CN103436994A - Fe-Ni alloy/C composite nanofiber microwave absorbent, preparation method and application of absorbent - Google Patents
Fe-Ni alloy/C composite nanofiber microwave absorbent, preparation method and application of absorbent Download PDFInfo
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Abstract
The invention discloses a high-performance Fe-Ni alloy/C composite nanofiber microwave absorbent and a preparation method thereof. The absorbent is prepared by electrostatic spinning and a post heat treatment one-step method; a synthetic technology is simple; the mean diameters of obtained fibers are 200-400nm; generated Fe-Ni alloy nanoparticles are relatively uniformly distributed in or on the surfaces of the carbon nanofibers, and are wrapped by a graphitized carbon layer; and the absorbent has better oxidation resistance and corrosion resistance. The density of a wave absorption coating prepared by compositing with silica gel is only 0.8-1.0g/cm<3> when the content of the absorbent is 3-10wt%; when the thickness of the coating is 1.2-2.0mm, the minimum reflection loss of the absorbent reaches -40dB to -95dB; the effective absorption band width with the reflection loss less than -10dB at 2-18GHz reaches 10.2GHz;a whole Ku wave band and an X wave band are covered; and the absorbent has the advantages of light mass, broadband, strong absorption, convenient adjustment of electromagnetic parameters, and the like.
Description
Technical field
The invention belongs to the electromagnetic wave absorbent material field, relate in particular to a kind of Novel broadband, lightweight, absorb one-dimensional magnetic carbon-based nano composite wave-suction material and preparation method thereof by force.
Background technology
Electromagnetic wave absorbent material military project and civil aspect all have a wide range of applications, become that the military equipment electromagnetism is stealthy, the focus of the technical field research such as electromagnetic shielding and anti-electromagnetic-radiation interference.Absorbing material mainly depends on filling radio-radar absorber wherein to electromagnetic absorption.Development along with nanometer technology, although the tradition absorbent makes it to electromagnetic absorbent properties, be greatly increased and improve as the low-dimensional nanometer of ferrite and magnetic metal material, the one-component absorbent still is difficult to meet the requirement of " thin thickness, quality are light, bandwidth, absorption strong " that development of modern scientific technology proposes absorbing material performance.So it may be to realize one of effective way that absorbing property essence breaks through that multiple absorbent is carried out to the compound nanostructured composite wave-suction material of making, and is also an important directions of absorbing material future development simultaneously.Utilize cooperative effect and the adjustable advantage of electromagnetic parameter of composite, the absorbent that difference is absorbed to frequency range, different loss mechanism carries out polynary compound, structure composition, microscopic appearance and electromagnetic parameter by regulating material to be to realize its impedance matching, thereby to reach low-density, to absorb and wide band effect by force.
The tradition absorbing material is often because density is large, poor stability or absorption band is narrow, matching thickness is large etc. that shortcoming has restricted its development and application.Carbon nano-fiber, as a kind of important absorbing material, relies on its low-density, high temperature resistant, the anticorrosive and excellent advantages such as electric property to be subject to people's favor.Yet, as typical dielectric loss material, its electromagnetic matching is poor, and electromagnetic wave is had to strong reflectivity.At present, carbon nano-fiber absorbing material in application mostly is surperficial cladded magnetic metal coating or magnetic oxide coating, to reach, carbon nano-fiber is carried out the magnetic modification and improves the purpose of its electromagnetic matching, the performance when absorbing property of the composite obtained all is better than single the use.But due to the magnetic metal that plates or deposit or the alloy coat surface that is positioned at carbon fiber, it is anti-oxidant and decay resistance is poor, thereby has limited to a certain extent the normal use of this type of magnetic carbon fiber composite under some complex environments.
