CN105862145A - Shell-layer-core-layer structure nano composite wave absorbing material and preparation method thereof - Google Patents

Shell-layer-core-layer structure nano composite wave absorbing material and preparation method thereof Download PDF

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CN105862145A
CN105862145A CN201610244974.3A CN201610244974A CN105862145A CN 105862145 A CN105862145 A CN 105862145A CN 201610244974 A CN201610244974 A CN 201610244974A CN 105862145 A CN105862145 A CN 105862145A
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shell
layer
nitrate
fiber
composite
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CN105862145B (en
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王志华
赵琳
余建华
王普红
郭磊
丁志军
杜斌
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PLA 63975 ARMY
Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning

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  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The invention relates to a shell-layer-core-layer structure nano composite wave absorbing material and a preparation method thereof. A chemical formula of the wave absorbing material is expressed as MFe12O19/BaTiO3. The preparation method includes: using M nitrate, iron nitrate, polyvinyl pyrrolidone and N, N-dimethyl formamide proportionally to prepare shell-layer spinning liquid; using barium acetate and butyl titanate as raw materials, and using polyvinyl pyrrolidone, alcohol, glacial acetic acid and water proportionally to prepare core-layer spinning liquid; subjecting the shell-layer spinning liquid and the core-layer spinning liquid to coaxial electrostatic spinning to obtain a composite precursor fiber; calcining the composite precursor fiber at 600-800 DEG C to obtain a shell-layer-core-layer structure MFe12O19/BaTiO3 nano composite fiber. Minimum reflection loss of the material within a frequency range of 2-18 GHz reaches -23.64 dB, and effective frequency bandwidth is 1.36 GHz. The preparation method is simple in process, uniform and stable in substance and high in process controllability.

