CN105862145B - A kind of nano combined absorbing material of shell core structure and preparation method thereof - Google Patents

A kind of nano combined absorbing material of shell core structure and preparation method thereof Download PDF

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CN105862145B
CN105862145B CN201610244974.3A CN201610244974A CN105862145B CN 105862145 B CN105862145 B CN 105862145B CN 201610244974 A CN201610244974 A CN 201610244974A CN 105862145 B CN105862145 B CN 105862145B
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shell
polyvinylpyrrolidone
fiber
core structure
nitrate
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CN105862145A (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)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

The present invention relates to a kind of shell core structure nano-composite fiber absorbing material and preparation method thereof, the chemical formula of the absorbing material is expressed as MFe12O19/BaTiO3.The preparation method of the absorbing material is：Shell layer spinning solution is made into proportion with M nitrate and ferric nitrate, polyvinylpyrrolidone and N, N dimethylformamide；It is raw material with barium acetate, butyl titanate, polyvinylpyrrolidone, ethanol, glacial acetic acid and water are made into sandwich layer spinning solution in proportion.Shell layer spinning solution and sandwich layer spinning solution are subjected to coaxial electrostatic spinning, obtain composite precursor fiber；Through 600 800 DEG C of roastings, shell core structure MFe is obtained12O19/BaTiO3Nano-composite fiber.Material minimal reflection loss in 2~18GHz frequency range reaches 23.64dB, effective frequency belt width 1.36GHz.This preparation method technique is simple, material stable homogeneous, process controllability are high.

