CN112331436B - Preparation method of coaxial magnetic nano cable based on exchange bias - Google Patents
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- 230000005291 magnetic effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 60
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 49
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 9
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 41
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000006073 displacement reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 2
- 230000005294 ferromagnetic effect Effects 0.000 abstract description 11
- 230000005290 antiferromagnetic effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000011258 core-shell material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 238000012546 transfer Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0072—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity one dimensional, i.e. linear or dendritic nanostructures
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/016—Apparatus or processes specially adapted for manufacturing conductors or cables for manufacturing co-axial cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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Abstract
The invention relates to a preparation method of a coaxial magnetic nano cable composite material based on exchange bias, which utilizes the coaxiality of a carbon nano tube graphite layer and the reducibility of carbon elements to synthesize a multilayer coaxial magnetic nano cable (carbon nano tube/carbide/ferromagnetic metal/antiferromagnetic oxide, CNTs/Ni) with exchange bias effect 3 C/Ni/NiO), constructing a shell/core/carbon-based quaternary magnetic nano-coaxial structure, introducing carbide functional factors, and increasing the effective anisotropy field of the material by virtue of the exchange bias effect between the antiferromagnetic layer and the ferromagnetic layer, thereby increasing the coercivity of the composite material. According to the invention, the ferromagnetic layer is directly obtained by reducing CNTs carbon elements without hydrogen reduction, and contains carbide functional factors of the weak ferromagnetic layer, and the microstructures of the antiferromagnetic layer, the ferromagnetic layer and the carbide layer are controllable, so that the exchange bias effect performance of the coaxial magnetic nano cable can be regulated and controlled, and meanwhile, CNTs are shell layers, so that the composite material performance is more stable.
Description
Technical Field
The invention relates to the field of preparation of magnetic composite materials, in particular to a preparation method of a coaxial magnetic nano cable composite material based on exchange bias.
Background
Carbon Nanotubes (CNTs) mainly comprise single-layer or multi-layer coaxial round tubes composed of carbon atoms in hexagonal arrangement, are special one-dimensional hollow nano structures, have excellent heat resistance, corrosion resistance and impact resistance, good heat transfer and electric conduction performance, and have a series of comprehensive properties such as self-lubricity and biocompatibility, which have been found by Iijma since 1991 as research hot spots.
The coaxial nano cable is composed of a nano wire with a core part as a monomer, an outer layer is coated with a heterogeneous nano shell, and the core part nano wire and the outer shell are coaxial and a core shell system. The coaxial nano cable has three characteristics of one dimension, core-shell and coaxial, and can combine the advantages of the three characteristics so as to optimize the comprehensive performance. The coaxial magnetic nano cable is a core-shell system formed by one-dimensional magnetic nano materials, is an important basic magneto-electronic component material, and has a good application prospect in the fields of ultra-high density magnetic recording, spin electronic devices, targeted drug delivery, tunnel junctions, catalytic sensors and the like.
The magnetic crystal anisotropy of each nano material of the coaxial magnetic nano cable can be reduced along with the reduction of the particle size, and at the moment, the magnetic nano particles can easily lose stable magnetic order by thermal disturbance to become superparamagnetism, so that the further integration and microminiaturization development of the magnetic memory device are limited. In 2003 Skumryev et al reported [ Nature, 2003, 423:850-853 ] that superparamagnetic behavior in ferromagnetic materials could be overcome by using the exchange bias effect of a ferromagnetic/antiferromagnetic interface. In addition, the carbide functional factor has weak ferromagnetism, and can further improve the coercive force of the composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a coaxial magnetic nano cable based on exchange bias, which utilizes the coaxiality of a carbon nano tube graphite layer and the reducibility of carbon elements to synthesize a multilayer coaxial magnetic nano cable (carbon nano tube/carbide/ferromagnetic metal/antiferromagnetic oxide, CNTs/Ni) with exchange bias effect 3 C/Ni/NiO), constructing a shell/core/carbon-based quaternary magnetic nano-coaxial structure, introducing carbide functional factors, and increasing the effective anisotropy field of the material by virtue of the exchange bias effect between the antiferromagnetic layer and the ferromagnetic layer, thereby increasing the coercivity of the composite material.
