CN104213250B - NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption, microwave absorbing coating and preparation method - Google Patents
NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption, microwave absorbing coating and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of NCZFO BTO sections Magnet electroceramics composite nano fiber microwave absorption, microwave absorbing coating and preparation method, wherein absorbent is by spinel structure ferromagnetism Ni0.4Co0.2Zn0.4Fe2O4With perovskite structure ferroelectricity BaTiO3Nanocrystalline constituted；Average grain size is 20～50nm, BaTiO3Average grain size be 20～60nm, biphase crystal grain is axially uniformly distributed along fiber, and fibre diameter is about 100～300nm.Magnetoelectricity composite nano fiber prepared by the present invention almost all has strong absorption in whole 2～18GHz frequency range, have bandwidth, absorb strong, low cost and electromagnetic parameter and absorption characteristic can the advantage such as wide scope regulation and control, have good application prospect in fields such as electro-magnetic wave absorption and shielding, anti-electromagnetic interference and pollutions.
Description
Technical field
The invention belongs to electromagnetic wave absorbent material field, particularly relate to ferromagnetic/ferroelectricity composite wave-suction material with one-dimensional nano structure and preparation method thereof, refer specifically to Ni0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber microwave absorption and technology of preparing thereof.
Background technology
Along with using the electronics of G hertz frequency electromagnetic wave and developing rapidly and extensively applying of communication apparatus, the electromagnetic interference thus brought and electromagnetic radiation pollution are the most serious, and the demand of electromagnetism stealth is promoted by modern weapons equipment the most day by day simultaneously.In order to eliminate or reduce electromagnetic interference and electromagnetic pollution, and effectively reducing the radar signature signal of weaponry to improve its existence defence capability and overall operational performance, novel high-performance electromagnetic wave absorbent material has become the development focus in civilian and military field, various countries.Absorbing material depends on filling radio-radar absorber therein to the absorption of electromagnetic wave.Development along with nanotechnology, although the absorbent properties of electromagnetic wave are greatly increased and improve by the low-dimensional nanorize of conventional absorbents such as ferrite and magnetic metal material, but relatively poor due to its electromagnetic impedance match characteristic when finding to use single dielectric loss or magnetic loss absorbent, its absorbing property is the most still difficult to meet the requirement of " thin, light, wide, strong " that absorbing material performance is proposed by development of modern scientific technology.Then multiple absorbent is carried out compound nanostructured composite wave-suction material of making and becomes an important directions of current absorbing material field development.Utilize cooperative effect and the adjustable advantage of electromagnetic parameter of composite, difference absorbs frequency range, the absorbent of different loss mechanisms carries out multiple elements design, by structure composition, microscopic appearance and the electromagnetic parameter of regulation material to realize its impedance matching, reach low-density, strong absorption and wide band effect.
Ferroelectricity/ferromagnetic Multiferroic composite material is a kind of advanced material with magnetoelectricity transformation function, its magnetoelectricity transformation function is to be realized by ferroelectric phase and the ferromagnetic i.e. magnetic couplings effect of alternate product effect, and the technical field such as current measurement at magnetoelectric transducer (magnetic field, electric field detecting etc.), conductor magneto-electric energy conversion, data storage, microwave sounding and ultra-high-tension power transmission line has broad application prospects.So far people have carried out in-depth study in a large number to its magnetoelectric effect, but the ferroelectricity of this type of Multiferroic composite material, ferromagnetic coexist and its collaborative loss effect, also it is strong absorption, the important foundation of broadband microwave absorbing material simultaneously, but from the point of view of the retrieval of patent and document, the most fewer to the electromagnetic property of this type of material and the research of absorbing property, material shape is also concentrated mainly on zero dimension ferroelectricity/ferromagnetic composite granule.Result of study display ferroelectricity reveals more excellent microwave absorbing property with the composite table of ferromagnetic material, and ferroelectric nano powder body and ferromagnetic nano-powder are carried out physical mixed, obtained Co by such as A. Mandal etc.0.5Zn0.5Fe2O4/Pb(Zr0.52Ti0.48)O3(A. Mandal and C.K. Das, Electronic materials based on Co0.5Zn0.5Fe2O4/Pb(Zr0.52Ti0.48)O3
Nanocomposites, Journal of Electronic Materials, 2013,42:121-128) and Co0.2Ni0.4Zn0.4Fe2O4/
BaTiO3 (A. Mandal and C.K. Das, Effect of BaTiO3 on the
microwave absorbing properties of Co-doped Ni-Zn ferrite nanocomposites,
Journal of Applied Polymer Science, 2014, DOI:10.1002/APP.39926) composite nano-powder absorbing material, find these ferroelectricity/ferromagnetic composite nano-powder absorbance at X-band (8.2 ~ 12.4GHz) all more than 90%, minimal reflection loss reach about 42 to 48dB.
