CN113708086B - Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof - Google Patents
Transition metal nano powder/carbon nano tube composite material and preparation method and application thereof Download PDFInfo
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 159
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 143
- 239000002131 composite material Substances 0.000 title claims abstract description 86
- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 49
- 150000003624 transition metals Chemical class 0.000 title claims abstract description 49
- 239000011858 nanopowder Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000004744 fabric Substances 0.000 claims abstract description 47
- 239000011358 absorbing material Substances 0.000 claims abstract description 16
- 229920000742 Cotton Polymers 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 44
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 10
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- WXTMDXOMEHJXQO-UHFFFAOYSA-N 2,5-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC(O)=CC=C1O WXTMDXOMEHJXQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 230000020477 pH reduction Effects 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000002048 multi walled nanotube Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 126
- 229910052759 nickel Inorganic materials 0.000 description 60
- 230000000694 effects Effects 0.000 description 29
- 238000010521 absorption reaction Methods 0.000 description 12
- 230000035699 permeability Effects 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000002310 reflectometry Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 230000007423 decrease Effects 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 239000002105 nanoparticle Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
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- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
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- 238000002329 infrared spectrum Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
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- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000009991 scouring Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
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- 230000001070 adhesive effect Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002052 molecular layer Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 description 1
- 229910014033 C-OH Inorganic materials 0.000 description 1
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
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- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
- H01Q17/005—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems using woven or wound filaments; impregnated nets or clothes
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a transition metal nano powder/carbon nano tube composite material, a preparation method and application thereof, and belongs to the technical field of composite materials. The preparation method of the transition metal nano powder/carbon nano tube composite material comprises the following steps: and mixing and heating the acidified carbon nano tube and the transition metal nano powder to obtain the transition metal nano powder/carbon nano tube composite material. The invention not only prepares the transition metal nano powder with extremely high purity, but also utilizes the reaction of the transition metal nano powder and the carbon nano tube to ensure that the transition metal nano powder is uniformly attached on the surface of the carbon nano tube, thus preparing the composite material with stable dielectric loss; and the cotton fabric is immersed in the composite material, so that the fabric material with excellent wave absorbing performance is prepared, and a research foundation is provided for developing flexible wave absorbing materials and development of stealth technology.
Description
Technical Field
The invention relates to the field of composite materials, in particular to a transition metal nano powder/carbon nano tube composite material, a preparation method and application thereof.
Background
The wave absorbing material plays an important role in the radar stealth field, the aerospace field, the NFC antenna field and the like. The radar stealth is realized by using the appearance design, and the radar wave absorber is generally adopted to achieve the stealth purpose due to the limitation of targets and forms and high realization difficulty and high cost.
Nickel (Ni) is a hard and diffuse metal with strong ferromagnetism, which can produce a high degree of polishing and corrosion resistance. The chemical properties are more active but more stable. Nickel (Ni) is mainly used for shielding electromagnetic radiation interference and other materials in conductive pigment materials made of paint, plastics and the like. However, the density of the metallic nickel is generally higher, the metallic nickel can be used as a wave-absorbing material to be coated to increase the overall quality, and the metallic nickel has poor oxidation resistance in the application process and serious oxidation at the temperature higher than 500 ℃ so that the metallic nickel cannot be used in a large scale.
The carbon nanotube material is one new kind of one-dimensional flexible carbon atom nanometer material with carbon atom passing sp 2 The hybridized and tightly combined arrangement can form a honeycomb crystal structure, has the characteristics of large length-diameter ratio, low density, large specific surface area, high conductivity, high mechanical strength and the like, and shows good wave absorption characteristics from visible light to infrared wave frequency bands, but has smaller microwave permeability, so that the further improvement of the wave absorption performance of the carbon nano tube is limited.
Based on the reasons, the transition metal nano powder/carbon nano tube composite material provided by the invention can improve the microwave permeability of the carbon nano tube, and simultaneously overcome the problems of high density and easy oxidation of the magnetic metal powder, and has great development significance for the application of the transition metal and the carbon nano material in the wave absorbing material.