In order to achieve the above object, the present invention provides a method for preparing a coaxial magnetic nano cable, which is characterized by comprising the following steps:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structures, refluxing 2 h at 120-150 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. proper amount of Ni (NO) 3 ) 2 •6 H 2 Dissolving O and CNTs in the mixed solution of diethylene glycol and diethanolamine, ultrasonic dispersing for 30 min, stirring in water bath at 80deg.C, adding a certain amount of NH dropwise 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO with a certain pressure 2 Then placing the reaction kettle into an oil inlet bath pot for stirring reaction for a period of time; 3. the obtained product is filtered and then put into a muffle furnace for calcination for 1-3 hours at 200-250 ℃; 4. after the sample is cooled, washing nickel salt on the surface of the carbon nano tube by distilled water, and then cooling the sample at 5000-10000 r.min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the mixed solution of diethylene glycol and diethanolamine is 1:1-1:3;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 0.5-1T;
said displacement CO 2 The pressure intensity is 0.1-0.5 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 150-250 ℃, and the reaction time is 10-24 h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 250-300 ℃ at a speed of 5 ℃/min in air, preserving heat for 1-h, then introducing argon, heating to 550-750 ℃ at a speed of 5 ℃/min, preserving heat for 30-300 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
The invention has the advantages that: the method of the invention directly utilizes CNTs carbon element reduction to obtain the ferromagnetic layer without hydrogen reduction, and contains the carbide functional factors of the weak ferromagnetic layer, and the microstructures of the antiferromagnetic layer, the ferromagnetic layer and the carbide layer are controllable, so that the exchange bias effect performance of the coaxial magnetic nano cable can be regulated and controlled, and meanwhile, CNTs are shell layers to enable the composite material performance to be more stable.
Drawings
FIG. 1 is CNTs/Ni prepared in the examples 3 C/Ni/NiO composite material in H FC Field cooling of =10koeTo an M-H plot of 10K, the coercivity and exchange bias field of the composite can be obtained from the plot.
Detailed Description
The invention will now be described in detail with reference to examples for a better understanding of the objects, features and advantages of the invention. Although the invention is described in connection with this particular embodiment, it is not intended to be limited to the particular embodiment described. On the contrary, the invention is intended to cover alternatives, modifications and equivalents, which may be included within the spirit and scope of the invention as defined by the appended claims. The process parameters which are not particularly marked can be carried out by conventional techniques.
Example 1: the preparation method of the coaxial magnetic nano cable based on the exchange bias is specifically completed by the following steps:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structure, refluxing 2 h at 150 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. 2 mmol Ni (NO) 3 ) 2 •6 H 2 Dissolving O and 10 mg CNTs in the mixed solution of diethylene glycol and diethanolamine, performing ultrasonic dispersion for 30 min, and then adding 4mmol NH dropwise after fully stirring uniformly in a water bath at 80 DEG C 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO 2 Then placing the reaction kettle into an oil inlet bath kettle for stirring reaction; 3. the obtained product is filtered and then put into a muffle furnace for calcination at 200 ℃ for 3 h; 4. after the sample is cooled, the distilled water is used for cleaning the nickel salt on the surface of the carbon nano tube, and then the sample is cooled in 10000 r min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the mixed solution of diethylene glycol and diethanolamine is 1:1;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 0.5T;
said displacement CO 2 The pressure of (2) is 0.1 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 200 ℃, and the reaction time is 15 h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 250 ℃ at a speed of 5 ℃/min in air, preserving heat for 1 h, then introducing argon, heating to 750 ℃ at a speed of 5 ℃/min, preserving heat for 30 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
For the sample prepared in example 1, at H FC Test M-H plot of field cool 10 kOe to field cool 10K, from which a coercivity Hc of 431 Oe and exchange bias field H of the composite material can be obtained E 94 Oe.