So far report is also rarely had for the electromagnetic property of one-dimensional nano structure ferroelectricity/ferromagnetic composite material such as ferroelectricity/ferromagnetic composite nano-fiber and the research of absorbing property.Compared with powder body absorbent, absorbing material containing nanofiber absorbent not only has excellent mechanical property and physicochemical property, and utilize the shape anisotropy of fiber, can also be improved it in the electromagnetic consumable of microwave frequency band and absorption efficiency, it has also become a kind of rising novel wave-absorbing material；Nanofiber is due to its one-dimensional architectural characteristic and confinement effect simultaneously, ferromagnetic and biphase the realization in microscopic dimensions of ferroelectricity can be made to be uniformly distributed, can solve the problem that the particle aggregation and heterogeneous distribution problem the most easily occurred in three-dimensional block, two-dimensional film and zero dimension powder body, it is greatly improved biphase contact area, strengthen two alternate efficient couplings and loss cooperative effect, be expected to strengthen microwave absorption intensity further and widen absorption band.Preparing oxide ceramics and the technology of complex micro nanometer fiber relative to other, method of electrostatic spinning has the advantages such as simple to operate, with low cost, efficient, has realized industrialized production in some field at present.Xie Shuhong etc. use the method for combination of sol-gel electrostatic spinning to be prepared for CoFe2O4-Pb(Zr x Ti 1-x )O3And CoFe2O4-
Pb(Zr x Ti1-x ) ferromagnetic ferroelectricity composite nano-fiber material (S.H. Xie, J.Y. Li, Y.Y. Liu, L.N.
Lan, Y.C. Zhou, Electrospinning and multiferroic properties of NiFe2O4-Pb(Zr0.52Ti0.48)O3
composite nanofibers, Journal of Applied Physics, 2008, 104:024115；S.H. Xie, J.Y. Li, Y.
Qiao, Y.Y. Liu, L.N. Lan, Y.C. Zhou, S.T. Tan, Multiferroic CoFe2O4-Pb(Zr0.52Ti0.48)O3
nanofibers by electrospinning, Applied Physics
Letters, 2008, 92:062901; CN101274844A).Be employed technical scheme comprise that with glycol methyl ether, glacial acetic acid, second alcohol and water as solvent, make ferroelectric precursor solution, ferromagnetic precursor solution and polymer solution the most respectively, then remix and the most agitated make electrospinning precursor solution, ferroelectric-ferromagnetic composite nano-fiber is prepared through electrostatic spinning molding and calcination processing after, wherein in configuration ferroelectric precursor solution processes, solution need to be aged 3 ~ 7 days, is also added into citric acid as chelating agen when configuring ferromagnetic precursor solution.Can be seen that whole preparation process still suffers from technique complex, operate relatively complicated that the shortcoming such as time-consuming long is unfavorable for large-scale production.
Therefore, developing technique and be simple and convenient to operate, low cost, be prone to the ferromagnetic ferroelectricity composite nano fiber electrostatic spinning preparation technology of large-scale production, the research for ferromagnetic/ferroelectricity composite nano fiber has great importance with application.