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, and in particular to shell-core structure nano-composite fiber inhales ripple Material and preparation method thereof.
Background technology
Strontium ferrite (SrFe12O19) be a kind of ferromagnetic material, have high coercivity, larger saturation magnetization and The advantages that excellent chemical stability, it is widely used in the fields such as magnetic recording device, microwave absorbing material.
Barium titanate (BaTiO3) it is a kind of ferroelectric material, there is high dielectric constant, excellent ferroelectricity and piezoelectric property, have There is the features such as chemical stability is good, cost is cheap, barium-titanate material can be applied to eliminate electromagnetic pollution harm, prevent electromagnetic interference And electromagnetic information exposure etc., but they the are present shortcoming such as absorption band is narrow, absorption intensity is low.
At present, single material is difficult to meet various forms of demands, 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 titanate, carborundum, nitridation Silicon etc.) it is combined, the relative permeability of composite can be made to be approximately equal to relative dielectric constant, the absorbing property of material can be improved. The compound method of common used material has a lot, mainly includes coaxial electrostatic spinning method, in-situ compositing, blending method etc..Wherein, coaxially Shell-caryogram fiber can be made in electrostatic spinning technique, have range of choice is wide, combined efficiency is high, device is easy, cost is cheap, The features such as process controllability is high, turns into gradually and prepare one of main path of nanometer composite fiber material.
Patent CN104987056 mixes nickel-copper-zinc ferrite and secret system's perovskite-like ferroelectric ceramics by ball grinding method, Iron-Ferroelectric Composites are obtained, but metal oxide particle is also easy to produce autohemagglutination phenomenon in mechanical milling process, and process is lengthy and jumbled.
It is multiple that patent CN102093045 uses uniform co-precipitation out-phase cladding process to prepare core shell structure barium titanate-barium ferrite Powder body material is closed, but because the precipitation number of each metal is different, reaction condition requires harsh.
Document Avinash B, Yiu W M, Rattikorn Y, Sujitra U.RSC Adv, 2014,4:55217- In 55223, BaTiO is prepared by blending method3、CoFe2O4Composite precursor spinning solution, by electrospinning process by BaTiO3、 CoFe2O4It is compound, and detect its magnetic electricity performance.But find uncertain material in combination product be present by characterizing, product it is pure Degree is larger to final performance impact.
At present, shell-core structure ferrite/barium titanate nano complex fiber material is prepared simultaneously using coaxial electrostatic spinning The research that ripple field is inhaled applied to microwave has no report.
The content 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, The materials application inhales ripple field in microwave.
The technical scheme is that prepare MFe using coaxial electrostatic spinning technology12O19/BaTiO3Composite precursor Fiber, through high-temperature calcination, obtain the composite nano fiber with shell-core structure.Product stable homogeneous prepared by this method, Process controllability is high, and not uncertain material is present.
Shell provided by the invention-core structure nano-composite fiber absorbing material, is represented by MFe12O19/BaTiO3, Wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one kind；The 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, and surface is smooth.
The preparation method of above-mentioned shell-core structure nano-composite fiber absorbing material, is comprised the following steps that：
A. at room temperature, by mixed nitrate, polyvinylpyrrolidone and DMF mixed preparing in proportion Shell solution, wherein nitrate, polyvinylpyrrolidone, DMF mass ratio are 1：(1-3)：(10-15)；
The mixed nitrate is divalence nitrate M (NO3)2, ferric nitrate mixture, wherein M2+With Fe3+Mol ratio For 1:12, wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one kind；
B. by polyvinylpyrrolidone, ethanol, barium acetate, butyl titanate, glacial acetic acid and water mixed preparing core in proportion 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 the mol ratio of barium acetate and butyl titanate is 1:1；
Polyvinylpyrrolidone used is organic polymer spinning-aid agent in the shell solution and sandwich layer solution, its molecule Measure as 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 Zuo Wei not coaxial electrostatic spinning outer layer and internal layer；Outer tube carries out electrostatic spinning, its technique using No. 8 No. 16 syringe needles, inner tube syringe needles Parameter is：Voltage 10-20kV, ectonexine fltting speed 0.3-2mL/h, distance 10-20cm, rotating speed 200-500rpm are received, spun 25-40 DEG C of temperature of silk；Obtain composite precursor fiber；
D. by the composite precursor fiber that step C is obtained in 50-100 DEG C of drying；Then with 1-5 DEG C/min heating rate 600-800 DEG C of calcining 1-5h is risen to, with the near room temperature of 1-5 DEG C/min rate of temperature fall, obtains MFe12O19/BaTiO3Nano combined fibre Dimension.
The present invention general principle be：M will be contained2+And Fe3+Solution and the solution containing Ba, Ti, utilize coaxial electrostatic Spining technology, obtain MFe12O19/BaTiO3Composite precursor fiber, then through high-temperature heat treatment, obtain with shell-core structure MFe12O19/BaTiO3Composite nano fiber.
The present invention is had the following advantages relative to prior art and effect：
1. MFe is prepared using spinning hair first12O19/BaTiO3Nano-composite fiber, this method is simple to operate, material is homogeneous Stable, process controllability height.
2. the MFe prepared12O19/BaTiO3Nano-composite fiber and single SrFe12O19、BaTiO3The absorbing property of material Compared, composite material exhibits have gone out the advantage of " thickness of thin, bandwidth, absorption are strong ", and its absorbing property is much better than single SrFe12O19、BaTiO3Material.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) photo of the composite fibre sample of embodiment 1；
Fig. 2 is ESEM (SEM) photo of the composite precursor fiber sample of embodiment 1；
Fig. 3 is transmission electron microscope (TEM) photo of the composite fibre sample of embodiment 1；
Fig. 4 is ESEM (SEM) photo of the composite precursor fiber sample of embodiment 2；
Fig. 5 is transmission electron microscope (TEM) photo of the composite fibre sample of embodiment 3；
Fig. 6 is composite fibre and single SrFe in comparative example12O19Nanofiber reflection loss comparison diagram.
Specific embodiment
Embodiment 1
A. 0.021g strontium nitrates, 0.484g ferric nitrates, 0.75g polyvinylpyrrolidones and 5mL N, N- dimethyl methyls are weighed Acid amides 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 acetates, 1mL butyl titanates, 2mL glacial acetic acid and 1mL water are weighed, It is stirred at room temperature uniformly to being completely dissolved, that is, obtains the sandwich layer solution of stable homogeneous.
C. 5mL shells solution and 5mL sandwich layer solution are respectively placed in coaxial electrostatic spinning outer tube and inner tube, as coaxial Electrostatic spinning outer layer and internal layer spinning solution, using needle head in 16 extra needle heads, No. 8, carry out coaxial electrostatic spinning, voltage 10kV, ectonexine fltting speed 0.3mL/h, distance 15cm is received, rotating speed 1000rpm, 30 DEG C of spinning temperature, obtains compound precursor Body fiber；
D. the composite precursor fiber that step C is obtained is put into 100 DEG C of dry 24h in drying box, after drying, is put into Muffle In stove, heating rate 1 DEG C/min, 750 DEG C of constant temperature 1h, 1 DEG C/min of rate of temperature fall, 200 DEG C of normal temperature coolings are cooled to, you can To SrFe12O19/BaTiO3Nano-composite fiber.
Product is accredited as SrFe through X-ray diffraction (Fig. 1)12O19With BaTiO3Composite, pass through SEM scanning electron microscope (SEM) photographs It is 100nm that (Fig. 2), which observes composite precursor fibre diameter, by TEM transmission electron microscope pictures (Fig. 3) observe product for 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 nitrates, 0.484g ferric nitrates, 1.5g polyvinylpyrrolidones and 7.5mL N, N- dimethyl are weighed Formamide 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 acetates, 1.3mL butyl titanates, 2.8mL glacial acetic acid with 1.3mL water, it is stirred at room temperature uniformly to being completely dissolved, that is, obtains the sandwich layer solution of stable homogeneous.
C. 5mL shells 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, using needle head in 16 extra needle heads, No. 8, coaxial electrostatic spinning, voltage 18kV are carried out, ectonexine pushes away Enter speed 1mL/h, receive distance 10cm, rotating speed 1000rpm, 30 DEG C of spinning temperature, obtain composite precursor fiber；
D. the composite precursor fiber that step C is obtained is put into 100 DEG C of dry 24h in drying box, after drying, is put into Muffle In stove, heating rate 5 DEG C/min, 800 DEG C of constant temperature 1h, 5 DEG C/min of rate of temperature fall, 200 DEG C of normal temperature coolings are cooled to, you can obtain SrFe12O19/BaTiO3Nano-composite fiber.
It is 200nm that product observes composite precursor fibre diameter by SEM scanning electron microscope (SEM) photographs (Fig. 4).
Embodiment 3
A. 0.021g strontium nitrates, 0.484g ferric nitrates, 0.75g polyvinylpyrrolidones and 5mL N, N- dimethyl methyls are weighed Acid amides 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 acetates, 1mL butyl titanates, 2mL glacial acetic acid and 1mL water are weighed, It is stirred at room temperature uniformly to being completely dissolved, that is, obtains the sandwich layer solution of stable homogeneous.
C. 5mL shells 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, using needle head in 16 extra needle heads, No. 8, coaxial electrostatic spinning, voltage 20kV are carried out, ectonexine pushes away Enter speed 2mL/h, receive distance 20cm, rotating speed 1000rpm, 30 DEG C of spinning temperature, obtain composite precursor fiber；
D. the composite precursor fiber that step C is obtained is put into 100 DEG C of dry 24h in drying box, after drying, is put into Muffle In stove, heating rate 1 DEG C/min, 650 DEG C of constant temperature 1h, 1 DEG C/min of rate of temperature fall, 200 DEG C of normal temperature coolings are cooled to, you can obtain SrFe12O19/BaTiO3Nano-composite fiber.
Product goes out product shell-core structure by observable in TEM transmission electron microscope pictures (Fig. 5), and its outer layer is a diameter of 180-200nm, a diameter of 50-90nm of internal layer.
Comparative example
The SrFe that will be prepared in embodiment 112O19/BaTiO3Nano-composite fiber is surveyed by the netted analyzer of vector Examination, while single SrFe is prepared by electrostatic spinning12O19Nanofiber carries out reflection loss contrast.The two is using paraffin as base Body material, sample is mixed with paraffin according to 3: 2 mass ratio, sample is prepared using coaxial rings method, the frequency range of measurement for 2~ 18GHz.Composite fibre and single SrFe12O19Nanofiber reflection loss contrasts, and as a result sees 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, it is a kind of thickness of thin, bandwidth, absorbs strong high-performance wave-absorbing material.
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 absorption
* BaTiO is illustrated3The data of material come from document Qing Y C, Zhou W C, Luo F, Zhu D M.J.Magn.Magn.Mater.,2011,323:In 600-606.

