CN102251305B - Preparation of cobalt nickel ferrite/ polyvinyl pyrrolidone composite magnetic nano fibers - Google Patents

Preparation of cobalt nickel ferrite/ polyvinyl pyrrolidone composite magnetic nano fibers Download PDF

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CN102251305B
CN102251305B CN 201110176335 CN201110176335A CN102251305B CN 102251305 B CN102251305 B CN 102251305B CN 201110176335 CN201110176335 CN 201110176335 CN 201110176335 A CN201110176335 A CN 201110176335A CN 102251305 B CN102251305 B CN 102251305B
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pvp
preparation
composite magnetic
polyvinyl pyrrolidone
cobalt nickel
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CN102251305A (en
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李耀刚
唐亚
王宏志
张青红
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Donghua University
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Abstract

The invention relates to a preparation method of cobalt nickel ferrite/ polyvinyl pyrrolidone (PVP) composite magnetic nano fibers. The preparation method comprises the following steps of: (1) preparing modified Co1-xNixFe2O4 nano particles; and (2) preparing PVP ethanol solution, uniformly dispersing the modified Co1-xNixFe2O4 nano particles obtained in the step (1) into the PVP ethanol solution, stirring the solution for 12 to 24 hours to obtain Co1-xNixFe2O4/ PVP mixed solution, and performing electrostatic spinning by using the Co1-xNixFe2O4/ PVP mixed solution as spinning stock solution to obtain the cobalt nickel ferrite/ PVP composite magnetic nano fibers. The preparation method is simple, can effectively improve the dispersibility of the magnetic particles in the polymer solution, has low requirement for production equipment, and is easy to realize industrialized production; and the diameter of the prepared magnetic fibers is distributed uniformly and in a range of 300 to 500 nanometers, and the magnetic fibers have good magnetic performance.