Description

A kind of nano combined absorbing material of shell-core structure and preparation method thereof
Technical field
The invention belongs to chemical fibre absorbing material field, be specifically related to shell-core structure nano-composite fiber and inhale ripple Material and preparation method thereof.
Background technology
Strontium ferrite (SrFe12O19) be a kind of ferromagnetic material, have high coercivity, bigger saturation magnetization and The advantages such as excellent chemical stability, are widely used in the fields such as magnetic recording device, microwave absorbing material.
Barium metatitanate. (BaTiO3) it is a kind of ferroelectric material, there is high dielectric constant, excellent ferroelectricity and piezoelectric property, tool Having the features such as chemical stability is good, with low cost, barium-titanate material can be applicable to eliminate electromagnetic pollution harm, prevent electromagnetic interference And the aspect such as electromagnetic information exposure, but there is the shortcomings such as absorption band is narrow, absorption intensity is low in them.
At present, single material is difficult to meet the demand of multi-form, and Development of Nanometer Material tends to diversification, for inhaling ripple Material, by ferrite wave absorbing agent (strontium ferrite, Ni ferrite etc.) and media ceramic class wave absorbing agent (Barium metatitanate., carborundum, nitridation Silicon etc.) combine, the relative permeability of composite can be made to approximate relative dielectric constant, the absorbing property of material can be improved. The method that common used material is combined has a lot, mainly includes coaxial electrostatic spinning method, in-situ compositing, blending method etc..Wherein, coaxially Electrostatic spinning technique can prepare shell-caryogram fiber, have range of choice width, combined efficiency is high, device is easy, with low cost, Process controllability high, becomes one of main path preparing nanometer composite fiber material gradually.
Nickel-copper-zinc ferrite and secret system perovskite-like ferroelectric ceramics are mixed by patent CN104987056 by ball grinding method, Obtain ferrum-Ferroelectric Composites, but in mechanical milling process, metal oxide particle is easily generated autohemagglutination phenomenon, and process is lengthy and jumbled.
It is multiple that patent CN102093045 uses uniformly co-precipitation out-phase cladding process to prepare nucleocapsid structure Barium metatitanate .-Barium hexaferrite Close powder body material, but owing to the precipitation number of each metal is different, reaction condition requires harshness.
Document Avinash B, Yiu W M, Rattikorn Y, Sujitra U.RSC Adv, 2014,4:55217- In 55223, prepare BaTiO by blending method3、CoFe2O4Composite precursor spinning liquid, by electrospinning process by BaTiO3、 CoFe2O4Compound, and detect its magnetic electricity performance.But find through characterizing, combination product exists uncertain material, product pure Spend bigger to final performance impact.
At present, coaxial electrostatic spinning is used to prepare shell-core structure ferrite/barium titanate nano complex fiber material also The research being applied to microwave suction ripple field has no report.
Summary of the invention
It is an object of the invention to provide a kind of shell-core structure nano-composite fiber absorbing material and preparation method thereof, This materials application inhales ripple field in microwave.
The technical scheme is that, utilize coaxial electrostatic spinning technology to prepare MFe12O19/BaTiO3Composite precursor Fiber, through high-temperature calcination, obtains the composite nano fiber with shell-core structure.Product stable homogeneous prepared by this method, Process controllability is high, does not has uncertain material.
Shell-core structure nano-composite fiber absorbing material that the present invention provides, is represented by MFe12O19/BaTiO3, Wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one；This nanometer composite fiber material is shell-core structure, The a diameter of 160-180nm of its outer layer, a diameter of 40-80nm of internal layer, fiber thickness is uniform, smooth surface.
The preparation method of above-mentioned shell-core structure nano-composite fiber absorbing material, specifically comprises the following steps that
A., under room temperature, mixed nitrate, polyvinylpyrrolidone and DMF are mixed in proportion preparation Shell solution, wherein nitrate, polyvinylpyrrolidone, DMF mass ratio are 1:(1-3): (10-15)；
Described mixed nitrate is bivalence nitrate M (NO3)2, the mixture of ferric nitrate, wherein M2+With Fe3+Mol ratio For 1:12, wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one；
B. polyvinylpyrrolidone, ethanol, Barium acetate, butyl titanate, glacial acetic acid and water are mixed in proportion preparation core Layer solution, wherein polyvinylpyrrolidone, ethanol, Barium acetate, butyl titanate, glacial acetic acid, the mass ratio of water are 1:(8-12): (2-5): (2-5): (5-8): (1-3)；And Barium acetate is 1:1 with the mol ratio of butyl titanate；
Polyvinylpyrrolidone used in described shell solution and sandwich layer solution is organic polymer spinning-aid agent, its molecule Amount is 100000-130000；
C. above-mentioned shell solution being placed in coaxial electrostatic spinning outer tube, sandwich layer solution is placed in coaxial electrostatic spinning inner tube, point Not as coaxial electrostatic spinning outer layer and internal layer；Outer tube uses No. 16 syringe needles, No. 8 syringe needles of inner tube, carries out electrostatic spinning, its technique Parameter is: voltage 10-20kV, ectonexine fltting speed 0.3-2mL/h, receiving range 10-20cm, rotating speed 200-500rpm, spins Silk temperature 25-40 DEG C；Obtain composite precursor fiber；
D. composite precursor fiber step C obtained is in 50-100 DEG C of drying；Then with the heating rate of 1-5 DEG C/min Rise to 600-800 DEG C of calcining 1-5h, with the 1-5 DEG C/min near room temperature of rate of temperature fall, obtain MFe12O19/BaTiO3Nano combined fibre Dimension.
The ultimate principle of the present invention is: will be containing M2+And Fe3+Solution and solution containing Ba, Ti, utilize coaxial electrostatic Spining technology, obtains MFe12O19/BaTiO3Composite precursor fiber, then through high-temperature heat treatment, obtain that there is shell-core structure MFe12O19/BaTiO3Composite nano fiber.
The present invention has such advantages as relative to prior art and effect:
Spinning is used to send out preparation MFe first12O19/BaTiO3Nano-composite fiber, the method is simple to operate, material is homogeneous Stable, process controllability height.
