tetrahydrofuran;
(2) drawing a carbon nanotube array with the diameter of 20-100mm by adopting an array spinning method to form a carbon nanotube film, twisting the carbon nanotube film to prepare carbon nanotube fibers with the diameter of 20-120 mu m and the length of 5-20cm, and spraying the ferrocene solution obtained in the step (1) on the surface of the formed carbon nanotube film in the film drawing process;
(3) and (3) carrying out Joule heat treatment on the carbon nanotube fiber prepared in the step (2) for 29-31s in an argon atmosphere, wherein the current intensity of a direct current power supply for the Joule heat treatment is 300-500 mA.
2. The method of claim 1, wherein: the organic solvent is petroleum ether.
3. The method of claim 1, wherein: the diameter of the carbon nano tube array is 60-80 mm.
4. The method of claim 1, wherein: the diameter of the carbon nano tube fiber is 90-110 mu m.
5. The method of claim 1, wherein: the joule heating treatment time was 30 seconds.
6. The method of claim 1, wherein: the organic solvent is petroleum ether, the diameter of the carbon nanotube array is 60-80mm, the diameter of the carbon nanotube fiber is 90-110 mu m, the protective atmosphere is argon atmosphere, and the Joule heat treatment time is 30 s.
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