CN104213250A - NCZFO-BTO-type ferromagnetic-ferroelectric ceramic composite nano fiber wave absorbent, wave absorbing coating and preparation method - Google Patents

NCZFO-BTO-type ferromagnetic-ferroelectric ceramic composite nano fiber wave absorbent, wave absorbing coating and preparation method Download PDF

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CN104213250A
CN104213250A CN201410337943.3A CN201410337943A CN104213250A CN 104213250 A CN104213250 A CN 104213250A CN 201410337943 A CN201410337943 A CN 201410337943A CN 104213250 A CN104213250 A CN 104213250A
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composite nano
nano fiber
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ferroelectric
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CN104213250B (en
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向军
李佳乐
叶芹
刘敏
徐加焕
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Zhejiang Runyou New Material Technology Co ltd
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Jiangsu University of Science and Technology
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Abstract

The invention discloses an NCZFO-BTO-type ferromagnetic-ferroelectric ceramic composite nano fiber wave absorbent, a wave absorbing coating and a preparation method. The wave absorbent is formed by a spinel-structured ferromagnetic Ni0.4Co0.2Zn0.4Fe2O4 and a perovskite-structure ferroelectric BaTiO3 nanocrystalline. The Ni0.4Co0.2Zn0.4Fe2O4 is 20-50 nm in average grain size. The BaTiO3 is 20-60 nm in average grain size. The grains of the two phases are uniformly distributed in an axial direction of the fiber. A diameter of the fiber is about 100-300 nm. The ferromagnetic-ferroelectric composite nano fiber has strong absorption in almost all of a frequency band of 2-18 GHz. The ferromagnetic-ferroelectric composite nano fiber is wide in frequency band, is strong in absorption, is low in cost, has a widely controllable range in electromagnetic parameters and microwave absorption characteristics, and has an excellent application prospect in the fields of absorption and shield of electromagnetic waves and resistance of electromagnetic interference and pollution.

Description

NCZFO-BTO sections magnet electroceramics composite nano fiber microwave absorption, microwave absorbing coating and preparation method
Technical field
The invention belongs to electromagnetic wave absorbent material field, particularly relate to ferromagnetic/ferroelectric composite wave-suction material with one-dimensional nano structure and preparation method thereof, specifically refer to Ni 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3composite nano fiber microwave absorption and technology of preparing thereof.
Background technology
Along with the develop rapidly and the extensive use that use the electromagnetic electronics of G hertz frequency and communication apparatus, the electromagnetic interference brought thus and electromagnetic radiation pollution are also serious all the more, and modern weapons equipment also promotes day by day to the demand of electromagnetism stealth simultaneously.In order to eliminate or reduce electromagnetic interference and electromagnetic pollution, and the radar signature signal of effective reduction weaponry is 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 wherein to electromagnetic absorption.Along with the development of nanometer technology, although conventional absorbents to be greatly increased to electromagnetic absorbent properties as the low-dimensional nanometer of ferrite and magnetic metal material and to improve, but because its electromagnetic impedance match characteristic is relatively poor when finding to use single dielectric loss or magnetic loss absorbent, its absorbing property is generally still difficult to meet the requirement of development of modern scientific technology to " thin, light, wide, strong " that absorbing material performance proposes.So multiple absorbent is carried out compound to make the important directions that nanostructured composite wave-suction material becomes the development of current absorbing material field.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, reaching low-density, to absorb and wide band effect by force.