Description

The preparation of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers
Technical field
The invention belongs to the preparation field of nano-magnetic fibre, particularly relate to a kind of preparation method of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers.
Background technology
Nanofiber refers to have two dimension to be in line (pipe) material of nano-scale at three-dimensional space, and general diameter or caliber are nanoscale, and length is larger.The characteristics of nanofiber maximum are that its specific area is larger, cause its surface energy and surface-activity with respect to the zero-dimension nano material great raising to be arranged, thereby have excellent chemistry, physical property.Because these good character, nano-fiber material have become the forward position of new material research.Magnetic nanoparticle has unique the structure and magnetic properties, all has wide practical use in various fields such as biology, medical science, environmental protection.Partly substitute the non-single type ferrite forms by ion, its character often has very wide selectable range, thereby satisfies the needs of different application, but specific area is less and be easy to reunion and but limited its application.Ferrite particle is scattered in the polymer preparation one-dimensional inorganic particle nanofiber has greatly widened its application, and at present electrostatic spinning technique to prepare nanofiber be a kind of comparatively simple technology, the fibre diameter of preparation is less, continuity is better.
The cobalt Ni ferrite is a kind of complex ferrite of electromagnetic performance excellence, has the premium properties such as intensity of magnetization height, chemical stability be good.And polyvinylpyrrolidone (PVP) is both water-soluble, is dissolved in again majority of organic solvent, and toxicity is very low, the physiology intermiscibility is good, obtains a wide range of applications in the fields such as medicine, food, cosmetics.
Prepare the one-dimensional inorganic nanofiber by electrostatic spinning technique, mainly contain at present two kinds of methods, a kind of is to prepare first the inorganic matter precursor solution, solution is prepared into nonwoven fabric then obtains inorfil by post processings such as calcinings; Another kind is that the inorganic particle that will prepare is dispersed in the polymer solution, prepares inorfil by electrostatic spinning technique again.Present work mainly concentrates on front a kind of method, and the work that the latter carries out is less, and main problem is dispersed bad in polymer of the difficult control of the pattern of inorganic particle and size and particle.The people such as Montana Sangmanee have been reported to preparation Co (NO at Applied Physics A 97 (2009) 167～177 3) 2, Fe (NO 3) 3The PVP precursor solution, by the standby CoFe of diameter about 450nm of electro-spinning 2O 4Nano-magnetic fibre.The people such as Wichaid Ponhan have been reported to preparation Cu (NO at Solid State Sciences11 (2009) 479～484 3) 2, Fe (NO 3) 3The PVP precursor solution, by the standby CuFe of diameter about 90nm of electro-spinning 2O 4Nano-magnetic fibre.It is more that the work of precursor solution spinning is carried out, and is a kind of comparatively ripe technology, but it is less that inorganic nanoparticles is dispersed in the polymer work of direct fabrics, and main cause is that granule-morphology and dispersiveness are difficult to resolve and determine.The people such as Hang Wang have been reported to the Fe that utilizes about 20nm at Materials Research Bulletin 44 (2009) 1676-1680 3O 4Particle is dispersed in the PVP solution by the magnetic-particle nanofiber about the standby diameter 500nm of electro-spinning.The people such as Di Zhang have been reported to Fe at Polymer 50 (2009) 4189～4198 3O 4Nanoparticulate dispersed prepares the magnetic Nano fiber that diameter is evenly distributed by changing spinning parameter in PAN/DMF solution.
At present prepare the ferrite magnetic particle nanofiber by electrostatic spinning technique and mainly have following difficult point: ferrite particle is easy to sedimentation in polymer solution, cause its dispersiveness bad, directly causes distribution of fiber diameters uneven.
The magnetic Nano fiber has important using value in fields such as electro-magnetic wave absorption, catalysis materials, so the preparation of magnetic Nano fiber is the focus of studying at present.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers, and this preparation method is simple, is easy to suitability for industrialized production; Prepared composite magnetic nanofiber even particle distribution, distribution of fiber diameters homogeneous.
The preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers of the present invention comprises:
(1) cobalt Ni ferrite (Co 1-xNi xFe 2O 4) modification of nano particle
At room temperature, with cobalt Ni ferrite Co 1-xNi xFe 2O 4Nanoparticulate dispersed 300～600 turns/min stirs 1～2h, make Co in toluene 1-xNi xFe 2O 4Nano particle is dispersed in the toluene; Then under nitrogen atmosphere, dripping 1/5～1/15 methacrylic acid 3-(trimethoxy is silica-based) propyl ester (KH-570) for volume of toluene, 300～600 turn under the room temperature/after min stirs 4～6h, collect product with magnet, washing, oven dry namely gets modification Co 1-xNi xFe 2O 4Nano particle; Wherein the mass volume ratio of ferrite particle and toluene solution is 1: 12～1: 20g/ml;
(2) Co 1-xNi xFe 2O 4The preparation of/PVP composite magnetic nanofiber
Polyvinylpyrrolidone PVP is dissolved in the absolute ethyl alcohol, and stirring at room 12～24h obtains the PVP ethanolic solution; Modification Co with step (1) gained 1-xNi xFe 2O 4Nano particle is dispersed in the described PVP ethanolic solution, and 300～600 turn under the room temperature/and min stirs 12～24h, gets Co 1-xNi xFe 2O 4/ PVP mixed liquor; With described Co 1-xNi xFe 2O 4/ PVP mixed liquor carries out electrostatic spinning as spinning solution, namely gets the cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers.
The trade mark of methacrylic acid 3-(trimethoxy the is silica-based) propyl ester (KH-570) described in the step (1) is A-174 (U.S. combinating carbide company), KBM-503 (Japanese SHIN-ETSU HANTOTAI) or SH-6030 (Dow corning company), and preferentially selecting the trade mark is the KH-570 of A-174.
Washing described in the step (1) is for cleaning with carrene and ethanol.
Bake out temperature described in the step (1) is 40～60 ℃, and the time is 12～24h.
The molecular weight of the polyvinylpyrrolidone described in the step (2) is 30000-1300000.
The mass fraction of PVP ethanolic solution is 8～10% described in the step (2).
Co described in the step (2) 1-xNi xFe 2O 4Co in the/PVP mixed liquor 1-xNi xFe 2O 4The mass ratio of particle and PVP is 2: 1～4: 1.
Being operating as of electrostatic spinning described in the step (2): with described Co 1-xNi xFe 2O 4/ PVP mixed liquor is poured in the syringe, then described syringe is fixed on the miniflow pump, advancing speed is 20～40 μ L/min, and nozzle is 10～20cm with the distance that receives aluminium foil, adds 10～15kV electrostatic field and carry out spinning and obtain magnetic fibre between nozzle and reception aluminium foil.