Summary of the invention
Goal of the invention: for the problem and shortage of above-mentioned existing existence, the purpose of this invention is to provide a kind of magnetic carbon fiber absorbing material and the simple novel high-performance one-dimensional magnetic of technique metal/carbon Composite Microwave absorbent and preparation method thereof of being different from the past.The prepared Fe-Ni alloy of the present invention/C composite nano fiber, average diameter is between 200～400nm, it is inner or surperficial that the Fe-Ni alloy nanoparticle is distributed in carbon nano-fiber more equably, and wrapped up by the graphitization carbon-coating, there is stronger anti-oxidant and corrosion resistance, be a kind of light weight, wideband, absorb by force, electromagnetic parameter is adjustable and the electromagnetic wave absorbent material of good combination property.When absorbent contents is 3～10wt%, coating layer thickness while being 1.2～2.0mm, the density of silica gel complex is only 0.8～1.0g/cm
3, its microwave absorption peak value Da is Dao – 40 Zhi – 95dB, and the frequency range of 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 the Fe-Ni alloy nanoparticle, and top layer is wrapped up by the graphitization carbon-coating, the average diameter of this compound Nano carbon fiber is 200～400nm.
The preparation method of a kind of above-mentioned iron-nickel alloy/carbon composite nano-fiber microwave absorption comprises the following steps:
Step 1: the spinning solution preparation adds polyacrylonitrile, and is stirred to dissolving fully in dimethyl formamide (DMF); And then add ferric acetyl acetonade and nickel acetylacetonate and continue to stir dissolving fully, obtain even, transparent, stable spinning solution;
Step 2: the spinning solution that step 1 is obtained moves in electrostatic spinning apparatus, and carry out electrostatic spinning and obtain polymer-metal salt composite precursor fiber, and by the precursor fibre dry 10～24h under 80～120 ℃ collected;
Step 3: under inert gas conditions, step 2 is obtained to the composite precursor fiber after pre-oxidation, and obtain the Fe-Ni/C composite nano fiber through carbonization treatment.
As preferably, in the described spinning solution of 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, the described electrostatic spinning process parameter of step 2 is: voltage 10～22kV, and solution advances speed 0.2～0.8mL/h, and curing distance is 15～25cm, and temperature is 15～30 ℃, and humidity is less than 60%.
As preferably, the described pre-oxidation design parameter of step 3 is: temperature is 180～280 ℃, temperature retention time 1～3h, and heating rate is 1～5 ℃/min.
As preferably, the described carbonization treatment design parameter of step 3 is: temperature is 600～1300 ℃, and atmosphere is argon gas or nitrogen, temperature retention time 1～3h, and heating rate is 2～10 ℃/min.
A kind of microwave absorbing coating based on above-mentioned Fe-Ni alloy/C composite nano fiber microwave absorption, this microwave absorbing coating be take silica gel as matrix, 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 has the following advantages: the prepared Fe-Ni alloy of the present invention/C composite nano fiber microwave absorbing material not only have lightweight, frequency range is wide, absorb the characteristics such as strong, but also there is stronger anti-oxidant and corrosion resistance, magnetic Fe-the introducing of Ni alloy significantly improves and has improved the absorbing property of carbon nano-fiber, and the technical field such as, electromagnetic shielding stealthy at electromagnetism and anti-electromagnetic-radiation interference has broad application prospects; The present invention adopt electrostatic spinning in conjunction with later stage heat treatment process one-step synthesis Fe-Ni alloy/C composite nano fiber, the syntheti c route proposed can be expanded easily for constructing the magnetic carbon fiber microwave absorption containing other magnetic metals or alloy material; Method with respect to other for the preparation of the magnetic carbon fiber composite, it is simple that technology of preparing of the present invention has technique, with low cost, and productive rate, than high, can prepare target product Fe-Ni alloy/C composite nano fiber continuously in a large number.
