CN103436996B - Ni/C composite nano fiber microwave absorption, preparation method and application thereof - Google Patents
Ni/C composite nano fiber microwave absorption, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of high performance magnetic carbon back composite nano fiber microwave absorption and preparation method thereof, this composite nano fiber adopts electrostatic spinning to obtain in conjunction with Post isothermal treatment one-step method, synthesis technique is simple, the average diameter of gained fiber is 100 ~ 300nm, it is inner or surperficial that the Ni nano particle generated is distributed in carbon nano-fiber more equably, 's wrap up by graphitization carbon-coating, there is stronger anti-oxidant and corrosion resistance.With the compounded microwave absorbing coating of silica gel when absorbent contents is 3 ~ 10wt%, its density is only 0.8 ~ 1.0g/cm
3, when coating layer thickness is 1.2 ~ 2.0mm, its minimal reflection loss Da – 36 Zhi – 71dB, reaches 9.7GHz at effective Absorber Bandwidth of 2 ~ 18GHz scope internal reflection loss little Yu – 10dB, covers the X-band of whole Ku wave band and 95%.There is light weight, wideband, by force absorption, electromagnetic parameter facilitate the advantages such as adjustable.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material field, particularly relate to a kind of Novel broadband, lightweight, strong absorption one-dimensional magnetic carbon-based nano composite wave-suction material and preparation method thereof.
Background technology
Electromagnetic wave absorbent material military project and civil in all have a wide range of applications, become the focus of the technical field researchs such as military equipment electromagnetism stealth, electromagnetic shielding and anti-electromagnetic-radiation interference.Absorbing material depends on filling radio-radar absorber wherein to electromagnetic absorption.Along with the development of nanometer technology, although the low-dimensional nanometer of conventional absorbents as ferrite and magnetic metal material makes it be greatly increased to electromagnetic absorbent properties and improve, one-component absorbent is still difficult to meet the requirement of development of modern scientific technology to " thickness is thin, quality is light, bandwidth, absorption strong " that absorbing material performance proposes.So multiple absorbent being carried out compound, to make nanostructured composite wave-suction material may be realize one of effective way that absorbing property essence breaks through, and is also an important directions of absorbing material future development simultaneously.Utilize the cooperative effect of composite and the adjustable advantage of electromagnetic parameter, difference is absorbed frequency range, the absorbent of different loss mechanism carries out multiple elements design, by regulating the structure composition of material, microscopic appearance and electromagnetic parameter to realize its impedance matching, thus to reach low-density, to absorb and wide band effect by force.
Tradition absorbing material is often because density is large, poor stability or absorption band is narrow, matching thickness is large etc. that shortcoming constrains its development and application.Carbon nano-fiber, as a kind of important absorbing material, is subject to the favor of people by means of advantages such as its low-density, high temperature resistant, anticorrosive and excellent electric properties.But as typical dielectric loss material, its electromagnetic matching is poor, has strong reflectivity to electromagnetic wave.At present, carbon nano-fiber absorbing material in application mostly is Surface coating magnetic metal coating or magnetic oxide coating, carry out magnetic modification to carbon nano-fiber to reach and improve the object of its electromagnetic matching, the absorbing property of the composite obtained all is better than performance during single use.But due to the magnetic metal that plates or deposit or alloy coat be positioned at the surface of carbon fiber, it is anti-oxidant and decay resistance is poor, thus limits the normal use of this type of magnetic carbon fiber composite under some complex environments to a certain extent.
Summary of the invention
Goal of the invention: for above-mentioned existing Problems existing and deficiency, the object of this invention is to provide one and is different from magnetic carbon fiber absorbing material and technique simple novel high-performance one-dimensional magnetic metal/carbon Composite Microwave absorbent, preparation method and application thereof in the past.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of Ni/C composite nano fiber microwave absorption, described compound Nano carbon fiber doping includes Ni nano particle, and top layer is wrapped up by graphitization carbon-coating, the average diameter of this composite Nano Carbon fibe is 100 ~ 300nm.
A preparation method for above-mentioned Ni/C composite nano fiber microwave absorption, comprises the following steps:
Step 1: spinning solution is prepared, and adds polyacrylonitrile in dimethyl formamide (DMF), and is stirred to and dissolves completely; And then add nickel acetylacetonate and continue to be stirred to and dissolve completely, obtain even, transparent, stable spinning solution;
Step 2: spinning solution step 1 obtained moves in electrostatic spinning apparatus, carries out electrostatic spinning and obtains polymer-metal salt composite precursor fiber, and the precursor fibre dry 10 ~ 24h at 80 ~ 120 DEG C that will collect;
Step 3: under inert gas conditions, obtains composite precursor fiber after pre-oxidation, and obtains Ni/C composite nano fiber through carbonization treatment by step 2.