Disclosure of Invention
The invention aims to provide a transition metal nano powder/carbon nano tube composite material, a preparation method and application thereof, so as to solve the problems in the prior art, the transition metal nano powder/carbon nano tube composite material is obtained by mixing and heating the acidified carbon nano tube and the transition metal nano powder, and cotton fabric is immersed in the composite material solution to obtain the fabric with excellent wave absorbing performance, thereby providing a good foundation for the discovery of novel wave absorbing materials and the development of stealth technology.
In order to achieve the above object, the present invention provides the following solutions:
one of the technical schemes of the invention is as follows: a preparation method of a transition metal nano powder/carbon nano tube composite material comprises the following steps: and mixing and heating the acidified carbon nano tube and the transition metal nano powder to obtain the transition metal nano powder/carbon nano tube composite material.
Further, the acidification treatment specifically includes: mixing carbon nano tube with acid solution in 1-5 g: and (3) mixing 150-300 mL of the mixture, heating and refluxing at 100-120 ℃ for 8-16 h (the condition that all the solution is black and sticky indicates that the carbon nano tube is completely acidified, or else, refluxing is continued until all the solution is black and sticky), and washing and drying to obtain the acidized carbon nano tube.
Further, when the solution is entirely black and the solution is black and viscous, it indicates that the carbon nanotubes have been fully acidified; if part of the solution is yellow (the yellow solution is an impurity solution containing nitrogen dioxide), separating the yellow solution, refluxing again until all the solution is black, standing for a period of time after refluxing, filtering with deionized water, washing the solution to be neutral, and drying for 24 hours to obtain the acidized carbon nanotube.
The purpose of the acidification treatment is to increase the activity of carbon nanotubes (MWCNTs), to perform a preliminary purification, to remove impurities.
Further, the carbon nanotubes are multiwall carbon nanotubes; the acidic solution is a concentrated nitric acid solution with the mass fraction of 68-75%.
Further, the preparation of the transition metal nano powder specifically comprises the following steps: and mixing the transition metal salt solution with ethylene glycol, sequentially adding a sodium hydroxide solution, a sodium borohydride solution and a hydrazine hydrate solution, and stirring to obtain the transition metal nano powder.
Further, the mass fraction of sodium hydroxide in the sodium hydroxide solution is 40%.
Still further, the sodium borohydride solution has a pH of 14.
Sodium borohydride can be rapidly decomposed in neutral or acidic solution, and a small amount of ammonia water is needed to be added for hydrolysis prevention during preparation.
Further, the mass fraction of the hydrazine hydrate solution is 20%.
Still further, a small amount of NaOH solution in the hydrazine hydrate solution, (hydrazine hydrate alkaline polar imposition NaOH solution more easily adjusts the reaction), a white paste-like consistency is formed.
Still further, the transition metal salt solution, ethylene glycol, sodium hydroxide solution, sodium borohydride solution, and hydrazine hydrate solution are mixed according to a volume ratio of 3:2:2:2: 1.
Further, the transition metal salt solution is a nickel sulfate solution.
Further, the carbon nano tube after acidification treatment is further subjected to the following treatment before being mixed with the transition metal nano powder for heating: ultrasonic treatment in absolute alcohol solution, and ultrasonic treatment in 2, 5-dihydroxybenzoic acid solution.
The second technical scheme of the invention is as follows: a transition metal nano powder/carbon nano tube composite material prepared by a preparation method of the transition metal nano powder/carbon nano tube composite material.
The third technical scheme of the invention: an application of a transition metal nano-powder/carbon nano-tube composite material in preparing a wave-absorbing material.
The technical scheme of the invention is as follows: a preparation method of a wave-absorbing material comprises the following steps: preparing the transition metal nano powder/carbon nano tube composite material of claim 7 into a composite material aqueous solution, soaking the pretreated cotton fabric in the composite material aqueous solution, padding, and drying to obtain the wave-absorbing material.