The cobalt Ni ferrite Co that adopts among the present invention 1-xNi xFe 2O 4Nano particle is take ethylene glycol as solvent, and solvent-thermal method synthesizes cobalt Ni ferrite Co 1-xNi xFe 2O 4Nano particle (0＜x＜1); Its concrete preparation method sees Chinese patent CN101891483A, and open day is on November 24th, 2010.
The present invention is by to the ferrite particle modifying surface, so that itself and polymer end of the chain generating keys close, solved ferrite particle and be easy to sedimentation in polymer solution, causes its dispersiveness bad, thereby directly causes the problem of distribution of fiber diameters inequality.
Beneficial effect
(1) preparation method's technique of the present invention is simple, and is low to the production equipment requirement, is easy to suitability for industrialized production;
(2) preparation method of the present invention compares preparation precursor solution electrostatic spinning, prepared composite magnetic nanofiber need not the post processings such as calcining, in the spinning process, magnetic nanoparticle is difficult for occuring sedimentation in polymer, the magnetic-particle good dispersion can effectively be avoided the extensive reunion of ferrite particle;
(3) the prepared composite magnetic nanofiber diameter of the present invention is evenly distributed, and has good magnetic property.
Description of drawings
Fig. 1. be the infrared spectrum of the modified cobalt Ni ferrite particle of embodiment 1;
Fig. 2. be the Co of embodiment 1 1-xNi xFe 2O 4The stereoscan photograph of/PVP composite magnetic nanofiber;
Fig. 3. be the Co of embodiment 1 1-xNi xFe 2O 4The hysteresis curve figure of/PVP composite magnetic nanofiber.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
(1) takes by weighing 1.35g Co 1-xNi xFe 2O 4(x=0.2) particle, be dispersed in the toluene solution of 18ml, 600 turn under the room temperature/min mechanical ultrasonic stirring 1h, then under nitrogen atmosphere, drip 3.6ml Silane coupling reagent KH-570 (trade mark is A-174), 300 turn under the room temperature/min mechanical ultrasonic stirring 6h, collect product with magnet, and carrene and ethanol clean, 50 ℃ of baking 18h namely get modification Co 0.8Ni 0.2Fe 2O 4Nano particle;
(2) taking by weighing 0.45g PVP (30000) is dissolved in the 5.2ml ethanol, 600 turn under the room temperature/min mechanical ultrasonic stirring 12h, 1.35g modified cobalt Ni ferrite particle is dispersed in the PVP solution, making the mass ratio of ferrite particle and PVP is 3: 1,600 turn under the room temperature/and min mechanical ultrasonic stirring 12h, in mixed liquor injected plastic syringe, be fixed on the micro-fluid pump, at the fltting speed of 20 μ L/min, the electrostatic field of 10kV obtains Co under the acceptance distance of 20cm 0.8Ni 0.2Fe 2O 4/ PVP composite magnetic nanofiber.
Fig. 1 is Fourier's infrared spectrum of present embodiment modification ferrite particle, and absworption peak is at 580cm among the figure -1The place is the Fe-O key in the cobalt Ni ferrite, and absworption peak is at 1017cm -1And 1172cm -1The place is the C-O singly-bound, and absworption peak is at 1700cm -1The place is the two keys of C=O, and absworption peak is at 1460cm -1, 2850cm -1And 2926cm -1The place is CH 2Group, the existence of these absworption peaks show Silane coupling reagent KH-570 with the magnetic-particle surface grafting, embedding figure is modification ferrite particle and the settleability contrast of unmodified ferrite particle in ethanol, a is the modification ferrite particle among the figure, b is unmodified ferrite particle, a still is muddy after the week as seen from the figure, shows that modified effect is good.
Fig. 2 is the field emission scanning electron microscope figure of present embodiment magnetic fibre, can find out that distribution of fiber diameters is comparatively even, in 300～500nm scope.Fig. 3 is the hysteresis curve figure of the resulting magnetic fibre of present embodiment, can find out that this composite magnetic nanofiber intensity of magnetization is higher, reaches 30emu/g.
Embodiment 2
(1) takes by weighing 1.6g Co 1-xNi xFe 2O 4(x=0.6) particle, be dispersed in the toluene solution of 25ml, 300 turn under the room temperature/min mechanical ultrasonic stirring 2h, then under nitrogen atmosphere, drip 1.75ml Silane coupling reagent KH-570 (trade mark is SH-6030), 600 turn under the room temperature/min mechanical ultrasonic stirring 4h, collect product with magnet, and carrene and ethanol clean, 40 ℃ of baking 24h namely get modification Co 0.4Ni 0.6Fe 2O 4Nano particle; Fourier's infrared spectrum of modification ferrite particle show Silane coupling reagent KH-570 with the magnetic-particle surface grafting.
(2) taking by weighing 0.4g PVP (100000) is dissolved in the 5.8ml ethanol, 400 turn under the room temperature/min mechanical ultrasonic stirring 18h, 1.6g modified cobalt Ni ferrite particle is dispersed in the PVP solution, making the mass ratio of ferrite particle and PVP is 4: 1,400 turn under the room temperature/and min mechanical ultrasonic stirring 18h, in mixed liquor injected plastic syringe, be fixed on the micro-fluid pump, at the fltting speed of 40 μ L/min, the electrostatic field of 15kV obtains Co under the acceptance distance of 10cm 0.4Ni 0.6Fe 2O 4/ PVP composite magnetic nanofiber.
ESEM display fibers diameter distributes comparatively even, and fibre diameter is in 300～500nm scope.Hysteresis curve figure test shows: this magnetic fibre has good magnetic property.
Embodiment 3
(1) takes by weighing 1.0g Co 1-xNi xFe 2O 4(x=0.4) particle, be dispersed in the toluene solution of 20ml, 400 turn under the room temperature/min mechanical ultrasonic stirring 1.5h, then under nitrogen atmosphere, drip 2.0ml Silane coupling reagent KH-570 (trade mark is KBM-503), 400 turn under the room temperature/min mechanical ultrasonic stirring 5h, collect product with magnet, and carrene and ethanol clean, 60 ℃ of baking 12h namely get modification Co 0.4Ni 0.6Fe 2O 4Nano particle; Fourier's infrared spectrum of modification ferrite particle show Silane coupling reagent KH-570 with the magnetic-particle surface grafting.
(2) taking by weighing 0.5g PVP (1300000) is dissolved in the 6.4ml ethanol, 600 turn under the room temperature/min mechanical ultrasonic stirring 12h, 1.0g modified cobalt Ni ferrite particle is dispersed in the PVP solution, making the mass ratio of ferrite particle and PVP is 2: 1,300 turn under the room temperature/and min mechanical ultrasonic stirring 24h, in mixed liquor injected plastic syringe, be fixed on the micro-fluid pump, at the fltting speed of 30 μ L/min, the electrostatic field of 12kV obtains Co under the acceptance distance of 15cm 0.6Ni 0.4Fe 2O 4/ VP composite magnetic nanofiber.
ESEM display fibers diameter distributes comparatively even, and fibre diameter is in 300～500nm scope.Hysteresis curve figure test shows: this magnetic fibre has good magnetic property.