In spinning solution described in step 1, the mass fraction of polyacrylonitrile is 5 ~ 12%; The mass fraction of nickel acetylacetonate is 4 ~ 13%.
Described in step 2, electrostatic spinning process parameter is: voltage 10 ~ 22kV, and solution advances speed 0.2 ~ 0.8mL/h, and solidification distance is 15 ~ 25cm, and temperature is 15 ~ 30 DEG C, and humidity is less than 60%.
Described in step 3, pre-oxidation design parameter is: temperature is 180 ~ 280 DEG C, temperature retention time 1 ~ 3h, and heating rate is 1 ~ 5 DEG C/min.
Described in step 3, carbonization treatment design parameter is: temperature is 600 ~ 1300 DEG C, and atmosphere is argon gas or nitrogen, temperature retention time 1 ~ 3h, and heating rate is 2 ~ 10 DEG C/min.
Based on a microwave absorbing coating for above-mentioned Ni/C composite nano fiber microwave absorption, take silica gel as matrix, the Ni/C composite nano fiber microwave absorption of the 3 ~ 10wt% that adulterates in silica gel, and the thickness of microwave absorbing coating is 1.2 ~ 2.0mm.
Beneficial effect: compared with prior art; the present invention had the following advantages: the Ni/C composite nano fiber microwave absorbing material prepared by the present invention not only have lightweight, frequency range is wide, absorb the features such as strong; but also there is stronger anti-oxidant and corrosion resistance; the introducing of magnetic metal Ni significantly improves and improves the absorbing property of carbon nano-fiber, has broad application prospects in technical fields such as electromagnetism stealth, electromagnetic shielding and anti-electromagnetic-radiation interference; The present invention's Ni/C composite nano fiber that adopted electrostatic spinning in conjunction with Post isothermal treatment process one-step synthesis, the syntheti c route proposed can expand the magnetic carbon fiber microwave absorption for constructing containing other magnetic metals or alloy material easily; Relative to other methods for the preparation of magnetic carbon fiber composite, it is simple that technology of preparing of the present invention has technique, and with low cost, productive rate is high comparatively, can prepare target product Ni/C composite nano fiber continuously in a large number.
Accompanying drawing explanation
Fig. 1 is the SEM photo of Ni/C composite nano fiber prepared by the embodiment of the present invention 1;
Fig. 2 is the XRD spectra of Ni/C composite nano fiber prepared by the embodiment of the present invention 1;
Fig. 3 is the Ni/C composite nano fiber of the embodiment of the present invention 1 preparation and the reflection loss curve of silica gel complex.
Detailed description of the invention
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
The present invention's magnetic Ni/C composite nano fiber that adopted electrostatic spinning in conjunction with Post isothermal treatment one-step synthesis, preparation technology is simple, Ni nano particle is embedded in carbon nano-fiber comparatively equably, and wrap up by graphitization carbon-coating, stop the contact with air, substantially increase its anti-oxidant and corrosion resistance, prepared Ni/C composite nano fiber is the electromagnetic wave absorbent material of a kind of light weight, wideband, strong absorption, high comprehensive performance.
The method of the concrete Ni/C of preparation composite nano fiber microwave absorption mainly comprises the preparation of solution, the electrostatic spinning process of precursor fibre and pre-oxidation thereof and carbonization treatment.Its concrete steps are:
(1) by a certain amount of polyacrylonitrile (PAN, mean molecule quantity 150000) join in appropriate solvent dimethylformamide (DMF), in 50 ~ 70 DEG C of heating water baths and magnetic agitation 2 ~ 5h to PAN dissolve completely, and then add a certain amount of nickel acetylacetonate, continue magnetic agitation 10 ~ 15h at normal temperatures and obtain even, transparent, stable spinning solution.In this spinning solution, the mass fraction of PAN is 5 ~ 12% (preferably 6 ~ 10%), and the mass fraction of nickel acetylacetonate is 4 ~ 13% (preferably 6 ~ 10%), and all the other are solvent DMF.