Example 2: the preparation method of the coaxial magnetic nano cable based on the exchange bias is specifically completed by the following steps:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structure, refluxing 2 h at 150 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. 2 mmol Ni (NO) 3 ) 2 •6 H 2 Dissolving O and 20mg CNTs in the mixed solution of diethylene glycol and diethanolamine, performing ultrasonic dispersion for 30 min, and then adding 4mmol NH dropwise after fully stirring uniformly in a water bath at 80 DEG C 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO 2 Then placing the reaction kettle into an oil inlet bath kettle for stirring reaction; 3. the obtained product is filtered and then put into a muffle furnace for calcination at 250 ℃ for 1 h; 4. after the sample is cooled, the distilled water is used for cleaning the nickel salt on the surface of the carbon nano tube, and then the sample is cooled down in the temperature of 5000 r min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the mixed solution of diethylene glycol and diethanolamine is 1:1;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 1T;
said displacement CO 2 The pressure of (2) is 0.5 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 150 ℃, and the reaction time is 24h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 300 ℃ in air at a speed of 5 ℃/min, preserving heat for 1 h, then introducing argon, heating to 550 ℃ at a speed of 5 ℃/min, preserving heat for 300 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
For the sample prepared in example 2, at H FC The M-H plot of the field cool-to-10K test of 10 kOe, from which the coercivity Hc of the composite material is 319 Oe and the exchange bias field H can be obtained E 51 Oe.
Example 3: the preparation method of the coaxial magnetic nano cable based on the exchange bias is specifically completed by the following steps:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structure, refluxing 2 h at 120 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. 2 mmol Ni (NO) 3 ) 2 •6 H 2 Dissolving O and 10 mg CNTs in the mixed solution of diethylene glycol and diethanolamine, performing ultrasonic dispersion for 30 min, and then adding 4mmol NH dropwise after fully stirring uniformly in a water bath at 80 DEG C 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO 2 Then placing the reaction kettle into an oil inlet bath kettle for stirring reaction; 3. the obtained product is filtered and then put into a muffle furnace for calcination at 220 ℃ for 2 h; 4. after the sample is cooled, the distilled water is used for cleaning the nickel salt on the surface of the carbon nano tube, and then 8000 r min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the mixed solution of diethylene glycol and diethanolamine is 1:3;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 0.8T;
said displacement CO 2 The pressure of (2) is 0.1 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 250 ℃, and the reaction time is 10 h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 280 ℃ in air at a speed of 5 ℃/min, preserving heat for 1 h, then introducing argon, heating to 600 ℃ at a speed of 5 ℃/min, preserving heat for 100 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
For the sample prepared in example 3, at H FC Test M-H plot of field cool 10 kOe to field cool 10K, from which a coercivity Hc of 390 Oe and exchange bias field H of the composite material can be obtained E 65 Oe.
Example 4: the preparation method of the coaxial magnetic nano cable based on the exchange bias is specifically completed by the following steps:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structure, refluxing 2 h at 120 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. 2 mmol Ni (NO) 3 ) 2 •6 H 2 Dissolving O and 15 mg CNTs in the mixed solution of diethylene glycol and diethanolamine, performing ultrasonic dispersion for 30 min, and then adding 4mmol NH dropwise after fully stirring uniformly in a water bath at 80 DEG C 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO 2 Then placing the reaction kettle into an oil inlet bath kettle for stirring reaction; 3. the obtained product is filtered and then put into a muffle furnace for calcination at 200 ℃ for 3 h; 4. after the sample is cooled, the distilled water is used for cleaning the nickel salt on the surface of the carbon nano tube, and then 7000 r.min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the mixed solution of diethylene glycol and diethanolamine is 1:3;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 1T;
said displacement CO 2 The pressure of (2) is 0.1 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 200 ℃, and the reaction time is 15 h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 300 ℃ in air at a speed of 5 ℃/min, preserving heat for 1 h, then introducing argon, heating to 750 ℃ at a speed of 5 ℃/min, preserving heat for 200 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
For the sample prepared in example 4, at H FC Test M-H plot of field cool 10 kOe to field cool 10K, from which a coercivity Hc of 354 Oe and exchange bias field H of the composite material can be obtained E 54, oe.