Summary of the invention
Goal of the invention: for the problem and shortage of above-mentioned existing existence, one chemical composition of the present invention be (n)Ni0.4Co0.2Zn0.4Fe2O4/(1–n)BaTiO3(0<n<
100mol%) and the ferromagnetic/ferroelectric ceramics composite nano fiber microwave absorption with excellent absorbing property and preparation method thereof; solve the application in electro-magnetic wave absorption field of the magnetoelectric ceramic composite nano fiber blank, and existing technology of preparing exist complex technical process, complex operation, relatively costly, be difficult to the technical problems such as large-scale production.
Technical scheme: for achieving the above object, the present invention by the following technical solutions: a kind of NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption, chemical composition be (n) Ni0.4Co0.2Zn0.4Fe2O4/(1–n)BaTiO3, 0 <n< 100 mol% are by spinel structure ferromagnetism Ni0.4Co0.2Zn0.4Fe2O4With perovskite structure ferroelectricity BaTiO3Nanocrystalline constituted；Described Ni0.4Co0.2Zn0.4Fe2O4Average grain size be 20～50nm, BaTiO3Average grain size be 20～60nm, biphase crystal grain is axially uniformly distributed along fiber, and fibre diameter is about 100～300nm.
Another object of the present invention there is provided the preparation method of a kind of above-mentioned composite nano fiber microwave absorption, comprise the following steps: slaine is first dissolved in solvent by concentration ratio by (1) according to the stoichiometric proportion of product, then add polyvinylpyrrolidone, continue stirring and directly prepare the spinning solution that composition is uniform, transparent, stable in 2～8 hours；(2) step (1) gained spinning solution is made PVP/ slaine precursor fibre through high-voltage electrostatic spinning, and be dried process at 80 ~ 100 DEG C；(3) precursor fibre that step (2) prepares is carried out heat treatment in air atmosphere, finally prepare the nanometer crystalline Ni that degree of crystallinity is high, crystal formation growth is perfect0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber.
Described slaine is nickel acetate, cobalt acetate, zinc acetate, Barium acetate, ferric acetyl acetonade and butyl titanate；Described solvent is ethanol and the mixed solvent of acetic acid composition, and ethanol is 0.25～4 with the mass ratio of acetic acid.
In spinning solution, the mass fraction of polyvinylpyrrolidone is 7～12%, and the mass fraction of slaine is 10%～18%.
In step (2), electrostatic spinning electric field intensity is 0.6～1.5kV/cm, and solution advances speed 0.2～0.8mL/h, and temperature is 15～30 DEG C, relative humidity less than 50%.
Heat treatment temperature described in step (3) is 800～1200 DEG C, and heating rate is 0.5～5 DEG C/min, and temperature retention time is 1～8 hour.
It addition, the invention also discloses a kind of microwave absorbing coating applying above-mentioned composite nano fiber microwave absorption, described composite nano fiber wave absorbent is coated uniformly on matrix, forms the coating of 2～4mm.All having strong absorption, minimal reflection loss to reach 46dB in 2～18GHz frequency ranges, the reflection loss effective Absorber Bandwidth less than 10dB almost can cover whole S-band to Ku wave band.