Still further, the preprocessing specifically includes: soaking cotton fabric with the size of 25cm multiplied by 25cm in 50 times of alkali liquor, desizing in water bath at 80-90 ℃ for 30min, washing with water, and boiling off.
Still further, the pre-treated lye is sodium hydroxide solution, and the concentration of the lye is 10g/L.
Still further, the scouring specifically includes: the cotton fabric was boiled in a 20g/L sodium hydroxide solution for 2 hours.
The pretreatment aims at removing pectin, cotton seed hulls, grease, wax, nitrogen-containing substances and ash and other impurities such as greasy dirt which are attached to the cotton fabric during weaving, and PVA chemical and starch slurry and other substances which can be added during processing, so that the influence of the substances on experimental results can be reduced.
Further, the padding time is 30min; the drying temperature is 60 ℃.
The invention discloses the following technical effects:
according to the invention, the transition metal nano powder is uniformly attached to the surface of the carbon nano tube by acidizing the carbon nano tube, so that the transition metal nano powder/carbon nano tube composite material with extremely high purity is obtained, oxidation is not easy to occur when the transition metal nano powder/carbon nano tube composite material is applied at the temperature higher than 500 ℃, the transition metal is attached to the carbon nano tube, the weight of the wave-absorbing material is effectively reduced, and meanwhile, the transition metal has magnetism and excellent conductivity of the carbon nano tube, so that the transition metal nano powder/carbon nano tube composite material has the properties of both the transition metal and the carbon nano tube, the wave-absorbing property of the material is effectively improved, and the composite material with moderate conductivity, good stability, stable dielectric loss and lower magnetic loss is prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart showing the preparation of a nickel/carbon nanotube composite material according to example 1 of the present invention;
FIG. 2 is an X-ray diffraction spectrum analysis chart of the composite material and the carbon nanotubes prepared in the embodiment 1 of the present invention, wherein CNTs are carbon nanotubes and Ni-CNTs are nickel nanoparticle/carbon nanotube composite material;
FIG. 3 is an SEM image of the composite material and carbon nanotubes prepared in example 1 of the present invention, wherein a and b are SEM images of the nickel/carbon nanotube composite material, and c and d are SEM images of the carbon nanotube composite material;
FIG. 4 is an infrared spectrum analysis chart of the composite material and the carbon nanotubes prepared in the embodiment 1 of the present invention, wherein CNTs are carbon nanotubes and Ni-CNTs are nickel/carbon nanotube composite material;
FIG. 5 is a graph showing the real and imaginary parts of the complex dielectric constants of the composite material and the carbon nanotubes prepared in example 1 of the present invention, wherein Ni-CNTs ε 'is the real part of the complex dielectric constant of the nickel/carbon nanotube composite material, ni-CNTs ε "is the imaginary part of the complex dielectric constant of the nickel/carbon nanotube composite material, CNTs ε' is the real part of the complex dielectric constant of the carbon nanotubes, and CNTs ε" is the imaginary part of the complex dielectric constant of the carbon nanotubes;
FIG. 6 is a graph of real and imaginary parts of complex permeability of the composite material and carbon nanotubes prepared in example 1 of the present invention, ni-CNTs μ 'is the real part of complex permeability of the nickel/carbon nanotube composite material, ni-CNTs μ″ is the imaginary part of complex permeability of the nickel/carbon nanotube composite material, CNTs μ' is the real part of complex permeability of the carbon nanotubes, CNTs μ″ is the imaginary part of complex permeability of the carbon nanotubes;
FIG. 7 is a graph showing the dielectric loss tangent tan delta e of the composite material and carbon nanotubes prepared in example 1 of the present invention, wherein CNTs are carbon nanotubes and Ni-CNTs are nickel/carbon nanotube composite material;
FIG. 8 is a graph of the magnetic loss tangent tan δm of the composite material and carbon nanotubes prepared in example 1 of the present invention, wherein CNTs are carbon nanotubes and Ni-CNTs are nickel/carbon nanotube composite material;
FIG. 9 shows the wave absorbing effect of Ku wave bands of the composite materials prepared in examples 2 to 6 of the present invention;
FIG. 10 is a graph showing the wave absorbing effect of the X-band of the composite materials prepared in examples 2 to 6 of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
Example 1
A preparation method of a transition metal/carbon nano tube composite material comprises the following steps:
(1) 150mL of concentrated nitric acid solution and 1g of multiwall carbon nanotube are added into a 500mL round bottom flask, reflux treatment is carried out at 120 ℃ until all the solution turns black, heating is stopped when the solution is black and thick, deionized water is used for filtering and washing to be neutral after standing, and the acidified carbon nanotube is obtained after drying for 24h in an electric heating hot air drying box.
