CN102286805B - Li-Zn ferrite magnetic nanometer fiber and preparation method thereof - Google Patents
Li-Zn ferrite magnetic nanometer fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a Li-Zn ferrite magnetic nanometer fiber and a preparation method thereof. The spinel type Li-Zn ferrite magnetic nanometer fiber is prepared by adopting a high-voltage electrostatic spinning technology which comprises the following technical steps of: 1, preparing spinning solution; 2, carrying out electrostatic spinning to prepare the precursor fiber; and 3, carrying out high-temperature calcinations to obtain the pure phase crystal Li-Zn ferrite continuous nanometer fiber. The appearance of the target nanometer fiber can be perfectly controlled through regulating the chemical composition of the solution and the electric spinning process parameters. The method and the equipment provided by the invention are simple, the cost is low, a large amount of Li-Zn ferrite magnetic nanometer fiber can be continuously prepared, the diameter of the obtained fiber is 50 to 100nm, good magnetism can be obtained at the room temperature, and the wide application aspects are realized in the fields such as micro nanometer electronic devices, magnetic sensors, flexible magnetic bodies, microwave absorption, electromagnetic shielding and the like.
Description
Technical field
The invention belongs to the magnetic Nano material field, be specifically related to a kind of ferrite nano fiber and technology of preparing thereof.
Background technology
One-dimensional magnetic nano material such as nanotube, nanobelt, nano wire and nanofiber etc. not only have various special effectses such as the small-size effect of common nano particle, skin effect, quantum size effect, macro quanta tunnel effect, coulomb blockade and quantum tunneling effect and Dielectric confinement effect etc., but also have unique shape anisotropy and magnetic anisotropy, at optics, electricity, the aspects such as magnetic property have shown and have been different from corresponding body material, the excellent specific property of nano particle and film, this is so that they are in the very big interest that has caused people aspect basic research and the high-tech application and showing great attention to, be considered to construct the important constituent element of new function electromagnetic functional material and device, be expected at high density magnetic recording, Sensitive Apparatus, the micro-nano electronic device, the nanometer magnet, spin electric device, electro-magnetic wave absorption, the aspects such as catalysis and biomedicine obtain practical application.
Along with developing rapidly of microwave and microelectronic engineering technology, advanced absorbing material becomes increasingly conspicuous in the importance in the fields such as anti-electromagnetic interference and stealth technology.The magnetic fibre absorbent is because its shape anisotropy and magnetic anisotropy, can obtain very high magnetic conductivity at long axis direction, can break away from the isotropism dusty material to the restriction of Effective permeability, therefore can in the smaller situation of duty, obtain higher magnetic conductivity, thereby be conducive to alleviate coating weight and widen frequency band to electro-magnetic wave absorption.So after the magnetic nano powder absorbent, the development of magnetic micro nanometer fiber absorbent and exploitation become a focus in this field gradually.At present domestic and international research to the magnetic fibre absorbent mainly concentrates on magnetic metal and the alloy micro nanometer fiber absorbent thereof, but its low non-oxidizability, susceptibility-to-corrosion and high frequency Kelvin effect etc. will affect again them in the serviceability of extreme environment.The ferrite micro nanometer fiber not only has traditional ferritic low-dielectric, high resistivity and is easy to the advantages such as coupling, but also have than features such as the higher non-oxidizability of magnetic metal and alloy fiber and corrosion resistances, the shape anisotropy of fiber also helps the natural resonant frequency that overcomes ferrite itself and crosses the low and lower problems such as the Snoek limit simultaneously, thereby can greatly improve it in magnetic conductivity and magnetic loss and the frequency of utilization scope of microwave frequency band, be expected to develop into a kind of novel high-performance microwave absorption that can satisfy the Modern Stealth Technique growth requirement.