(2) spinning solution prepared is moved in electrostatic spinning apparatus, voltage be 10 ~ 22kV (preferably 11 ~ 17kV), receiving range is 15 ~ 25cm (preferably 18 ~ 23cm), solution feeding rate is 0.2 ~ 0.8mL/h (preferably 0.3 ~ 0.6mL/h), environment temperature is 15 ~ 30 DEG C, humidity is carried out electrostatic spinning and made PAN/ nickel acetylacetonate composite precursor fiber, and the precursor fibre collected put into baking oven in 80 ~ 120 DEG C of drying 10 ~ 24h under being less than the condition of 60%.
(3) dried precursor fibre is risen to 180 ~ 280 DEG C (preferably 220 ~ 260 DEG C) with the speed of 1 ~ 5 DEG C/min (preferably 2 ~ 3 DEG C/min) by room temperature in air atmosphere and carry out pre-oxidation, temperature retention time 1 ~ 3h, naturally cools to room temperature with stove afterwards.
(4) fiber sample after pre-oxidation is heated to 600 ~ 1300 DEG C and is incubated 1 ~ 3h carry out carbonization treatment by room temperature with the speed of 2 ~ 10 DEG C/min (preferably 3 ~ 6 DEG C/min) again under argon gas or nitrogen atmosphere, naturally cool to room temperature under argon gas or nitrogen atmosphere after, obtain Ni/C composite nano fiber microwave absorption.
Embodiment 1
The polyacrylonitrile (PAN) of 0.9g is joined in the conical flask filling 8.3g dimethyl formamide (DMF), in 50 DEG C of heating water baths and magnetic agitation 3h to PAN dissolve completely, and then add the nickel acetylacetonate of 0.8g, continue magnetic agitation 15h at normal temperatures and obtain even, transparent, stable spinning solution.In this spinning solution, the mass fraction of PAN is 9%, and the mass fraction of nickel acetylacetonate is 8%, and all the other are solvent DMF.The spinning solution prepared is moved in electrostatic spinning apparatus, voltage be 15kV, receiving range is 15cm, solution feeding rate is 0.5mL/h, spinnerette diameters 0.9mm, environment temperature is 20 ~ 25 DEG C, humidity is carried out electrostatic spinning and made PAN/ nickel acetylacetonate composite precursor fiber, and the precursor fibre collected put into baking oven in 80 DEG C of dry 10h under being the condition of 35 ~ 45%.Dried precursor fibre is risen to 250 DEG C with the speed of 2 DEG C/min by room temperature in air atmosphere and carries out pre-oxidation, temperature retention time 3h, naturally cool to room temperature with stove afterwards.Fiber sample after pre-oxidation is heated to 1000 DEG C and is incubated 1h carry out carbonization treatment by room temperature with the speed of 5 DEG C/min more under an argon atmosphere, obtain Ni/C composite nano fiber microwave absorption after naturally cooling to room temperature under an argon atmosphere, its average diameter is about 150nm.Take silica gel as matrix, prepared Ni/C composite nano fiber is that absorbent is made into microwave absorbing coating, when absorbent contents is 5wt%, when coating layer thickness is 1.7mm, its minimal reflection loss Da Dao – 71dB, effective Absorber Bandwidth of 2 ~ 18GHz scope internal reflection rate little Yu – 10dB is 8.3GHz, and frequency range is 9.7 ~ 18GHz.
Embodiment 2
Basic process is with embodiment 1.Unlike: the content of the PAN in spinning solution is 7wt%, and nickel acetylacetonate content is 4wt%, and Pre oxidation is 240 DEG C, carburizing temperature 800 DEG C, and the average diameter of the Ni/C composite nano fiber of acquisition is about 140nm; When absorbent useful load be 3wt%, coating layer thickness be 1.9mm time, minimal reflection loss Wei – 38dB, effective Absorber Bandwidth 6.7GHz, frequency range is 8.8 ~ 15.5GHz.
Embodiment 3
Basic process is with embodiment 1.Unlike: carburizing temperature is 1200 DEG C, and the average diameter of the Ni/C composite nano fiber obtained is about 120nm; When absorbent useful load be 3wt%, coating layer thickness be 1.8mm time, minimal reflection loss Wei – 46dB, effective Absorber Bandwidth 7.8GHz, frequency range is 10.2 ~ 18GHz.