The accompanying drawing explanation
The SEM photo of the Fe-Ni/C composite nano fiber that Fig. 1 is the embodiment of the present invention 2 preparations;
The XRD spectra of the Fe-Ni/C composite nano fiber that Fig. 2 is the embodiment of the present invention 2 preparations;
The Fe-Ni/C composite nano fiber that Fig. 3 is the embodiment of the present invention 3 preparations and the reflection loss curve of silica gel complex.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
The method of the Fe-Ni of preparation alloy provided by the invention/C composite nano fiber microwave absorption mainly comprises electrostatic spinning process and pre-oxidation and the carbonization treatment of the preparation of solution, precursor fibre.Its concrete steps are:
(1) by a certain amount of polyacrylonitrile (PAN, mean molecule quantity 150000) join in appropriate solvent dimethyl formamide (DMF), in 50～70 ℃ of heating water baths magnetic agitation 2～5h to PAN, dissolve fully, and then add a certain amount of ferric acetyl acetonade and nickel acetylacetonate, continue at normal temperatures magnetic agitation 10～15h and make 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, be that 10～22kV (preferably 11～17kV), receiving range are that 15～25cm (preferably 18～23cm), solution delivery rate are that 0.2～0.8mL/h (preferably 0.3～0.6mL/h), environment temperature are that 15～30 ℃, humidity are less than and carry out electrostatic spinning under 60% condition and make PAN/ ferric acetyl acetonade nickel/ferric acetyl acetonade composite precursor fiber at voltage, and the precursor fibre of collecting is put into to baking oven in 80～120 ℃ of drying 10～24h.
(3) dried precursor fibre is risen to 180～280 ℃ (preferably 220～260 ℃) with the speed of 1～5 ℃/min (preferably 2～3 ℃/min) by room temperature in air atmosphere and carry out pre-oxidation, temperature retention time 1～3h, naturally cool to room temperature with stove afterwards.
(4) fiber sample after pre-oxidation is heated to 600～1300 ℃ and be incubated 1～3h and carry out carbonization treatment with the speed of 2～10 ℃/min (preferably 3～6 ℃/min) by room temperature again under argon gas or nitrogen atmosphere, obtains Fe-Ni/C composite nano fiber microwave absorption naturally cool to room temperature under argon gas or nitrogen atmosphere after.
Embodiment 1
0.7g PAN is joined in the conical flask that fills 8.6g DMF, in 50 ℃ of heating water baths magnetic agitation 3h to PAN, dissolve fully, and then add 0.5133g ferric acetyl acetonade and 0.1867 nickel acetylacetonate, continue at normal temperatures magnetic agitation 15h and make 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, be that 12kV, receiving range are that 23cm, solution delivery rate are that 0.3mL/h, spinnerette diameters 0.8mm, environment temperature are to carry out electrostatic spinning under 20～25 ℃, the humidity condition that is 35～45% to make PAN/ ferric acetyl acetonade nickel composite precursor fiber at voltage, and the precursor fibre of collecting is put into to baking oven in 80 ℃ of dry 10h.Dried precursor fibre is risen to 240 ℃ with the speed of 2 ℃/min by room temperature in air atmosphere and carry out pre-oxidation, temperature retention time 3h, naturally cool to room temperature with stove afterwards.Fiber sample after pre-oxidation is heated to 1200 ℃ and be incubated 1h and carry out carbonization treatment with the speed of 5 ℃/min by room temperature again under argon gas atmosphere, obtain Fe-Ni alloy/C composite nano fiber microwave absorption naturally cool to room temperature under argon gas atmosphere after, its average diameter is about 260nm.Take silica gel as matrix, prepared Fe-Ni alloy/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, Da is Dao – 42dB in its minimal reflection loss, 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.Different: carburizing temperature is 1000 ℃, and the average diameter of the Fe-Ni alloy obtained/C composite nano fiber is about 280nm; When coating layer thickness is 1.9mm, Da is Dao – 41dB in its minimal reflection loss, and effectively Absorber Bandwidth is 9.2GHz, and frequency range is 8.8～18GHz.
Embodiment 3
Basic process is with embodiment 1.Different: in spinning solution, the quality of ferric acetyl acetonade and nickel acetylacetonate is respectively 0.7333g and 0.2667g, and slaine content is 10wt%, and carburizing temperature is 1000 ℃, and the average diameter of the Fe-Ni alloy of acquisition/C composite nano fiber is about 250nm; When the absorbent useful load is 5wt%, coating layer thickness while being 1.7mm, 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.Different: 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, slaine content 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 ℃, and carburizing temperature is 1000 ℃, and the average diameter of the Fe-Ni alloy obtained/C composite nano fiber is about 450nm; When the absorbent useful load is 5wt%, coating layer thickness while being 1.7mm, minimal reflection loss Wei – 46dB, effective Absorber Bandwidth 8.1GHz, frequency range is 9.9～18GHz.