One-dimensional magnetic preparations of nanomaterials method is varied, roughly can be divided into the physical template assisting growth and synthesize two aspects without templated chemistry.Template assisting growth technology often utilizes the concrete grammars such as space confinement effect combined with electrochemical deposition, chemical deposition or epitaxial growth of template (such as porous anodic alumina films, porous polycarbonate film, mesopore molecular sieve, CNT etc.) that magnet is grown in the duct of template, thus the magnetic material that acquisition has the one-dimentional structure feature.With respect to template, prepare the one-dimensional magnetic nano material without the templated chemistry synthetic method and then seem more convenient and flexible.The one, its equipment is simple, small investment, and output is larger, is easy to be converted into suitability for industrialized production; The 2nd, can control by number of ways pattern parameter and the high preferred orientation of one-dimensional nano structure, obtain to have different microstructural one-dimensional nano structure magnetic materials.Mainly comprise liquid phase and magnetic field auxiliary liquid phase method, induced by magnetic field organic metal thermal decomposition method and method of electrostatic spinning etc. without the templated chemistry synthetic method.Method of electrostatic spinning is that polymer solution or melt spray the silk stretching and a kind of technology of preparing of formation superfine fibre by means of the high-pressure electrostatic effect, at first being proposed in 1934 by Formhals, is a kind of simple, the effective ways that prepare continuous, as to have macro length micro nanometer fiber.Because electrostatic spinning technique is very strict to the requirement of spinning solution viscosity, so originally mainly be used to prepare the high polymer micro nanometer fiber.Over past ten years, the solution that it is found that the sol-gel process preparation also can satisfy electrostatic spinning well to the requirement of viscosity, become gradually possibility so inorganic matter is carried out Electrospun, utilize at present this technology successfully to prepare a large amount of inorganic matters and inorganic-inorganic composite micro-nano rice fiber.
The Li-Zn ferrite is the very important spinel structure soft magnetic materials of a class, have that high resistance is high, squareness ratio and Curie temperature, the characteristics such as the saturation magnetization adjustable range is wide, remanent magnetism counter stress sensitiveness is low, temperature stability good, magnetostriction coefficient is low and microwave dielectric loss is little and be widely used in making the microwave devices such as microwave frequency band phase shifter, isolator, circulator, at aspects such as electro-magnetic wave absorption and anti-electromagnetic interference important application is arranged also simultaneously.So far, people mainly concentrate on nano-powder and the film the development of Li-Zn ferrite nano material, there is not yet the report of relevant Li-Zn ferrite one-dimensional nano structure material.
Summary of the invention
Only exist Li-Zn ferrite magnetic nano powder and film not to have the problem of Li-Zn ferrimagnetism one-dimensional nano structure in order to solve prior art, the invention provides Li-Zn ferrite magnetic nano fiber and preparation method thereof, method technique is simple, and is raw materials used and equipment is cheap.The prepared Li-Zn ferrite nano of the present invention fiber is single-phase cubic spinel structure, and pattern is controlled, and fibre diameter is about 50～100nm, at room temperature has good magnetic.
Technical scheme of the present invention is: a kind of preparation method of Li-Zn ferrite magnetic nano fiber, adopt the solution method of electrostatic spinning to prepare polymer/metal inorganic salts composite precursor fiber, and then through suitably naturally cooling to the Li-Zn ferrite nano fiber product that room temperature obtains the pure phase crystalline state after the roasting heat processing.Wherein, the preparation of spinning solution is according to chemical formula Li
0.5-0.5xZn
xFe
2.5-0.5xO
4The desired stoichiometric proportion in 0＜x＜1 is the ratio Li of amount of substance: Zn: Fe=0.5-0.5x: x: 2.5-0.5x takes by weighing corresponding metal inorganic salt and joins to be stirred in the polymer solution and form homogeneous phase, transparent, stable spinning solution, and described metal inorganic salt is nitrate or the acetate of lithium metal, zinc and iron.
Sintering temperature is 350～600 ℃ during described heat treatment, temperature retention time 1～3 hour, 2～5 ℃/min of heating rate.
Polymer in the described polymer solution is any one in polyvinylpyrrolidone, polyvinyl alcohol, the polyacrylonitrile, and solvent is the arbitrary or several arbitrary proportion mixture in water, ethanol or the dimethyl formamide.
Technological parameter during electrostatic spinning is: voltage 10～25kV, solution feed rate 0.3～1.0mL/h, receiving range 10～25cm, 15～30 ℃ of temperature, humidity 35～60%RH.
The mass fraction of polymer is 3～15% in the described spinning solution, and the mass fraction of slaine is 4～20%.The external diameter of used syringe needle is 0.7～0.9mm during the solution electrostatic spinning.
The Li-Zn ferrite magnetic nano fiber that the preparation method of described Li-Zn ferrite magnetic nano fiber prepares, fibre diameter is 50～100nm, pure cubic spinel structure, space group are Fd3m, at room temperature have good magnetic.
Beneficial effect:
1, the preparation method is simple, and is with low cost, and productive rate is higher.
2, microscopic appearance is good, and fibre diameter reaches real nanometer scale, is about 50～100nm, and draw ratio is high, and monodispersity is good.
3, at room temperature have good magnetic, the Li-Zn ferrite nano particles close with size compared, and Li-Zn ferrite nano fiber is owing to its significant shape anisotropy shows higher coercivity.
4, this product has broad application prospects in fields such as micro-nano electronic device, Magnetic Sensor, flexible magnet, microwave absorption and electromagnetic shieldings.