(2) Preparing nickel nano powder: 1g of nickel sulfate was dissolved in 75mL of distilled water, 50mL of ethylene glycol, 50mL of 10% strength by mass aqueous NaOH solution, 50mL of NaBH having a pH of 14 and 5% strength by mass were added 4 Aqueous solution (NaBH) 4 A small amount of ammonia water is added into the aqueous solution to prevent nitric acid hydrolysis), 25mLN 2 H 4 Solution (N) 2 H 4 Adding a small amount of NaOH salt water solution into the solution to form a white pasty sticky matter, uniformly mixing, and then stirring at high speed (stirring is finer) under the working condition of room temperature and humidity to prepare nickel nano powder (namely nickel nano particles) with the morphology of chain sphere nano particle crystals, and mixing and cleaning the nickel nano powder with a small amount of absolute ethyl alcohol3 times, drying under vacuum and refrigerating.
(3) Preparation of nickel/carbon nanotube composite material: adding 0.05g of acidified carbon nano tube into 100mL of 75% ethanol solution, carrying out ultrasonic treatment for 1h, adding (50) mL of 2, 5-dihydroxybenzoic acid, carrying out ultrasonic treatment for 30min, adding (1) g of nickel nano powder, mixing, stirring, carrying out centrifugal treatment, repeatedly washing with deionized water, and drying at 60 ℃ for 12h to obtain the nickel/carbon nano tube composite material, wherein the preparation process is shown in figure 1.
Example 2
A preparation method of a wave-absorbing material comprises the following steps:
(1) Pretreatment of cotton fabric: 200g of cotton fabric with the size of 25cm multiplied by 25cm is added into 10kg of 10g/L sodium hydroxide solution, desizing is carried out for 30min in a constant-temperature water bath with the temperature of 80-90 ℃, hot water with the temperature of 80-90 ℃ is used for washing twice for 10min each time, water with the temperature of 50-60 ℃ is used for washing, finally cold water is used for washing to be neutral, the cotton fabric is dried in the air and then is put into 20g/L sodium hydroxide solution, the temperature is raised to be boiling and the boiling and scouring time is kept for 2h, the desizing step is repeated after the scouring, and then the pretreated cotton fabric is hung in an oven with the temperature of not more than 60 ℃ for drying.
(2) 1g of the nickel/carbon nano tube composite material prepared in the example 1 is dissolved in 199mL of deionized water to prepare nickel/carbon nano tube composite material dispersion liquid with the mass fraction of 0.5%, the pretreated cotton fabric is soaked in the nickel/carbon nano tube composite material dispersion liquid for 30min, the process is repeated for three times, and finally the wave-absorbing material is obtained by drying in an oven at about 60 ℃.
Example 3
The difference from example 2 is that the mass fraction of the nickel/carbon nanotube composite dispersion in step (2) is 1%.
Example 4
The difference from example 2 is that the mass fraction of the nickel/carbon nanotube composite dispersion in step (2) is 3%.
Example 5
The difference from example 2 is that the mass fraction of the nickel/carbon nanotube composite dispersion in step (2) is 5%.
Example 6
The difference from example 2 is that the mass fraction of the nickel/carbon nanotube composite dispersion in step (2) is 7%.