2. the MFe of preparation12O19/BaTiO3Nano-composite fiber and single SrFe12O19、BaTiO3The absorbing property of material Comparing, composite material exhibits has gone out the advantage of " thickness is thin, bandwidth, absorption strong ", and its absorbing property is much better than single SrFe12O19、BaTiO3Material.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) photo of embodiment 1 composite fibre sample；
Fig. 2 is scanning electron microscope (SEM) photo of embodiment 1 composite precursor fiber sample；
Fig. 3 is transmission electron microscope (TEM) photo of embodiment 1 composite fibre sample；
Fig. 4 is scanning electron microscope (SEM) photo of embodiment 2 composite precursor fiber sample；
Fig. 5 is transmission electron microscope (TEM) photo of embodiment 3 composite fibre sample；
Fig. 6 is the composite fibre in comparative example and single SrFe12O19Nanofiber reflection loss comparison diagram.
Specific embodiments
Embodiment 1
A. 0.021g strontium nitrate, 0.484g ferric nitrate, 0.75g polyvinylpyrrolidone and 5mL N, N-dimethyl methyl are weighed Amide mixes, and is stirred at room temperature uniformly to being completely dissolved, obtains the shell solution of stable homogeneous；
B. 0.35g PVP, 3.5mL ethanol, 0.75g barium acetate, 1mL butyl titanate, 2mL glacial acetic acid and 1mL water are weighed, It is stirred at room temperature uniformly to being completely dissolved, i.e. obtains the sandwich layer solution of stable homogeneous.
C. 5mL shell solution and 5mL sandwich layer solution are respectively placed in coaxial electrostatic spinning outer tube and inner tube, as coaxially Electrostatic spinning outer layer and internal layer spinning liquid, use 16 extra needle head, needle head in No. 8, carry out coaxial electrostatic spinning, voltage 10kV, ectonexine fltting speed 0.3mL/h, receiving range 15cm, rotating speed 1000rpm, spinning temperature 30 DEG C, obtain compound precursor Body fiber；
D. 100 DEG C of dry 24h in drying baker put into by composite precursor fiber step C obtained, and after drying, put into Muffle In stove, 1 DEG C/min of heating rate, 750 DEG C of constant temperature 1h, 1 DEG C/min of rate of temperature fall, it is cooled to 200 DEG C of room temperature coolings, To SrFe12O19/BaTiO3Nano-composite fiber.
Product is accredited as SrFe through X-ray diffraction (Fig. 1)12O19With BaTiO3Composite, by SEM scanning electron microscope (SEM) photograph (Fig. 2) observing composite precursor fibre diameter is 100nm, by TEM transmission electron microscope picture (Fig. 3) observe product be shell- Core structure, a diameter of 160-180nm of its outer layer, a diameter of 40-80nm of internal layer.
Embodiment 2
A. 0.021g strontium nitrate, 0.484g ferric nitrate, 1.5g polyvinylpyrrolidone and 7.5mL N, N-dimethyl are weighed Methanamide mixes, and is stirred at room temperature uniformly to being completely dissolved, obtains the shell solution of stable homogeneous；
B. weigh 0.35g PVP, 3.5mL ethanol, 1.0g barium acetate, 1.3mL butyl titanate, 2.8mL glacial acetic acid with 1.3mL water, is stirred at room temperature uniformly to being completely dissolved, i.e. obtains the sandwich layer solution of stable homogeneous.
C. 5mL shell solution and 5mL sandwich layer solution are placed in coaxial electrostatic spinning inner tube, respectively as coaxial electrostatic spinning Silk outer layer and internal layer, uses 16 extra needle head, needle head in No. 8, carries out coaxial electrostatic spinning, voltage 18kV, and ectonexine pushes away Enter speed 1mL/h, receiving range 10cm, rotating speed 1000rpm, spinning temperature 30 DEG C, obtain composite precursor fiber；
D. 100 DEG C of dry 24h in drying baker put into by composite precursor fiber step C obtained, and after drying, put into Muffle In stove, 5 DEG C/min of heating rate, 800 DEG C of constant temperature 1h, 5 DEG C/min of rate of temperature fall, it is cooled to 200 DEG C of room temperature coolings, the most available SrFe12O19/BaTiO3Nano-composite fiber.
It is 200nm that product observes composite precursor fibre diameter by SEM scanning electron microscope (SEM) photograph (Fig. 4).
Embodiment 3
A. 0.021g strontium nitrate, 0.484g ferric nitrate, 0.75g polyvinylpyrrolidone and 5mL N, N-dimethyl methyl are weighed Amide mixes, and is stirred at room temperature uniformly to being completely dissolved, obtains the shell solution of stable homogeneous；
B. 0.35g PVP, 3.5mL ethanol, 0.75g barium acetate, 1mL butyl titanate, 2mL glacial acetic acid and 1mL water are weighed, It is stirred at room temperature uniformly to being completely dissolved, i.e. obtains the sandwich layer solution of stable homogeneous.
C. 5mL shell solution and 5mL sandwich layer solution are placed in coaxial electrostatic spinning inner tube, respectively as coaxial electrostatic spinning Silk outer layer and internal layer, uses 16 extra needle head, needle head in No. 8, carries out coaxial electrostatic spinning, voltage 20kV, and ectonexine pushes away Enter speed 2mL/h, receiving range 20cm, rotating speed 1000rpm, spinning temperature 30 DEG C, obtain composite precursor fiber；
D. 100 DEG C of dry 24h in drying baker put into by composite precursor fiber step C obtained, and after drying, put into Muffle In stove, 1 DEG C/min of heating rate, 650 DEG C of constant temperature 1h, 1 DEG C/min of rate of temperature fall, it is cooled to 200 DEG C of room temperature coolings, the most available SrFe12O19/BaTiO3Nano-composite fiber.
Product goes out product shell-core structure by observable in TEM transmission electron microscope picture (Fig. 5), and its outer layer is a diameter of 180-200nm, a diameter of 50-90nm of internal layer.
Comparative example
By the SrFe of preparation in embodiment 112O19/BaTiO3Nano-composite fiber is surveyed by the netted analyser of vector Examination, prepares single SrFe by electrostatic spinning simultaneously12O19Nanofiber carries out reflection loss contrast.Both is with paraffin as base Body material, mixes sample according to the mass ratio of 3: 2 with paraffin, use coaxial rings method prepare sample, the frequency range of measurement be 2～ 18GHz.Composite fibre and single SrFe12O19Nanofiber reflection loss contrasts, and result is shown in Fig. 6.
Table 1 lists SrFe12O19/BaTiO3Nano-composite fiber, SrFe12O19Nanofiber and BaTiO3The suction of material Ripple performance indications, from table 1, SrFe12O19/BaTiO3The absorbing property of nano-composite fiber is much better than single SrFe12O19、 BaTiO3Material, is that a kind of thickness is thin, high-performance wave-absorbing material that bandwidth, absorption are strong.
Table 1
Sample Matching thickness Effective frequency belt width Minimal reflection is lost
SrFe12O19/BaTiO3Nano-composite fiber 2.2mm 1.36GHz -23.64dB
SrFe12O19Nanofiber 3.6mm 0.88GHz -11.69dB
*BaTiO3Material 2mm 0 Without effectively absorbing
*, BaTiO is described3The data of material are from document Qing Y C, Zhou W C, Luo F, Zhu D M.J.Magn.Magn.Mater., in 2011,323:600-606.

