CN103436994B - Fe-Ni alloy/C/C composite nano fiber microwave absorption, preparation method and application thereof - Google Patents
Fe-Ni alloy/C/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 Fe-Ni alloy/C/C composite nano fiber microwave absorption and preparation method thereof, electrostatic spinning is adopted to obtain in conjunction with Post isothermal treatment one-step method, synthesis technique is simple, gained average fibre diameter is 200 ~ 400nm, it is inner or surperficial that the Fe-Ni alloy/C nano particle generated comparatively is uniformly distributed in carbon nano-fiber, 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 – 40 Zhi – 95dB, reaches 10.2GHz at effective Absorber Bandwidth of 2 ~ 18GHz scope internal reflection loss little Yu – 10dB, covers whole Ku wave band and X-band; 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 and preparation method thereof in the past.Fe-Ni alloy/C obtained by the present invention/C composite nano fiber, average diameter is between 200 ~ 400nm, it is inner or surperficial that Fe-Ni alloy/C nano particle is distributed in carbon nano-fiber more equably, and wrap up by graphitization carbon-coating, there is stronger anti-oxidant and corrosion resistance, be a kind of light weight, wideband, strong absorption, electromagnetic parameter is adjustable and the electromagnetic wave absorbent material of good combination property.When absorbent contents be 3 ~ 10wt%, coating layer thickness be 1.2 ~ 2.0mm time, the density of silica gel complex is only 0.8 ~ 1.0g/cm
3, the frequency range of its microwave absorption peak Da Dao – 40 Zhi – 95dB, 2 ~ 18GHz scope internal reflection loss little Yu – 10dB reaches 10.2GHz, covers whole Ku wave band and X-band.
Technical scheme: for achieving the above object, the present invention is by the following technical solutions: a kind of iron-nickel alloy/carbon composite nano-fiber microwave absorption, described compound Nano carbon fiber doping includes Fe-Ni alloy/C nano particle, and top layer is wrapped up by graphitization carbon-coating, the average diameter of this compound Nano carbon fiber is 200 ~ 400nm.
A preparation method for above-mentioned iron-nickel alloy/carbon 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 ferric acetyl acetonade and nickel acetylacetonate and continue to stir 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 Fe-Ni/C composite nano fiber through carbonization treatment by step 2.
As preferably, in spinning solution described in step 1, the mass fraction of polyacrylonitrile is 5 ~ 12%; The gross mass mark of ferric acetyl acetonade and nickel acetylacetonate is 4 ~ 13%.
As preferably, 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%.
As preferably, 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.
As preferably, 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.
A kind of microwave absorbing coating based on above-mentioned Fe-Ni alloy/C/C composite nano fiber microwave absorption, this microwave absorbing coating is matrix with silica gel, the Fe-Ni/C composite nano fiber microwave absorption of the 3 ~ 10wt% that adulterates in silica gel.
Beneficial effect: compared with prior art, the present invention had the following advantages: the Fe-Ni alloy/C prepared by the present invention/C composite nano fiber microwave absorbing material 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 Fe-Ni alloy/C 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 Fe-Ni alloy/C/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 Fe-Ni alloy/C/C composite nano fiber continuously in a large number.
Accompanying drawing explanation
Fig. 1 is the SEM photo of Fe-Ni/C composite nano fiber prepared by the embodiment of the present invention 2;
Fig. 2 is the XRD spectra of Fe-Ni/C composite nano fiber prepared by the embodiment of the present invention 2;
Fig. 3 is the Fe-Ni/C composite nano fiber of the embodiment of the present invention 3 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 method preparing Fe-Ni alloy/C/C composite nano fiber microwave absorption provided by the invention 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 ferric acetyl acetonade and 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 ferric acetyl acetonade and 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/ ferric acetyl acetonade nickel/ferric acetyl acetonade 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 Fe-Ni/C composite nano fiber microwave absorption.
Embodiment 1
0.7g PAN is joined in the conical flask filling 8.6g DMF, in 50 DEG C of heating water baths and magnetic agitation 3h to PAN dissolve completely, and then add 0.5133g ferric acetyl acetonade and 0.1867 nickel acetylacetonate, continue magnetic agitation 15h at normal temperatures and obtain even, transparent, stable spinning solution.In this spinning solution, the mass fraction of PAN is 7%, and the mass fraction of slaine is 7%, and all the other are solvent DMF.The spinning solution prepared is moved in electrostatic spinning apparatus, voltage be 12kV, receiving range is 23cm, solution feeding rate is 0.3mL/h, spinnerette diameters 0.8mm, environment temperature is 20 ~ 25 DEG C, humidity is carried out electrostatic spinning and made PAN/ ferric acetyl acetonade nickel 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 240 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 1200 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 Fe-Ni alloy/C/C composite nano fiber microwave absorption after naturally cooling to room temperature under an argon atmosphere, its average diameter is about 260nm.Take silica gel as matrix, prepared Fe-Ni alloy/C/C composite nano fiber is that absorbent is made into microwave absorbing coating, when absorbent contents is 3wt%, when coating layer thickness is 1.6mm, its minimal reflection loss Da Dao – 42dB, effective Absorber Bandwidth of 2 ~ 18GHz scope internal reflection rate little Yu – 10dB is 7.8GHz, and frequency range is 10.2 ~ 18GHz.