Embodiment 5
Basic process is with embodiment 1.Different: the quality of ferric acetyl acetonade and nickel acetylacetonate is respectively 0.4052g and 0.2948g, and Fe is 1:1 with the ratio of Ni amount of substance, and carburizing temperature is 1000 ℃, and the average diameter of the Fe-Ni alloy of acquisition/C composite nano fiber is about 240nm; When the absorbent useful load is 5wt%, coating layer thickness while being 1.7mm, minimal reflection loss Wei – 40dB, effective Absorber Bandwidth 8.5GHz, frequency range is 9.5～18GHz.
The present invention adopt electrostatic spinning in conjunction with later stage heat treatment one-step synthesis magnetic Fe-Ni alloy/carbon composite nano-fiber, preparation technology is simple, the Fe-Ni alloy nano particle is embedded in carbon nano-fiber comparatively equably, and wrapped up by the graphitization carbon-coating, stopped and the contacting of air, greatly improved its anti-oxidant and corrosion resistance, prepared Fe-Ni alloy/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 that the chemical composition by changing precursor fibre and pre-oxidation and carburizing temperature can regulate and control composite nano fiber is the content of C and Fe-Ni alloy, and then effectively regulates its microwave electromagnetic parameter and absorption characteristic.
Claims (7)
1. Fe-Ni alloy/C composite nano fiber microwave absorption, it is characterized in that: described compound Nano carbon fiber includes the Fe-Ni alloy nanoparticle, and its top layer is wrapped up by the graphitization carbon-coating, and the average diameter of this compound Nano carbon fiber is 200～400nm.
2. the preparation method of the described Fe-Ni alloy of claim 1/C composite nano fiber microwave absorption comprises the following steps:
Step 1: the spinning solution preparation adds polyacrylonitrile, and is stirred to dissolving fully in dimethyl formamide (DMF); And then add ferric acetyl acetonade and nickel acetylacetonate and continue to be stirred to dissolving fully, obtain even, transparent, stable spinning solution;
Step 2: the spinning solution that step 1 is obtained moves in electrostatic spinning apparatus, and carry out electrostatic spinning and obtain polymer-metal salt composite precursor fiber, and by the precursor fibre dry 10～24h under 80～120 ℃ collected;
Step 3: under inert gas conditions, step 2 is obtained to the composite precursor fiber after pre-oxidation, and obtain the Fe-Ni/C composite nano fiber through carbonization treatment.
3. the preparation method of Fe-Ni alloy/C composite nano fiber microwave absorption according to claim 2, it is characterized in that: in the described spinning solution of 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 composite nano fiber microwave absorption according to claim 2, it is characterized in that: the described electrostatic spinning process parameter of step 2 is: voltage 10～22kV, solution advances speed 0.2～0.8mL/h, curing distance is 15～25cm, temperature is 15～30 ℃, and humidity is less than 60%.
5. the preparation method of Fe-Ni alloy/C composite nano fiber microwave absorption according to claim 2, it is characterized in that: the described pre-oxidation design parameter of step 3 is: temperature is 180～280 ℃, temperature retention time 1～3h, heating rate is 1～5 ℃/min.
6. the preparation method of Fe-Ni alloy/C composite nano fiber microwave absorption according to claim 2, it is characterized in that: the described carbonization treatment design parameter of step 3 is: temperature is 600～1300 ℃, atmosphere is argon gas or nitrogen, temperature retention time 1～3h, and heating rate is 2～10 ℃/min.
7. an application rights requires the microwave absorbing coating of 1 described Fe-Ni alloy/C composite nano fiber microwave absorption, it is characterized in that: this microwave absorbing coating be take silica gel as matrix, the Fe-Ni alloy of the 3～10wt%/C composite nano fiber microwave absorption that adulterates in silica gel, coating density is 0.8～1.0g/cm
3.
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