Claims (1)
1. The preparation method of the coaxial magnetic nano cable is characterized by comprising the following steps of:
1) Preparation of CNTs: selecting multiwall CNTs with rigid structures, refluxing 2 h at 120-150 ℃ by using concentrated nitric acid, sequentially performing ultrasonic dispersion on methyldimethoxy silane, ethanol and distilled water, and drying for later use;
2) Preparation of NiO/CNTs: 1. 2 mmol of Ni (NO) 3 ) 2 •6 H 2 Dissolving O and 10-20 mg of CNTs in a mixed solution of diethylene glycol and diethanolamine, performing ultrasonic dispersion for 30 min, and then dropwise adding 4mmol of NH after fully and uniformly stirring in a water bath at 80 DEG C 3 ·H 2 O is a blend; 2. transferring the blend into a reaction kettle with a magnetic field to replace CO 2 Then placing the reaction kettle into an oil inlet bath pot for stirring reaction for a period of time; 3. the obtained product is filtered and then put into a muffle furnace for calcination for 1-3 hours at 200-250 ℃; 4. after the sample is cooled, washing nickel salt on the surface of the carbon nano tube by distilled water, and then cooling the sample at 5000-10000 r.min -1 Centrifugal separation is carried out at the rotating speed of 80 ℃ and vacuum drying is carried out to obtain a NiO/CNTs precursor;
the proportion of the diethylene glycol to the diethanolamine is 1:1-1:3;
the direction of the magnetic field is perpendicular to the stirring direction, and the size of the magnetic field is 0.5-1T;
said displacement CO 2 The pressure of the post-reaction kettle is 0.1-0.5 MPa;
the stirring speed in the oil bath pot is 400 r/min, the temperature is 150-250 ℃, and the reaction time is 10-24 h;
3）、CNTs/Ni 3 preparation of C/Ni/NiO: placing the material obtained in the step 2) into a tube furnace, heating to 250-300 ℃ at a speed of 5 ℃/min in air, preserving heat for 1-h, then introducing argon, heating to 550-750 ℃ at a speed of 5 ℃/min, preserving heat for 30-300 min, and naturally cooling to obtain CNTs/Ni 3 C/Ni/NiO composite material.
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| JP2004083296A (en) * | 2002-08-23 | 2004-03-18 | Koichi Kusabe | Magnetized carbon nanotube and magnetized nano carbon structure |
| CN104843805A (en) * | 2015-04-16 | 2015-08-19 | 电子科技大学 | CNTs@SiO2@Ni/Al-LDH shell structure three-dimensional nanometer material and preparation method thereof |
| WO2019189925A1 (en) * | 2018-03-30 | 2019-10-03 | 古河電気工業株式会社 | Carbon nanotube coated wire rod for coil, coil in which carbon nanotube coated wire rod for coil is used, and method for producing coil of carbon nanotube coated wire rod |
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| US9050605B2 (en) * | 2011-11-17 | 2015-06-09 | Lamar University, A Component Of The Texas State University System, An Agency Of The State Of Texas | Graphene nanocomposites |
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| JP2004083296A (en) * | 2002-08-23 | 2004-03-18 | Koichi Kusabe | Magnetized carbon nanotube and magnetized nano carbon structure |
| CN104843805A (en) * | 2015-04-16 | 2015-08-19 | 电子科技大学 | CNTs@SiO2@Ni/Al-LDH shell structure three-dimensional nanometer material and preparation method thereof |
| WO2019189925A1 (en) * | 2018-03-30 | 2019-10-03 | 古河電気工業株式会社 | Carbon nanotube coated wire rod for coil, coil in which carbon nanotube coated wire rod for coil is used, and method for producing coil of carbon nanotube coated wire rod |
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