Effect example 1
The carbon nanotubes and the nickel/carbon nanotube composite material prepared in example 1 were subjected to X-ray diffraction spectroscopy (XRD), respectively, and the internal structure of the material, the composition of molecules, etc. were known using a JEM-2100 transmission electron microscope (JEOL, japan). When the test is carried out, the adopted conditions are as follows: cu target, kα:0.15406nm, tube voltage: 36kV, tube current: 30mA, the scanning speed is 2 degrees/min, and the scanning range is 10-80 degrees; the results are shown in FIG. 2.
As can be seen from fig. 2, the chemical composition and crystal phase structure of the carbon nanotubes, nickel/carbon nanotube composite material were analyzed by XRD. The diffraction peak of the (002) crystal face of carbon and the diffraction peak of the (111) crystal face of nickel can be observed, compared with the diffraction peak of pure carbon nano tubes, the intensity of the diffraction peak of the carbon nano tubes in the composite material is reduced, the width is narrowed, no impurity peak appears, and the purity of the nickel nano powder in the prepared composite material is higher.
Effect example 2
The carbon nanotubes and the nickel/carbon nanotube composite material prepared in example 1 were subjected to microscopic morphology analysis (SEM), a tungsten filament optical scanning electron microscope of taiskin international trade (Shanghai group) company TESCAN VEGA3 was selected, a metal powder with a relatively large particle size was prepared into a sample, the sample was placed on a piece of conductive adhesive by a small-sized clamping button, the original was clamped on a sample tray by clamping the conductive adhesive, the powder sample was blown with an ear-washing ball several times to avoid falling off and to check whether screws were screwed, and the morphology of the sample was characterized, and the result was shown in fig. 3.
The nickel particles are uniformly adhered to the surface of the carbon nanotube as shown in fig. 3, the inner diameter size of nickel ions is about 10nm, the nickel ions are liquefied in the heating process and fall on the surface of the carbon nanotube, a layer of non-crystal face is formed on the surface of the carbon nanotube and forms chemical bonds with the carbon nanotube, the crystal phase is good, and the two substances coexist in a composite system.
Effect example 3
The carbon nanotubes and the nickel/carbon nanotube composite material prepared in example 1 were respectively subjected to infrared spectroscopic analysis (FT-IR), a Fourier transform type short wave infrared spectrometer was selected, which mainly adopts a non-dispersive infrared spectrometer, and the group composition of the composite material was detected by infrared spectroscopic analysis, and the result is shown in FIG. 4.
As can be seen from FIG. 4, at 3411cm -1 The broad peak at the position is the stretching vibration peak of-OH, which shows that the acidified carbon nano tube contains a large amount of hydroxyl groups, and the absorption peak is 2970cm -1 ，1630cm -1 ，1395cm -1 ，1064cm -1 The vibration characteristic peaks of C-H, C=C, C-OH, C-O are respectively. For the infrared spectrum curve of the nickel/carbon nanotube composite material, at 3411cm -1 the-OH peak is slightly enhanced, which is that after the nickel nano layer is coated, more-OH is provided, and besides the characteristic absorption peak of the carbon nano tube, the nickel nano layer is provided at 1553cm -1 ，1260cm -1 There is a new absorption peak, which represents the bending vibration of-N-H and the absorption peak of-C-N stretching shrinkage vibration, respectively. After the nickel nano particles are loaded on the surface of the carbon nano tube, the infrared spectrum curve of the carbon nano tube is approximately similar to that of the carbon nano tube, which shows that the nickel nano particles are loaded and have little influence on the active group structure of the carbon nano tube, and shows that the nickel/carbon nano tube composite material can be stably dispersed in base oil.