5, the present invention adopts the method for solution electrostatic spinning to prepare Li-Zn ferrite nano fiber, and its diameter can be controlled in below the 100nm.Gained Li-Zn ferrite nano fiber at room temperature has good magnetic, and can regulate and control by changing preparation technology parameter and chemical composition easily, has potential application prospect in high-tech sectors such as electro-magnetic wave absorption.
Description of drawings
Fig. 1 is experimental provision schematic diagram used in the present invention; Wherein 1 is syringe pump, and 2 is reservoir, and 3 is spinning head, 4 spinning solutions for ejection, and 5 is collector.
Fig. 2 is the electron scanning micrograph of the PVP/ inorganic salts composite precursor fiber of the embodiment of the invention 1 preparation;
Fig. 3 is the Li of the embodiment of the invention 1 preparation
0.35Zn
0.3Fe
2.35O
4The electron scanning micrograph of nanofiber;
Fig. 4 is the Li of the embodiment of the invention 1 preparation
0.35Zn
0.3Fe
2.35O
4The transmission electron microscope photo of nanofiber;
Fig. 5 is the Li of the embodiment of the invention 1 preparation
0.35Zn
0.3Fe
2.35O
4The X-ray diffraction spectrogram of nanofiber;
Fig. 6 is the Li of the embodiment of the invention 1 preparation
0.35Zn
0.3Fe
2.35O
4The room temperature hysteresis curve of nanofiber.
The specific embodiment
Following case study on implementation will the present invention will be further described.
The present invention adopts first the solution electrostatic spinning technique to prepare polymer/metal inorganic salts composite precursor fiber, and then makes the Li-Zn ferrite nano fiber product of pure phase crystalline state through suitable heat treatment process.
The used electrostatic spinning apparatus of the present invention is according to disclosed electrostatic spinning machine principle and structure assemble voluntarily, the lab scale that is applicable to carry out in the laboratory uses, as shown in Figure 1, mainly by DC high-voltage power supply (0～30kV), reservoir, spinning head, syringe pump and the several parts of collector consist of.Collector used in the present invention can be disk, cylinder, metallic plate, metal grill, tinfoil paper, aluminium foil etc.What reservoir used in this experiment is plastic injector, and what spinning head used is the stainless steel syringe needle.
Its concrete steps are:
(1) preparation of spinning solution: polymer is dissolved in the coordinative solvent, and magnetic agitation to polymer dissolves fully, then according to chemical formula Li
0.5-0.5xZn
xFe
2.5-0.5xO
4(0＜x＜1) desired stoichiometric proportion is Li: nitrate or acetate that Zn: Fe=0.5-0.5x: x: 2.5-0.5x takes by weighing an amount of lithium metal, zinc and iron join in the above-mentioned polymer solution in the lump, continue magnetic agitation about 2～15 hours, and formed homogeneous phase, transparent, stable spinning solution.The mass fraction of polymer is 3～15% in this solution, and is preferred 5～10%, and the mass fraction of slaine is 4～20%, preferred 6～12%, and all the other are solvent.
(2) electrostatic spinning process: above-mentioned spinning solution is transferred in the plastic injector with the stainless steel syringe needle, the external diameter of stainless steel syringe needle is 0.7～0.9mm, and be installed on the syringe pump, the stainless steel syringe needle links to each other with the positive pole of high voltage source, and collector links to each other and minus earth with the negative pole of high voltage source.Applying voltage is 10～25kV again, preferred 15～20kV, the solution feed rate is 0.3～1.0mL/h, preferred 0.5～0.8mL/h, receiving range is 10～25cm, preferred 15～20cm, and temperature is 15～30 ℃, humidity is to carry out electrostatic spinning under the condition of 35～60%RH, obtains the polymer/inorganic salt composite precursor fiber of lack of alignment.
(3) preparation of Li-Zn ferrite nano fiber: the precursor fibre of step (2) acquisition is put into program control electric furnace heat-treat in 80～100 ℃ of scopes after suitable drying, heating rate with 2～5 ℃/min is heated to 350～600 ℃ by room temperature, preferred 400～550 ℃, and under sintering temperature, be incubated 1～3 hour, naturally cool to room temperature with body of heater afterwards, can obtain Li-Zn ferrite nano fiber of the present invention.
The said polymer of the present invention is polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile etc., and preferably polyethylene pyrrolidones, mean molecule quantity are 1300000.
The said solvent of the present invention is water, ethanol or dimethyl formamide etc., preferred alcohol or water.