Embodiment 4
Basic process is with embodiment 1.Unlike: in spinning solution, the content of PAN is 10wt%, nickel acetylacetonate content is 10wt%, voltage is 12kV, receiving range is 23cm, fltting speed is 0.3mL/h, spinnerette diameters 0.8mm, and Pre oxidation is 240 DEG C, carburizing temperature is 1100 DEG C, and the average diameter of the Ni/C composite nano fiber obtained is about 260nm; When absorbent useful load be 3wt%, coating layer thickness be 2.0mm time, minimal reflection loss Wei – 61dB, effective Absorber Bandwidth 9.9GHz, frequency range is 8.1 ~ 18GHz.
Claims (7)
1. a Ni/C composite nano fiber microwave absorption, is characterized in that: described compound Nano carbon fiber doping includes Ni nano particle, and its surface is wrapped up by graphitization carbon-coating, and the average diameter of this compound Nano carbon fiber is 100 ~ 300nm.
2. a preparation method for Ni/C composite nano fiber microwave absorption described in claim 1, comprises the following steps:
Step 1: spinning solution is prepared, and adds polyacrylonitrile in dimethyl formamide (DMF), and is stirred to and dissolves completely; And then add nickel acetylacetonate and continue to be stirred to and dissolve completely, obtain even, transparent, stable spinning solution;
Step 2: spinning solution step 1 obtained moves in electrostatic spinning apparatus, carries out electrostatic spinning and obtains polymer-metal salt composite precursor fiber, and the precursor fibre dry 10 ~ 24h at 80 ~ 120 DEG C that will collect;
Step 3: under inert gas conditions, obtains composite precursor fiber after pre-oxidation, and obtains Ni/C composite nano fiber through carbonization treatment by step 2.
3. the preparation method of Ni/C composite nano fiber microwave absorption according to claim 2, is characterized in that: in spinning solution described in step 1, the mass fraction of polyacrylonitrile is 5 ~ 12%; The mass fraction of nickel acetylacetonate is 4 ~ 13%.
4. the preparation method of Ni/C composite nano fiber microwave absorption according to claim 3, it is characterized in that: described in step 2, electrostatic spinning process parameter is: voltage 10 ~ 22kV, solution advances speed 0.2 ~ 0.8mL/h, solidification distance is 15 ~ 25cm, temperature is 15 ~ 30 DEG C, and humidity is less than 60%.
5. the preparation method of Ni/C composite nano fiber microwave absorption according to claim 4, it is characterized in that: described in step 3, pre-oxidation design parameter is: temperature is 180 ~ 280 DEG C, temperature retention time 1 ~ 3h, heating rate is 1 ~ 5 DEG C/min.
6. the preparation method of Ni/C composite nano fiber microwave absorption according to claim 5, it is characterized in that: described in step 3, carbonization treatment design parameter is: temperature is 600 ~ 1300 DEG C, atmosphere is argon gas or nitrogen, temperature retention time 1 ~ 3h, and heating rate is 2 ~ 10 DEG C/min.
7. the microwave absorbing coating of Ni/C composite nano fiber microwave absorption described in an application rights requirement 1, it is characterized in that: this microwave absorbing coating take silica gel as matrix, the Ni/C composite nano fiber microwave absorption of doping 3 ~ 10wt% in silica gel, its density is only 0.8 ~ 1.0g/cm
3, microwave absorbing coating thickness is 1.2 ~ 2.0mm.
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| CN106229544A (en) * | 2016-10-08 | 2016-12-14 | 天津工业大学 | A kind of high performance lithium ionic cell cathode material Ni/C composite nano fiber and preparation method thereof |
| CN106252636A (en) * | 2016-10-08 | 2016-12-21 | 天津工业大学 | A kind of lithium ion battery hollow NiO/C nanofiber anode material and preparation method thereof |
| CN109037554A (en) * | 2018-06-26 | 2018-12-18 | 长沙矿冶研究院有限责任公司 | A kind of Ni/C composite nano-fiber membrane applied to lithium-sulfur cell and preparation method thereof and lithium-sulfur cell |
| CN111850821B (en) * | 2020-06-13 | 2022-12-09 | 北京化工大学 | Method for preparing electromagnetic wave absorbing material from hydrotalcite-based composite nanofiber |
| CN113913973A (en) * | 2021-11-12 | 2022-01-11 | 山东大学 | Ni/MnO/C composite nanofiber and preparation method and application thereof |
| CN114853095B (en) * | 2022-04-22 | 2024-02-06 | 陕西科技大学 | Preparation method of Cf/SiCNws/Ni composite material |
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