Beneficial effect: compared with prior art, the invention have the advantages that 1. present invention achieve the combination of ferromagnetic magnetic loss and ferroelectric dielectric loss by one-dimensional composite nano structure, the architectural characteristic and the confinement effect thereof that utilize monodimension nanometer material enhance the loss cooperative effect that ferromagnetic phase in system is alternate with ferroelectricity, it is thus achieved that high-performance magnetism electricity composite nano fiber absorbing material.2. the Ni of the present invention0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber microwave absorption has strong absorption in 4～18GHz frequency ranges, its electromagnetic parameter and Microwave Absorption Properties can be easily changed by the chemical composition of ferromagnetic phase and the ratio of ferroelectric phase and ferromagnetic phase and carry out Effective Regulation within the specific limits, has broad application prospects with fields such as radiation pollutions in electromagnetism stealth, electromagnetic shielding and anti-electromagnetic interference.3. the present invention uses the method for solution electrostatic spinning to prepare Ni0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber microwave absorption, is directly dissolved in institute's slaine and spin finish aid in solvent, it is not necessary to add other chelating agen or the most still aging, and its technical process is simple and convenient to operate, manufacturing cycle is short, low cost, utilizes large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the Ni of the embodiment of the present invention 1 preparation0.4Co0.2Zn0.4Fe2O4/BaTiO3The electron scanning micrograph of composite nano fiber；
Fig. 2 is the Ni of the embodiment of the present invention 1 preparation0.4Co0.2Zn0.4Fe2O4/BaTiO3The X-ray diffraction spectrogram of composite nano fiber；
Fig. 3 is the Ni of the embodiment of the present invention 1 preparation0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber microwave absorption microwave absorbing property curve in the range of 2 ~ 18GHz.
Detailed description of the invention
Below in conjunction with the accompanying drawings and specific embodiment, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate the present invention rather than limit the scope of the present invention, after having read the present invention, those skilled in the art all fall within the application claims limited range to the amendment of the various equivalent form of values of the present invention.
Embodiment 1:
According to ferromagnetic phase Ni0.5Zn0.5Fe2O4With ferroelectric phase BaTiO3nullMol ratio be 6: 4，Weigh 0.4062g butyl titanate respectively、0.3048g Barium acetate、0.1782g nickel acetate、0.0892g cobalt acetate、0.1572g zinc acetate、In the mixed solvent that 1.2645g ferric acetyl acetonade joins 10.7800g acetic acid and 4.6200g ethanol is formed (ethanol is about 0.43 with the mass ratio of acetic acid)，After at room temperature magnetic agitation to all slaines are completely dissolved，Weigh 1.6000g polyvinylpyrrolidone (PVP again，Mean molecule quantity is 1300000) join in above-mentioned solution，Continue magnetic agitation and within about 2 hours, formed homogeneous、Transparent、Stable spinning precursor solution，Wherein the weight/mass percentage composition of PVP is 8%，The weight/mass percentage composition of all slaines is 15%.The spinning solution prepared is moved in the electrostatic spinning apparatus (see Chinese patent 201110201848.7) being made up of DC high-voltage power supply, reservoir, spinning head, syringe pump and catcher, it is 0.75kV/cm (i.e. voltage 15kV, receiving range 20cm) in electric field intensity, solution feed speed is 0.45mL/h, indoor temperature is 20～25 DEG C, carries out electrostatic spinning and make PVP/ slaine composite precursor fiber under conditions of relative humidity 30～45%.The precursor fibre collected fully is placed in program control electric furnace in 100 DEG C in an oven after drying, it is heated to 1050 DEG C of roastings 3 hours with the speed of 1 DEG C/min by room temperature in air atmosphere, naturally cools to room temperature with stove afterwards and obtain chemical composition for (60mol%) Ni0.4Co0.2Zn0.4Fe2O4/(40mol%)BaTiO3Ferromagnetic/ferroelectricity composite nano fiber microwave absorption.Obtained composite nano fiber microscopic appearance is good, and thickness is more uniform, and average diameter is about 180nm (see figure 1), by spinel structure Ni0.5Zn0.5Fe2O4With perovskite structure BaTiO3Two phase compositions, without other dephasigns (as shown in Figure 2), ferromagnetic phase Ni0.4Co0.2Zn0.4Fe2O4Average grain size be 50nm, ferroelectric phase BaTiO3Average grain size be 53nm.When absorbent loading is 70% (mass fraction), when coating layer thickness is 2.0mm, monolayer (60mol%) Ni0.4Co0.2Zn0.4Fe2O4/(40mol%)BaTiO3The minimum reflectance of-silica gel microwave absorbing coating reaches 46dB at 14.2GHz.