Embodiment 1
Get 1.5000g polyvinylpyrrolidone (PVP, average molecular weight Mw=1300000) join in the mixed solvent that 15.6600g absolute ethyl alcohol and 10.4400g deionized water form, after at room temperature magnetic agitation to polymer dissolves fully, taking by weighing 2.1440g ferric nitrate, 0.0545g lithium nitrate and 0.2015g zinc nitrate joins in the above-mentioned PVP solution in the lump again, continue about 10 hours of magnetic agitation to form homogeneous phase, transparent, stable spinning solution, wherein the quality percentage composition of PVP is 5wt%, and the quality percentage composition of inorganic salts is 8wt%.
The spinning solution that obtains is incorporated in the electrostatic spinning apparatus, apply again voltage 15kV, the solution feed rate is 0.5mL/h, receiving range is 15cm, temperature is 20～25 ℃, humidity is to carry out electrostatic spinning under 40～50% the condition, the pattern of the PVP/ inorganic salts composite precursor fiber that makes as shown in Figure 2, its average diameter is about 200nm.
The precursor fibre of preparation is put into program control electric furnace heat-treat after suitable drying, be heated to 500 ℃ with the heating rate of 3 ℃/min by room temperature, and be incubated 2 hours under this temperature, naturally cool to room temperature with body of heater afterwards, obtaining chemical composition is Li
0.35Zn
0.3Fe
2.35O
4Li-Zn ferrite nano fiber product.Prepared Li
0.35Zn
0.3Fe
2.35O
4The nanofiber microscopic appearance is good, and the diameter narrow distribution is about 50～100nm (seeing Fig. 3, shown in 4), has single-phase cubic spinel structure (as shown in Figure 5), and room temperature specific saturation magnetization and coercivity are respectively 74.7Am
2Kg
-1And 11.4kAm
-1(as shown in Figure 6).
Basic preparation process is with embodiment 1, and the chemical composition of different is inorganic salts is the ratio of metallic element amount of substance: the quality of ferric nitrate, lithium nitrate and zinc nitrate is respectively 2.2022,0.0626 and 0.1351g.Prepared Li
0.4Zn
0.2Fe
2.4O
4The diameter of nanofiber is 50～100nm, has single-phase cubic spinel structure, and room temperature specific saturation magnetization and coercivity are respectively 67.8Am
2Kg
-1And 14.5kAm
-1
Embodiment 3
Basic preparation process is with embodiment 1, and the chemical composition of different is inorganic salts is the ratio of metallic element amount of substance: the quality of ferric nitrate, lithium nitrate and zinc nitrate is respectively 1.8624,0.0151 and 0.5224g.Prepared Li
0.1Zn
0.8Fe
2.1O
4The diameter of nanofiber is 50～100nm, has single-phase cubic spinel structure, and room temperature specific saturation magnetization and coercivity are respectively 8Am
2Kg
-1And 2.4kAm
-1
Embodiment 4
Basic preparation process is with embodiment 1, and the sintering temperature of precursor fibre that different is is 450 ℃.Prepared Li
0.35Zn
0.3Fe
2.35O
4The diameter of nanofiber is 50～100nm, has single-phase cubic spinel structure, and room temperature specific saturation magnetization and coercivity are respectively 67.8Am
2Kg
-1And 9.5kAm
-1
Basic preparation process is with embodiment 1, and the sintering temperature of precursor fibre that different is is 550 ℃.Prepared Li
0.35Zn
0.3Fe
2.35O
4The diameter of nanofiber is 50～100nm, has single-phase cubic spinel structure, and room temperature specific saturation magnetization and coercivity are respectively 80.5Am
2Kg
-1And 12.6kAm
-1
Embodiment 6
Basic preparation process is with embodiment 1, and the content of different is PVP is 10%, and the content of inorganic salts is 5%.
Embodiment 7
Basic preparation process is with embodiment 1, and that different is electrostatic spinning voltage 20kV, and receiving range is 20cm.
Embodiment 8
Basic preparation process is with embodiment 1, and different is with lithium acetate and zinc acetate respectively alternative lithium nitrate and zinc nitrate: the quality of ferric nitrate, lithium acetate and zinc acetate is respectively 2.1681,0.0815 and 0.1504g in the raw material.
Embodiment 9
Basic preparation process is with embodiment 8, and different is that used high molecular polymer is polyacrylonitrile (PAN, average molecular weight Mw=150000), and solvent is dimethyl formamide (DMF), and the content of PAN is 6wt%.
Embodiment 10
Basic preparation process is with embodiment 8, and different is that used high molecular polymer is polyvinyl alcohol (PVA, average molecular weight Mw=80000), and solvent is deionized water, and the content of PVA is 8wt%, spinning voltage 20kV, receiving range 20cm.