Effect example 4
Uniformly mixing the nickel/carbon nanotube composite material prepared in the embodiment 1 of the invention with paraffin wax at a mass ratio of 7:3, heating the mixture by an intelligent magnetic stirrer while stirring the mixture sufficiently, pouring the mixture into a specific mold (the mold is a coaxial ring with an inner diameter of 3.04mm and an outer diameter of 7 mm), taking out the coaxial ring from the mold after cooling and solidifying, and using VNA to test epsilon ' in a frequency range of 2-18 GHz to represent a real part of complex dielectric constant, and in addition epsilon ' represents an imaginary part of complex dielectric constant and mu ' represents an imaginary part of complex magnetic conductivity and dielectric loss tangent (tan delta) e ) Magnetic loss tangent (tan delta) m ) Six kinds ofIndex, and combining the related knowledge of transmission line theory, for the reflection loss value (R L ) Fitting the index to determine the size of the index under different thickness conditions; the electromagnetic wave absorption performance measurement results are shown in FIGS. 5 to 8.
As can be seen from FIG. 5, the imaginary maximum value can reach 120 and the real maximum value can reach 60 at 2-18 GHz. Along with the continuous increase of the test frequency, the real part and the imaginary part of the complex dielectric constant of the carbon nano tube wholly decline in a gradient manner, but the real part and the imaginary part also fluctuate up and down, but the imaginary part begins to gradually increase at about 16GHz, the imaginary part is increased to 60 after the initial 120 declines to 0, and the real part is increased to 60 after the initial 20 declines to-10; from the figure, the real part and the imaginary part of the complex dielectric constant of the carbon nanotube are large, which indicates that the carbon nanotube can absorb more incident electromagnetic waves and can carry out great loss attenuation on the electromagnetic waves, and the conductivity is strong but unstable; in the range of 2-18 GHz, the real part and the imaginary part of the complex dielectric constant of the nickel/carbon nano tube composite material are very stable by measuring electromagnetic parameters, the real part and the imaginary part of the complex dielectric constant of the nickel/carbon nano tube composite material reach peak values when the frequency is 12GHz, the real part and the imaginary part of the complex dielectric constant are consistent in overall trend, the imaginary part is always lower than the real part, and the stability and the mutual matching degree of the metal composite material such as the nickel/carbon nano tube are improved by adding nickel nano particles into the complex dielectric constant.
As can be seen from fig. 6, by testing that the real part and the imaginary part of the complex magnetic permeability of the electromagnetic parameter carbon nanotube float up and down between 0 and 10, and have obvious float in the range of 15 to 18GHz, the trend of the real part and the imaginary part are consistent, and at 17GHz, the real part and the imaginary part of the complex magnetic permeability reach peaks, respectively 8 and 4, which indicate that the magnetism of the carbon nanotube gradually increases with the increase of frequency, and indicate that the magnetic property of the carbon nanotube firstly increases and then decreases in the range of 15 to 18GHz, and the attenuation capability of the carbon nanotube firstly increases and then decreases. By testing electromagnetic parameters in the frequency range of 2-18 GHz, the real part and the imaginary part of the complex magnetic permeability of the nickel/carbon nanotube can be observed to be consistent with the increase of the frequency and maintained at 1, while the imaginary part is slightly changed near 0 along with the increase of the frequency, which indicates that the attenuation capability of the nickel/carbon nanotube to electromagnetic waves is relatively poor, the trend of the real part and the imaginary part is consistent, and the test shows that the carbon nanotube has better magnetic property in the range of 15-18 GHz.
As shown in fig. 7, the dielectric loss tangent (tan delta e) of the carbon nanotube increases with the frequency, then decreases, and then increases and decreases again, and two peaks occur in the whole frequency range, namely, in the two frequency ranges of 2-6 GHz and 14-18 GHz, respectively, the highest dielectric loss tangent (tan delta e) can reach 4, which indicates that the carbon nanotube has stronger but unstable and ineffective dielectric loss, and the dielectric loss tangent (tan delta e) of the nickel/carbon nanotube composite material is steadily increased with the frequency, which indicates that the nickel/carbon nanotube composite material has strong, stable and effective dielectric loss.