Embodiment 2
Basic process is with embodiment 1.Unlike: carburizing temperature is 1000 DEG C, and the average diameter of the Fe-Ni alloy/C obtained/C composite nano fiber is about 280nm; When coating layer thickness is 1.9mm, its minimal reflection loss Da Dao – 41dB, effective Absorber Bandwidth is 9.2GHz, and frequency range is 8.8 ~ 18GHz.
Embodiment 3
Basic process is with embodiment 1.Unlike: in spinning solution, the quality of ferric acetyl acetonade and nickel acetylacetonate is respectively 0.7333g and 0.2667g, and metal salt concentration is 10wt%, and carburizing temperature is 1000 DEG C, and the average diameter of the Fe-Ni alloy/C/C composite nano fiber of acquisition is about 250nm; When absorbent useful load be 5wt%, coating layer thickness be 1.7mm time, minimal reflection loss Wei – 95dB, effective Absorber Bandwidth 7.9GHz, frequency range is 9.5 ~ 17.4GHz.
Embodiment 4
Basic process is with embodiment 1.Unlike: in spinning solution, the content of PAN is 8wt%, the quality of ferric acetyl acetonade and nickel acetylacetonate is respectively 0.66g and 0.24g, metal salt concentration is 9wt%, voltage is 15kV, and receiving range is 15cm, and fltting speed is 0.5mL/h, spinnerette diameters 0.9mm, Pre oxidation is 250 DEG C, and carburizing temperature is 1000 DEG C, and the average diameter of the Fe-Ni alloy/C obtained/C composite nano fiber is about 450nm; When absorbent useful load be 5wt%, coating layer thickness be 1.7mm time, minimal reflection loss Wei – 46dB, effective Absorber Bandwidth 8.1GHz, frequency range is 9.9 ~ 18GHz.
Embodiment 5
Basic process is with embodiment 1.Unlike: the quality of ferric acetyl acetonade and nickel acetylacetonate is respectively 0.4052g and 0.2948g, and the ratio of Fe and Ni amount of substance is 1:1, and carburizing temperature is 1000 DEG C, and the average diameter of the Fe-Ni alloy/C/C composite nano fiber of acquisition is about 240nm; When absorbent useful load be 5wt%, coating layer thickness be 1.7mm time, minimal reflection loss Wei – 40dB, effective Absorber Bandwidth 8.5GHz, frequency range is 9.5 ~ 18GHz.
The present invention's magnetic Fe-Ni alloy/C/carbon composite nano-fiber that adopted electrostatic spinning in conjunction with Post isothermal treatment one-step synthesis, preparation technology is simple, Fe-Ni alloy/C 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 Fe-Ni alloy/C/C composite nano fiber is the electromagnetic wave absorbent material of a kind of light weight, wideband, strong absorption, high comprehensive performance.And the composition of composite nano fiber and the content of C and Fe-Ni alloy/C can be regulated and controled by changing the chemical composition of precursor fibre and pre-oxidation and carburizing temperature, and then effectively regulate its Micro-wave low-noise transistor and absorption characteristic.
Claims (7)
1. Fe-Ni alloy/C/C composite nano fiber microwave absorption, it is characterized in that: described compound Nano carbon fiber includes Fe-Ni alloy/C nano particle, its top layer is wrapped up by graphitization carbon-coating, and the average diameter of this compound Nano carbon fiber is 200 ~ 400nm.
2. a preparation method for Fe-Ni alloy/C described in claim 1/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 ferric acetyl acetonade and 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 Fe-Ni/C composite nano fiber through carbonization treatment by step 2.
3. the preparation method of Fe-Ni alloy/C/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 gross mass mark of ferric acetyl acetonade and nickel acetylacetonate is 4 ~ 13%.
4. the preparation method of Fe-Ni alloy/C/C composite nano fiber microwave absorption according to claim 2, 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 Fe-Ni alloy/C/C composite nano fiber microwave absorption according to claim 2, 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 Fe-Ni alloy/C/C composite nano fiber microwave absorption according to claim 2, 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 Fe-Ni alloy/C/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, Fe-Ni alloy/C/C composite nano fiber the microwave absorption of doping 3 ~ 10wt% in silica gel, coating density is 0.8 ~ 1.0g/cm
3.
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