Claims (2)

1. shell-core structure nano-composite fiber absorbing material, its chemical formula is MFe12O19/BaTiO3, wherein M2+Generation Table bivalent metal ion Sr2+、Ba2+、Pb2+In one；This nanometer composite fiber material is shell-core structure, and its outer layer is straight Footpath is 160-180nm, a diameter of 40-80nm of internal layer, and fiber thickness is uniform, smooth surface.
2. the method preparing the shell described in claim 1-core structure nano-composite fiber absorbing material, concrete steps As follows:
A., under room temperature, mixed nitrate, polyvinylpyrrolidone and DMF are mixed in proportion preparation shell Solution, wherein nitrate, polyvinylpyrrolidone, DMF mass ratio are 1:1-3:10-15；
Described mixed nitrate is bivalence nitrate M (NO3)2, the mixture of ferric nitrate, wherein M2+With Fe3+Mol ratio be 1: 12, wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one；
B. polyvinylpyrrolidone, ethanol, Barium acetate, butyl titanate, glacial acetic acid and water are mixed in proportion preparation sandwich layer molten Liquid, wherein polyvinylpyrrolidone, ethanol, Barium acetate, butyl titanate, glacial acetic acid, the mass ratio of water are 1:8-12:2-5:2- 5:5-8:1-3；And Barium acetate is 1:1 with the mol ratio of butyl titanate；
The molecular weight of the polyvinylpyrrolidone described in step A and step B is 100000-130000；
C. above-mentioned shell solution being placed in coaxial electrostatic spinning outer tube, sandwich layer solution is placed in coaxial electrostatic spinning inner tube, makees respectively For coaxial electrostatic spinning outer layer and internal layer；Outer tube uses No. 16 syringe needles, No. 8 syringe needles of inner tube, carries out electrostatic spinning, its technological parameter For: voltage 10-20kV, ectonexine fltting speed 0.3-2mL/h, receiving range 10-20cm, rotating speed 200-500rpm, spinning temperature Spend 25-40 DEG C；Obtain composite precursor fiber；
D. composite precursor fiber step C obtained is in 50-100 DEG C of drying；Then rise to the heating rate of 1-5 DEG C/min 600-800 DEG C of roasting 1-5h, with the 1-5 DEG C/min near room temperature of rate of temperature fall, obtains MFe12O19/BaTiO3Nano-composite fiber.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN106492779A (en) * 2016-09-29 2017-03-15 李跃军 The preparation method of core shell structure rare earth titanate dioxide composite nanofiber catalysis material
CN109913978A (en) * 2019-03-06 2019-06-21 武汉理工大学 A kind of nucleocapsid structure composite fibre and preparation method thereof and the application in polymer matrix flexible composite film
CN110863299A (en) * 2019-09-04 2020-03-06 西安工程大学 Piezoelectric BaTiO3/Fe3O4Preparation and application of/PAN electrostatic spinning wave absorption membrane
CN111321520A (en) * 2020-03-11 2020-06-23 天津理工大学 Method for coaxially and electrostatically spinning piezoelectric property of polyvinylidene fluoride/polyacrylonitrile reinforced fiber film
CN111850821A (en) * 2020-06-13 2020-10-30 北京化工大学 Method for preparing electromagnetic wave absorbing material from hydrotalcite-based composite nanofiber
CN113652769A (en) * 2021-08-30 2021-11-16 中国工程物理研究院激光聚变研究中心 Core-shell type Fe3Preparation of C/C fiber composite wave absorbing agent and application thereof in microwave absorption
CN114481364A (en) * 2021-12-31 2022-05-13 江苏大学 Janus type electromagnetic coupling microwave absorbent and preparation method thereof