Claims (1)

1. a kind of method of shell-core structure nano-composite fiber absorbing material, is comprised the following steps that：
A. at room temperature, by mixed nitrate, polyvinylpyrrolidone and DMF mixed preparing shell in proportion Solution, wherein nitrate, polyvinylpyrrolidone, DMF mass ratio are 1：1-3：10-15；
The mixed nitrate is divalence nitrate M (NO3)2, ferric nitrate mixture, wherein M2+With Fe3+Mol ratio be 1: 12, wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one kind；
B. by polyvinylpyrrolidone, ethanol, barium acetate, butyl titanate, glacial acetic acid and water, mixed preparing sandwich layer is molten in proportion 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 the mol ratio of barium acetate and butyl titanate is 1:1；
The molecular weight of polyvinylpyrrolidone described in step A and step B is 100000-130000；
C. above-mentioned shell solution is placed in coaxial electrostatic spinning outer tube, sandwich layer solution is placed in coaxial electrostatic spinning inner tube, made respectively For coaxial electrostatic spinning outer layer and internal layer；Outer tube carries out electrostatic spinning, its technological parameter using No. 8 No. 16 syringe needles, inner tube syringe needles For：Voltage 10-20kV, ectonexine fltting speed 0.3-2mL/h, receive distance 10-20cm, rotating speed 200-500rpm, spinning temperature 25-40 DEG C of degree；Obtain composite precursor fiber；
D. by the composite precursor fiber that step C is obtained in 50-100 DEG C of drying；Then risen to 1-5 DEG C/min heating rate 600-800 DEG C of roasting 1-5h, with the near room temperature of 1-5 DEG C/min rate of temperature fall, obtains MFe12O19/BaTiO3Nano-composite fiber； Wherein M2+Represent bivalent metal ion Sr2+、Ba2+、Pb2+In one kind；The 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, and surface is smooth.
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CN106492779B (en) * 2016-09-29 2019-02-01 李跃军 Core-shell structure rare earth titanate-dioxide composite nanofiber catalysis material preparation method
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
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
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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