Embodiment 2:
Basic process is with embodiment 1, and difference is: Ni0.4Co0.2Zn0.4Fe2O4With BaTiO3Mol ratio 5:5, butyl titanate, Barium acetate, nickel acetate, cobalt acetate, zinc acetate, the quality of ferric acetyl acetonade are respectively 0.5306g, 0.3983g, 0.1552g, 0.0777g, 0.1369g and 1.1013g, and the chemical composition of the ferromagnetic/ferroelectricity composite nano fiber microwave absorption obtained is (50mol%) Ni0.4Co0.2Zn0.4Fe2O4/(50mol%)BaTiO3, its average diameter is about 270nm, ferromagnetic phase Ni0.5Zn0.5Fe2O4Average grain size be about 56nm, ferroelectric phase BaTiO3Average grain size be about 60nm；When absorbent loading is 70% (mass fraction, lower same), when coating layer thickness is 3.0mm, monolayer (50mol%) Ni0.4Co0.2Zn0.4Fe2O4/(50mol%)BaTiO3The minimum reflectance of-silica gel microwave absorbing coating reaches 41dB at 5.1GHz.
Embodiment 3:
Basic process is with embodiment 1, and difference is: Ni0.4Co0.2Zn0.4Fe2O4With BaTiO3Mol ratio 9:1, butyl titanate, Barium acetate, nickel acetate, cobalt acetate, zinc acetate, the quality of ferric acetyl acetonade are respectively 0.0891g, 0.0669g, 0.2366g, 0.1184g, 0.2087g and 1.6789g, and the chemical composition of the ferromagnetic/ferroelectricity composite nano fiber microwave absorption obtained is (90mol%) Ni0.4Co0.2Zn0.4Fe2O4/(10mol%)BaTiO3, its average diameter is about 260nm, ferromagnetic phase Ni0.5Zn0.5Fe2O4Average grain size be about 38nm, ferroelectric phase BaTiO3Average grain size be about 20nm；When absorbent loading is 70%, and coating layer thickness is 3.5mm, monolayer (90mol%) Ni0.4Co0.2Zn0.4Fe2O4/(10mol%)BaTiO3The minimum reflectance of-silica gel microwave absorbing coating reaches 24dB at 8.9GHz.
Embodiment 4:
Basic process is with embodiment 1, and difference is: absorbent loading is 60%, and when coating layer thickness is 2.3mm, its minimum reflectance reaches 20.8dB at 8.3GHz.
In the present invention, spinel type ferrite is the microwave absorbing material that a kind of performance is the most excellent and application is ripe, has low-dielectric, high resistivity and is prone to the advantages such as coupling, and having higher non-oxidizability and decay resistance than magnetic metal material.The spinel type ferrite of fiber shape is also with the shape anisotropy of its uniqueness and overcomes spinel type ferrite resonant frequency and the problem such as the Snoek limit is low, improve this type of material in the pcrmeability of microwave frequency band and magnetic loss, and then be conducive to strengthening microwave absorbing property.Compared to existing spinel structure ferrite and perovskite structure ferroelectric physical mixed type composite granule absorbing material, the spinel structure ferrite of the present invention/perovskite structure ferroelectric composite nano fiber microwave absorption has broader effective adsorption frequency scope.For physical mixed type composite granule, the contact gear ratio of ferromagnetic and ferroelectric phase is loosely, and there is the phenomenons such as uneven, and by the composite nano fiber prepared by sol-gel and electrostatic spinning process, distributing very evenly of ferromagnetic and ferroelectric phase, and contact is closely, this is possible not only to strengthen the ferromagnetic magneto-electric coupled effect alternate with ferroelectricity, and what is more important can form good electromagnetic matching on a microscopic scale, enable more electromagnetic wave to be efficiently entering inside wave-absorber and be attenuated and absorb, thus result in effective absorption band and substantially widen.