Ferroelectric/ferromagnetic Multiferroic composite material is a kind of advanced material with magnetoelectricity transformation function, its magnetoelectricity transformation function is realized by ferroelectric phase and ferromagnetic alternate product effect and magnetic couplings effect, stores, the technical field such as the current measurement of microwave sounding and ultra-high-tension power transmission line has broad application prospects in magnetoelectric transducer (magnetic field, electric field detecting etc.), conductor magneto-electric energy conversion, data.So far people have carried out a large amount of and deep research to its magnetoelectric effect, but the ferroelectric, ferromagnetic of this type of Multiferroic composite material coexists and its collaborative loss effect, also be the important foundation of strong absorption, broadband microwave absorbing material simultaneously, but from the retrieval of patent and document, the research of the domestic and international electromagnetic property to this type of material and absorbing property is also fewer at present, material shape also mainly concentrates on ferroelectric/ferromagnetic composite granule of zero dimension.Result of study display is ferroelectric reveals more excellent microwave absorbing property with the composite table of ferromagnetic material, and such as ferroelectric nano powder and ferromagnetic nano-powder are carried out physical mixed by A. Mandal etc., obtain Co 0.5zn 0.5fe 2o 4/ Pb (Zr 0.52ti 0.48) O 3(A. Mandal and C.K. Das, Electronic materials based on Co 0.5zn 0.5fe 2o 4/ Pb (Zr 0.52ti 0.48) O 3nanocomposites, Journal of Electronic Materials, 2013,42:121-128) and Co 0.2ni 0.4zn 0.4fe 2o 4/ BaTiO 3(A. Mandal and C.K. Das, Effect of BaTiO 3on 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 that the absorptivity of these ferroelectric/ferromagnetic composite nano-powders at X-band (8.2 ~ 12.4GHz) is all more than 90%, minimal reflection loss reaches Yue – 42 Zhi – 48dB.
So far for one-dimensional nano structure ferroelectric/ferromagnetic composite material such as the electromagnetic property of ferroelectric/ferromagnetic composite nano-fiber and the research of absorbing property also rarely has report.Compared with powder absorbent, absorbing material containing nanofiber absorbent not only has excellent mechanical property and physicochemical property, and utilize the shape anisotropy of fiber, its electromagnetic consumable at microwave frequency band and absorption efficiency can also be improved, become a kind of rising novel wave-absorbing material; Nanofiber is due to its one dimension architectural characteristic and confinement effect simultaneously, ferromagnetic and ferroelectric two-phase can be made to realize being uniformly distributed in microscopic dimensions, the particle aggregation of normal easily appearance in three-dimensional block, two-dimensional film and zero dimension powder and heterogeneous distribution problem can be solved, greatly improve the contact area of two-phase, strengthen two alternate efficient couplings and loss cooperative effect, be expected to strengthen microwave absorption intensity further and widen absorption band.Prepare the technology of oxide ceramics and compound micro nanometer fiber relative to other, method of electrostatic spinning has the advantages such as simple to operate, with low cost, efficient, realizes suitability for industrialized production at present in some field.Xie Shuhong etc. adopt the method for combination of sol-gel electrostatic spinning to prepare CoFe 2o 4-Pb (Zr x ti 1- x ) O 3and CoFe 2o 4-Pb (Zr x ti 1- x ) ferromagnetic ferroelectric composite nano-fiber material (S.H. Xie, J.Y. Li, Y.Y. Liu, L.N. Lan, Y.C. Zhou, Electrospinning and multiferroic properties of NiFe 2o 4-Pb (Zr 0.52ti 0.48) O 3composite 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 CoFe 2o 4-Pb (Zr 0.52ti 0.48) O 3nanofibers by electrospinning, Applied Physics Letters, 2008,92:062901; CN101274844A).The technical scheme adopted is for solvent with glycol methyl ether, glacial acetic acid, second alcohol and water, first make ferroelectric precursor solution, ferromagnetic precursor solution and polymer solution respectively, and then mix through stir make electrospinning precursor solution, ferroelectric-ferromagnetic composite nano-fiber is obtained with calcination processing finally by electrostatic spinning is shaping, wherein in configuration ferroelectric precursor solution processes, solution needs ageing 3 ~ 7 days, also adds citric acid as chelating agent when configuring ferromagnetic precursor solution.Can find out that whole preparation process still exists technique comparatively complicated, operate comparatively loaded down with trivial details, the shortcomings such as length consuming time, are unfavorable for large-scale production.
Therefore, develop that technique is simple, easy to operate, cost is low, be easy to the ferromagnetic ferroelectric composite nano fiber electrostatic spinning preparation technology of large-scale production, the research and apply for ferromagnetic/ferroelectric composite nano fiber has great importance.