As can be seen from fig. 8, the magnetic loss tangent (tan δm) of the carbon nanotube increases and decreases, and then increases and decreases in the test frequency range, and particularly, the magnetic loss tangent fluctuates greatly up and down at 15GHz to 18GHz, but the magnetic loss tangent (tan δm) does not change much as a whole, indicating that the carbon nanotube has relatively unstable magnetic loss and strong magnetic loss at a part of the frequency. While the magnetic loss tangent (tan delta m) of the nickel/carbon nanotube composite material fluctuates only in a small range within the test frequency range of 2-18 GHz, and as a whole, the magnetic loss tangent (tan delta m) of the nickel/carbon nanotube composite material gradually decreases with the increase of the frequency, which indicates that the nickel/carbon nanotube composite material has relatively weak magnetic loss.
In summary, ε 'represents the real part of the complex permittivity, ε "represents the imaginary part of the complex permittivity, μ' represents the real part of the complex permeability, μ" represents the imaginary part of the complex permeability, the dielectric loss tangent (tan. Delta.) e ) Magnetic loss tangent (tan delta) m ) Six indexes can obtain that the conductivity of the carbon nano tube is too high to cause impedance mismatch, and the conductivity in a proper range can be just obtained after the nickel nano particles are added, and the composite material has good stability and stable dielectric loss from the angle, and the carbon nano tube hasThe composite material has very stable property after the transition metal is attached, and the magnetic loss is low.
Effect example 5
The wave-absorbing materials prepared in examples 2 to 6 were subjected to Ku-band and X-band wave-absorbing performance tests
As can be seen from fig. 9, the Ku band wave absorbing performance test was performed on the nickel/carbon nanotube coated fabric with different mass fractions, and when the mass fraction of the nickel/carbon nanotube coated fabric was 0.5%, there was little wave absorbing effect because the dispersion was too low, and during the coating process, the dispersion immersed in the fabric yarn and did not float on the surface to cause little wave absorbing effect of the fabric, and as the concentration of the dispersion increased, the wave absorbing effect of the coated fabric became better in turn, but as the frequency increased, the wave absorbing effect of the fabric decreased, indicating that the coated fabric was more suitable for Ku band downlink. We divide the Ku wave band into up and down, find that the wave absorbing effect of the coated fabric with the mass fraction of 7% is best-8 dB at the time of down 10.7-12.75GHz, the absorption rate can reach 84.2%, but the wave absorbing effect is unstable, the wave absorbing effect is in a linear weakening trend along with the increase of the frequency, and the wave absorbing effect of the coated fabric with the mass fraction of 3% is better and stable at the time of up 12.75-18.1GHz, the absorption rate is 68.4%.
As can be seen from fig. 10, the nickel/carbon nanotube coated fabric with different mass fractions was subjected to the X-band wave absorbing performance test, and it can be seen that the coated fabric with mass fractions of 0.5% and 1% has little wave absorbing effect in the X-band, about-2 dB, about 36.9% absorption rate, and most of the coated fabric is lost by reflection or transmission. The fabric reflectivity of the coated fabric with the mass fraction of 3% gradually decreases along with the increase of the frequency, namely the fabric wave absorbing effect is better and better, and the fabric reflectivity reaches-8 dB and the absorption rate is 84.2% when the frequency is 12.5 GHz. The fabric reflectivity of the coated fabric with the mass fraction of 5% is gradually reduced and gradually increased along with the increase of the frequency, namely the fabric wave absorbing effect of the coated fabric is slowly improved and then slowly deteriorated, and the fabric reflectivity reaches-10 dB and the absorption rate is 90% at the frequency of 10 GHz. And the reflectivity of the coated fabric with the mass fraction of 7% is increased sequentially along with the increase of the frequency, so that the wave absorbing effect of the fabric is poorer and worse.