Claims (5)
1. a preparation method for NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption, should
The chemical composition of NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption is
(n)Ni0.4Co0.2Zn0.4Fe2O4/(1–n)BaTiO3, 0 < n < 100mol%, it is by spinel structure ferromagnetism
Ni0.4Co0.2Zn0.4Fe2O4With perovskite structure ferroelectricity BaTiO3Nanocrystalline constituted；Described Ni0.4Co0.2Zn0.4Fe2O4
Average grain size be 20～50nm, BaTiO3Average grain size be 20～60nm, biphase crystal grain is along fiber axis
To being uniformly distributed, fibre diameter is 100～300nm；Described preparation method comprises the following steps:
(1) according to the stoichiometric proportion of product, slaine is first dissolved in solvent by concentration ratio, then adds poly-second
Alkene pyrrolidone, continues stirring and directly prepares the spinning solution that composition is uniform, transparent, stable in 2～8 hours；
(2) step (1) gained spinning solution is made PVP/ slaine precursor fibre through high-voltage electrostatic spinning, and
It is dried process at 80～100 DEG C；
(3) precursor fibre that step (2) prepares is carried out heat treatment in air atmosphere, finally prepare degree of crystallinity high,
Crystal formation grows perfect nanometer crystalline Ni0.4Co0.2Zn0.4Fe2O4/BaTiO3Composite nano fiber；Described slaine is acetic acid
Nickel, cobalt acetate, zinc acetate, Barium acetate, ferric acetyl acetonade and butyl titanate；Described solvent is ethanol and acetic acid composition
Mixed solvent, the mass ratio of ethanol and acetic acid is 0.25～4.
The system of NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption the most according to claim 1
Preparation Method, it is characterised in that: in spinning solution, the mass fraction of polyvinylpyrrolidone is 7～12%, the matter of slaine
Amount mark is 10%～18%.
The system of NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption the most according to claim 2
Preparation Method, it is characterised in that: in step (2), electrostatic spinning electric field intensity is 0.6～1.5kV/cm, and solution advances speed
0.2～0.8mL/h, temperature is 15～30 DEG C, relative humidity less than 50%.
The system of NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave absorption the most according to claim 2
Preparation Method, it is characterised in that: the heat treatment temperature described in step (3) is 800～1200 DEG C, heating rate be 0.5～
5 DEG C/min, temperature retention time is 1～8 hour.
5. the NCZFO-BTO sections Magnet electroceramics composite nano fiber microwave that a kind is applied obtained by claim 1 is inhaled
Receive agent microwave absorbing coating, it is characterised in that: described composite nano fiber wave absorbent is coated uniformly on matrix, formed 2～
The coating of 4mm.
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| EP3553830A4 (en) * | 2017-10-24 | 2020-03-11 | Huazhong University of Science and Technology | Ferroelectric-enhanced solar cell and preparation method therefor |
| WO2021076536A1 (en) * | 2019-10-17 | 2021-04-22 | Rogers Corporation | Nanocrystalline cobalt doped nickel ferrite particles, method of manufacture, and uses thereof |
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| CN101274844A (en) * | 2008-05-16 | 2008-10-01 | 湘潭大学 | Preparation for ferroelectric-ferromagnetic composite nano-fiber |
| CN102153338A (en) * | 2010-12-03 | 2011-08-17 | 浙江大学 | Seepage type barium titanate-nickel zinc ferrite composite ceramic wave absorption material and preparation method thereof |
| CN102418171B (en) * | 2011-07-26 | 2014-07-16 | 南京工业大学 | Nickel zinc ferrite microwave absorbent and preparation method thereof |
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| EP3553830A4 (en) * | 2017-10-24 | 2020-03-11 | Huazhong University of Science and Technology | Ferroelectric-enhanced solar cell and preparation method therefor |
| WO2021076536A1 (en) * | 2019-10-17 | 2021-04-22 | Rogers Corporation | Nanocrystalline cobalt doped nickel ferrite particles, method of manufacture, and uses thereof |
| US11869693B2 (en) | 2021-05-07 | 2024-01-09 | Imam Abdulrahman Bin Faisal University | Magnetoelectric multiferroic nanocomposite |
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