Summary of the invention
Goal of the invention: for above-mentioned existing Problems existing and deficiency, a kind of chemical composition of the present invention be ( n) Ni 0.4co 0.2zn 0.4fe 2o 4/ (1 – n) BaTiO 3(0< n< 100mol%) and have excellent absorbing property ferromagnetic/ferroelectric ceramics composite nano fiber microwave absorption and preparation method thereof; solve the application in electro-magnetic wave absorption field of magnetoelectric ceramic composite nano fiber blank, and complex technical process, complex operation, cost that existing technology of preparing exists are higher, the not easily technical problem 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) Ni 0.4co 0.2zn 0.4fe 2o 4/ (1 – n) BaTiO 3, 0< n<100 mol% is by spinel structure ferromagnetism Ni 0.4co 0.2zn 0.4fe 2o 4with perovskite structure ferroelectricity BaTiO 3nanocrystallinely to form; Described Ni 0.4co 0.2zn 0.4fe 2o 4average grain size be 20 ~ 50nm, BaTiO 3average grain size be 20 ~ 60nm, two-phase crystal grain is along fiber axis to being uniformly distributed, and fibre diameter is about 100 ~ 300nm.
Another object of the present invention there is provided a kind of preparation method of above-mentioned composite nano fiber microwave absorption, comprise the following steps: slaine is first dissolved in solvent by concentration ratio according to the stoichiometric proportion of product by (1), and then add polyvinylpyrrolidone, continue stirring and directly obtain uniform composition, transparent, stable spinning solution in 2 ~ 8 hours; (2) step (1) gained spinning solution is made PVP/ slaine precursor fibre through high-voltage electrostatic spinning, and carry out drying process at 80 ~ 100 DEG C; (3) precursor fibre obtained for step (2) heat-treated in air atmosphere, finally high, the crystal formation of obtained degree of crystallinity grows perfect nanometer crystalline Ni 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3composite nano fiber.
Described slaine is nickel acetate, cobalt acetate, zinc acetate, barium acetate, ferric acetyl acetonade and butyl titanate; Described solvent is the mixed solvent of ethanol and acetic acid composition, and the mass ratio of ethanol and acetic acid is 0.25 ~ 4.
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.
In 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 evenly coated on matrix, forms the coating of 2 ~ 4mm.In 2 ~ 18GHz frequency range, all have strong absorption, effective Absorber Bandwidth of minimal reflection loss Da Dao – 46dB, reflection loss Di Yu – 10dB almost can cover whole S-band to Ku wave band.
Beneficial effect: compared with prior art, the present invention has the following advantages: 1. the present invention achieves the combination of ferromagnetic magnetic loss and ferroelectric dielectric loss by one-dimensional composite nano structure, utilize the architectural characteristic of monodimension nanometer material and confinement effect thereof to enhance loss cooperative effect in system between ferromagnetic phase and ferroelectric phase, obtain high-performance magnetism electricity composite nano fiber absorbing material.2. Ni of the present invention 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3composite nano fiber microwave absorption has strong absorption in 4 ~ 18GHz frequency range, its electromagnetic parameter and Microwave Absorption Properties can carry out Effective Regulation conveniently by change is ferromagnetic with the ratio of ferroelectric phase and the chemical composition of ferromagnetic phase within the specific limits, have broad application prospects in electromagnetism stealth, electromagnetic shielding and the field such as anti-electromagnetic interference and radiation pollution.3. the present invention adopts the method for solution electrostatic spinning to prepare Ni 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3composite nano fiber microwave absorption, directly institute's slaine and spin finish aid are dissolved in solvent, without the need to adding other chelating agents or still aging for a long time, its technical process is simple, easy to operate, manufacturing cycle is short, cost is low, utilizes large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is Ni prepared by the embodiment of the present invention 1 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3the electron scanning micrograph of composite nano fiber;
Fig. 2 is Ni prepared by the embodiment of the present invention 1 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3the X-ray diffraction spectrogram of composite nano fiber;
Fig. 3 is Ni prepared by the embodiment of the present invention 1 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3the microwave absorbing property curve of composite nano fiber microwave absorption within the scope of 2 ~ 18GHz.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, 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.