According to the 2 graphs, the Ku wave band and the X wave band wave absorbing performance of various coated fabrics are tested, and according to the comparison of the 10 groups of data, the wave absorbing effect of the coated fabrics with the mass fraction of 0.5% and 1% is always less ideal, the coated fabrics with the mass fraction of 3% are always stable in the Ku wave band and the X wave band, and the reflectivity always fluctuates in the range of-5 dB to-4 dB; the wave absorbing effect of the coated fabric with the mass fraction of 5% in the X wave band is better than that of the coated fabric in the Ku wave band; the wave absorbing effect of the coated fabric with the mass fraction of 7% is optimal in the X-wave band or the Ku-wave band, but the stability is poor and the reflectivity is greatly floated. But when the mass fractions are the same, the wave absorbing effect of the X wave band is always better than that of the Ku wave band.
The nickel nano particles are uniformly attached to the surface of the carbon nano tube by carrying out chemical treatment on the carbon nano tube, and the nickel/carbon nano tube composite material is subjected to structural characterization, and after cotton fabric is coated, electromagnetic parameters, reflectivity and other parameters are tested, and the conclusion is as follows:
(1) The nickel/carbon nano tube composite material is uniformly attached after chemical treatment, no nickel oxide impurity peak appears, and the carbon nano tube loaded with nickel nano particles does not change the functional group, which indicates that the chemical reaction does not destroy chemical bonds.
(2) The conductivity of the nickel/carbon nano tube composite material accords with impedance matching, and has stable dielectric loss.
(3) In the X-band and the Ku-band, as the mass fraction increases, the lower the reflectivity of the fabric, the better the wave absorbing effect, the most stable wave absorbing effect is a coated fabric with the mass fraction of 3%, the reflectivity is-5 dB, the absorptivity is 68.4%, the best wave absorbing effect is a coated fabric with the mass fraction of 7%, the reflectivity is-12 dB, the absorptivity is 93.7%, and when the mass fractions are the same, the wave absorbing effect of the X-band is better than that of the Ku-band.
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (5)
1. The preparation method of the transition metal nano powder/carbon nano tube composite material is characterized by comprising the following steps of: mixing and heating the acidified carbon nano tube and the transition metal nano powder to obtain the transition metal nano powder/carbon nano tube composite material;
the preparation of the transition metal nano powder specifically comprises the following steps: mixing a transition metal salt solution with ethylene glycol, sequentially adding a 40% sodium hydroxide solution, a 14 pH sodium borohydride solution and a 20% hydrazine hydrate solution, and stirring to obtain the transition metal nano powder;
the volume ratio of the transition metal salt solution, the ethylene glycol, the sodium hydroxide solution, the sodium borohydride solution and the hydrazine hydrate solution is 3:2:2:2:1, a step of;
the transition metal salt solution is nickel sulfate solution;
the acidification treatment specifically comprises the following steps: mixing carbon nano tube with acid solution in 1-5 g: mixing 150-300 mL, heating and refluxing at 100-120 ℃ for 8-16 h, washing and drying to obtain the acidized carbon nano tube;
the carbon nanotubes are multi-wall carbon nanotubes; the acidic solution is a concentrated nitric acid solution with the mass fraction of 68-75%;
the carbon nano tube after acidification treatment is further subjected to the following treatment before being mixed with the transition metal nano powder for heating: ultrasonic treatment in absolute alcohol solution, and ultrasonic treatment in 2, 5-dihydroxybenzoic acid solution.
2. A transition metal nano-powder/carbon nano-tube composite material prepared by the preparation method of the transition metal nano-powder/carbon nano-tube composite material of claim 1.
3. The preparation method of the wave-absorbing material is characterized by comprising the following steps of: preparing the transition metal nano powder/carbon nano tube composite material of claim 2 into a composite material aqueous solution, soaking the pretreated cotton fabric in the composite material aqueous solution, padding, and drying to obtain the wave-absorbing material.
4. A method of producing a wave-absorbing material according to claim 3, wherein the padding time is 30min; the drying temperature is 60 ℃.
5. A wave-absorbing material prepared by the preparation method of any one of claims 3 to 4.
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