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CN101624283A (en) * 2008-07-07 2010-01-13 电子科技大学 Method for preparing BaFe12O and BaTiO3 multiplayer nano compound film/powder
CN103215690A (en) * 2013-05-09 2013-07-24 兰州理工大学 Preparation method and preparation device of nano fibers
CN104774346A (en) * 2015-04-30 2015-07-15 武汉艾特米克超能新材料科技有限公司 Light porous wave absorbing film and preparing method thereof

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JP2009052171A (en) * 2007-08-27 2009-03-12 Unitika Ltd Method for producing fine fiber aggregate and apparatus therefor
CN101624283A (en) * 2008-07-07 2010-01-13 电子科技大学 Method for preparing BaFe12O and BaTiO3 multiplayer nano compound film/powder
CN103215690A (en) * 2013-05-09 2013-07-24 兰州理工大学 Preparation method and preparation device of nano fibers
CN104774346A (en) * 2015-04-30 2015-07-15 武汉艾特米克超能新材料科技有限公司 Light porous wave absorbing film and preparing method thereof

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106492779A (en) * 2016-09-29 2017-03-15 李跃军 The preparation method of core shell structure rare earth titanate dioxide composite nanofiber catalysis material
CN109913978A (en) * 2019-03-06 2019-06-21 武汉理工大学 A kind of nucleocapsid structure composite fibre and preparation method thereof and the application in polymer matrix flexible composite film
CN110863299A (en) * 2019-09-04 2020-03-06 西安工程大学 Piezoelectric BaTiO3/Fe3O4Preparation and application of/PAN electrostatic spinning wave absorption membrane
CN111321520A (en) * 2020-03-11 2020-06-23 天津理工大学 Method for coaxially and electrostatically spinning piezoelectric property of polyvinylidene fluoride/polyacrylonitrile reinforced fiber film
CN111850821A (en) * 2020-06-13 2020-10-30 北京化工大学 Method for preparing electromagnetic wave absorbing material from hydrotalcite-based composite nanofiber
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
CN113652769A (en) * 2021-08-30 2021-11-16 中国工程物理研究院激光聚变研究中心 Core-shell type Fe3Preparation of C/C fiber composite wave absorbing agent and application thereof in microwave absorption
CN113652769B (en) * 2021-08-30 2023-08-22 中国工程物理研究院激光聚变研究中心 Core-shell Fe 3 Preparation of C/C fiber composite wave absorber and application thereof in microwave absorption
CN114481364A (en) * 2021-12-31 2022-05-13 江苏大学 Janus type electromagnetic coupling microwave absorbent and preparation method thereof

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