Embodiment 1:
According to ferromagnetic phase Ni 0.5zn 0.5fe 2o 4with ferroelectric phase BaTiO 3mol ratio be 6: 4, take 0.4062g butyl titanate respectively, 0.3048g barium acetate, 0.1782g nickel acetate, 0.0892g cobalt acetate, 0.1572g zinc acetate, 1.2645g ferric acetyl acetonade joins in the mixed solvent that 10.7800g acetic acid and 4.6200g ethanol forms (mass ratio of ethanol and acetic acid is about 0.43), after at room temperature magnetic agitation to all slaines dissolve completely, take 1.6000g polyvinylpyrrolidone (PVP again, mean molecule quantity is 1300000) join in above-mentioned solution, continue magnetic agitation and form homogeneous phase in about 2 hours, transparent, stable spinning precursor solution, wherein the mass percentage of PVP is 8%, the mass percentage of all slaines is 15%.The spinning solution prepared is moved in the electrostatic spinning apparatus (see Chinese patent 201110201848.7) be made up of DC high-voltage power supply, reservoir, spinning head, syringe pump and collector, be 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 the condition of relative humidity 30 ~ 45%.The precursor fibre collected is put into program control electric furnace more in an oven after 100 DEG C of abundant dryings, be heated to 1050 DEG C of roastings 3 hours with the speed of 1 DEG C/min by room temperature in air atmosphere, naturally cool to room temperature with stove afterwards and obtain chemical composition for (60mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (40mol%) BaTiO 3ferromagnetic/ferroelectric composite nano fiber microwave absorption.Obtained composite nano fiber microscopic appearance is good, and thickness is comparatively even, and average diameter is about 180nm (see figure 1), by spinel structure Ni 0.5zn 0.5fe 2o 4with perovskite structure BaTiO 3two phase compositions, without other dephasigns (as shown in Figure 2), ferromagnetic phase Ni 0.4co 0.2zn 0.4fe 2o 4average grain size be 50nm, ferroelectric phase BaTiO 3average grain size be 53nm.When absorbent loading is 70% (mass fraction), when coating layer thickness is 2.0mm, individual layer (60mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (40mol%) BaTiO 3the minimum reflectance of-silica gel microwave absorbing coating is at 14.2GHz place Da Dao – 46dB.
Embodiment 2:
Basic process is with embodiment 1, and difference is: Ni 0.4co 0.2zn 0.4fe 2o 4with BaTiO 3mol ratio 5:5, the quality of butyl titanate, barium acetate, nickel acetate, cobalt acetate, zinc acetate, ferric acetyl acetonade is respectively 0.5306g, 0.3983g, 0.1552g, 0.0777g, 0.1369g and 1.1013g, and the chemical composition of ferromagnetic/ferroelectric composite nano fiber microwave absorption obtained is (50mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (50mol%) BaTiO 3, its average diameter is about 270nm, ferromagnetic phase Ni 0.5zn 0.5fe 2o 4average grain size be about 56nm, ferroelectric phase BaTiO 3average grain size be about 60nm; When absorbent loading is 70% (mass fraction, lower same), when coating layer thickness is 3.0mm, individual layer (50mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (50mol%) BaTiO 3the minimum reflectance of-silica gel microwave absorbing coating is at 5.1GHz place Da Dao – 41dB.
Embodiment 3:
Basic process is with embodiment 1, and difference is: Ni 0.4co 0.2zn 0.4fe 2o 4with BaTiO 3mol ratio 9:1, the quality of butyl titanate, barium acetate, nickel acetate, cobalt acetate, zinc acetate, ferric acetyl acetonade is respectively 0.0891g, 0.0669g, 0.2366g, 0.1184g, 0.2087g and 1.6789g, and the chemical composition of ferromagnetic/ferroelectric composite nano fiber microwave absorption obtained is (90mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (10mol%) BaTiO 3, its average diameter is about 260nm, ferromagnetic phase Ni 0.5zn 0.5fe 2o 4average grain size be about 38nm, ferroelectric phase BaTiO 3average grain size be about 20nm; When absorbent loading is 70%, when coating layer thickness is 3.5mm, individual layer (90mol%) Ni 0.4co 0.2zn 0.4fe 2o 4/ (10mol%) BaTiO 3the minimum reflectance of-silica gel microwave absorbing coating is at 8.9GHz place Da Dao – 24dB.