Claims (7)
1. the preparation method of a Li-Zn ferrite magnetic nano fiber, it is characterized in that, adopt the solution method of electrostatic spinning to prepare polymer/metal inorganic salts composite precursor fiber, and then through suitably naturally cooling to the Li-Zn ferrite nano fiber product that room temperature obtains the pure phase crystalline state after the roasting heat processing, wherein, the preparation of spinning solution is according to chemical formula Li
0.5-0.5xZn
xFe
2.5-0.5xO
4The desired stoichiometric proportion in 0＜x＜1 is the ratio Li of amount of substance: Zn: Fe=0.5-0.5x: x: 2.5-0.5x takes by weighing corresponding metal inorganic salt and joins to be stirred in the polymer solution and form homogeneous phase, transparent, stable spinning solution, and described metal inorganic salt is nitrate or the acetate of lithium metal, zinc and iron.
2. the preparation method of Li-Zn ferrite magnetic nano fiber according to claim 1 is characterized in that, sintering temperature is 350～600 ℃ during described heat treatment, temperature retention time 1～3 hour, 2～5 ℃/min of heating rate.
3. the preparation method of Li-Zn ferrite magnetic nano fiber according to claim 1, it is characterized in that, polymer in the described polymer solution is any one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile, and solvent is arbitrary in water, ethanol or the dimethyl formamide or appoints several arbitrary proportion mixtures.
4. the preparation method of Li-Zn ferrite magnetic nano fiber according to claim 1 is characterized in that, the technological parameter during electrostatic spinning is: voltage 10～25kV, solution feed rate 0.3～1.0mL/h, receiving range 10～25cm, temperature is 15～30 ℃, humidity 35～60%RH.
5. the preparation method of Li-Zn ferrite magnetic nano fiber according to claim 1 is characterized in that, the mass fraction of polymer is 3～15% in the described spinning solution, and the mass fraction of slaine is 4～20%.
6. the preparation method of Li-Zn ferrite magnetic nano fiber according to claim 1 is characterized in that, the external diameter of used syringe needle is 0.7～0.9mm during the solution electrostatic spinning.
7. the Li-Zn ferrite magnetic nano fiber of the preparation method of arbitrary described Li-Zn ferrite magnetic nano fiber preparation according to claim 1～6, it is characterized in that described fibre diameter is 50～100nm, pure cubic spinel structure, space group is Fd3m, at room temperature has magnetic.
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| CN103232577B (en) * | 2013-04-02 | 2016-03-09 | 山东建筑大学 | A kind of magnetic nanometer composite material |
| CN103224595B (en) * | 2013-04-16 | 2015-11-11 | 山东建筑大学 | A kind of polymer-based nano absorbing material |
| CN103556304B (en) * | 2013-10-28 | 2015-12-09 | 江苏大学 | A kind of ferrite nanofiber strip and preparation method thereof |
| CN105200658B (en) * | 2014-06-30 | 2019-03-26 | 天津工业大学 | A kind of composite nano-fiber membrane and preparation method thereof for electromagnetic shielding |
| CN104313706A (en) * | 2014-09-29 | 2015-01-28 | 中鸿纳米纤维技术丹阳有限公司 | Novel high-efficiency nanofiber electrostatic spinning equipment |
| CN104451956B (en) * | 2014-12-25 | 2016-08-24 | 南京理工大学常熟研究院有限公司 | A kind of nanometer ferrite alloy material |
| CN107660111A (en) * | 2016-07-05 | 2018-02-02 | 中国人民解放军军械工程学院 | A kind of preparation method of amorphous li Zn ferrite cenosphere low-frequency wave-absorbing material |
| CN114566372B (en) * | 2022-03-14 | 2024-03-12 | 国网智能电网研究院有限公司 | Nickel-copper-zinc ferrite magnetic nano shuttle and preparation method thereof |
| CN114656269B (en) * | 2022-04-06 | 2023-04-07 | 中国科学院电工研究所 | Homogeneous fiber reinforced manganese-zinc ferrite material and preparation method thereof |
| CN115679479B (en) * | 2022-11-29 | 2024-10-01 | 厦门大学 | Spinel ferrite hollow fiber and preparation method thereof |
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| CN101914821B (en) * | 2010-05-14 | 2012-08-15 | 江苏大学 | Ni-Zn ferrite/SiO2 composite nano-fiber and preparation method thereof |
| CN101851814B (en) * | 2010-05-14 | 2012-11-07 | 江苏大学 | Iron-nickel alloy/nickel ferrite magnetic composite nanofiber and preparation method thereof |
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