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 is at 8.3GHz place Da Dao – 20.8dB.
In the present invention, spinel type ferrite is that a kind of performance is comparatively excellent and the microwave absorbing material that application is ripe, has low-dielectric, high resistivity and is easy 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 also can utilize the shape anisotropy of its uniqueness to overcome spinel type ferrite resonant frequency and the problem such as the Snoek limit is low, improve this type of material in the magnetic conductivity 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, spinel structure ferrite of the present invention/perovskite structure ferroelectric composite nano fiber microwave absorption has wider effective absorption frequency scope.For physical mixed type composite granule, the contact gear ratio of ferromagnetic and ferroelectric phase 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 closely, this not only can strengthen the magneto-electric coupled effect between ferromagnetic and ferroelectric phase, and what is more important can form good electromagnetic matching on a microscopic scale, enable more electromagnetic wave effectively enter into wave-absorber inside be attenuated and absorb, thus result in effective absorption band and obviously widen.

Claims (7)

1. a NCZFO-BTO sections magnet electroceramics composite nano fiber microwave absorption, is characterized in that: chemical composition for ( n) Ni 0.4co 0.2zn 0.4fe 2o 4/ (1 – n) BaTiO 3, 0< n<100 mol% is by spinel structure ferromagnetism Ni 0.4co 0.2zn 0.4fe 2o 4with perovskite structure ferroelectricity BaTiO 3nanocrystallinely to form; Described Ni 0.4co 0.2zn 0.4fe 2o 4average grain size be 20 ~ 50nm, BaTiO 3average grain size be 20 ~ 60nm, two-phase crystal grain is along fiber axis to being uniformly distributed, and fibre diameter is about 100 ~ 300nm.
2. a preparation method for composite nano fiber microwave absorption described in claim 1, comprises the following steps:
(1) according to the stoichiometric proportion of product, slaine is first dissolved in solvent by concentration ratio, and then adds polyvinylpyrrolidone, continue stirring and directly obtain uniform composition, transparent, stable spinning solution in 2 ~ 8 hours;
(2) step (1) gained spinning solution is made PVP/ slaine precursor fibre through high-voltage electrostatic spinning, and carry out drying process at 80 ~ 100 DEG C;
(3) precursor fibre obtained for step (2) heat-treated in air atmosphere, finally high, the crystal formation of obtained degree of crystallinity grows perfect nanometer crystalline Ni 0.4co 0.2zn 0.4fe 2o 4/ BaTiO 3composite nano fiber.
3. the preparation method of composite nano fiber microwave absorption according to claim 2, is characterized in that: described slaine is nickel acetate, cobalt acetate, zinc acetate, barium acetate, ferric acetyl acetonade and butyl titanate; Described solvent is the mixed solvent of ethanol and acetic acid composition, and the mass ratio of ethanol and acetic acid is 0.25 ~ 4.
4. the preparation method of composite nano fiber microwave absorption according to claim 2, it is characterized in that: in spinning solution, the mass fraction of polyvinylpyrrolidone is 7 ~ 12%, the mass fraction of slaine is 10% ~ 18%.
5. the preparation method of composite nano fiber microwave absorption according to claim 2, it is characterized in that: in step (2), electrostatic spinning electric-field intensity is 0.6 ~ 1.5kV/cm, solution advances speed 0.2 ~ 0.8mL/h, and temperature is 15 ~ 30 DEG C, relative humidity less than 50%.
6. the preparation method of composite nano fiber microwave absorption according to claim 2, it is characterized in that: the heat treatment temperature described in step (3) is 800 ~ 1200 DEG C, heating rate is 0.5 ~ 5 DEG C/min, and temperature retention time is 1 ~ 8 hour.
7. application rights requires a microwave absorbing coating for composite nano fiber microwave absorption described in 1, it is characterized in that: described composite nano fiber wave absorbent is evenly coated on matrix, forms the coating of 2 ~ 4mm.
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