Claims (7)

1. the preparation method of a cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers comprises:
(1) at room temperature, with cobalt Ni ferrite Co 1-xNi xFe 2O 4Nanoparticulate dispersed 300～600 turns/min stirs 1～2h in toluene; Then under nitrogen atmosphere, drip for 1/5～1/15 methacrylic acid 3-(trimethoxy of volume of toluene silica-based) propyl ester, 300～600 turn under the room temperature/after min stirs 4～6h, collect product with magnet, washing, oven dry namely gets modification Co 1-xNi xFe 2O 4Nano particle; Wherein the mass volume ratio of ferrite particle and toluene solution is 1:12～1:20g/ml;
(2) polyvinylpyrrolidone PVP is dissolved in the absolute ethyl alcohol, stirring at room 12～24h obtains the PVP ethanolic solution; Modification Co with step (1) gained 1-xNi xFe 2O 4Nano particle is dispersed in the described PVP ethanolic solution, and 300～600 turn under the room temperature/and min stirs 12～24h, gets Co 1-xNi xFe 2O 4/ PVP mixed liquor; With described Co 1-xNi xFe 2O 4/ PVP mixed liquor carries out electrostatic spinning as spinning solution, namely gets the cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers; The span of described x is 0.2～0.6.
2. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1 is characterized in that: the washing described in the step (1) is for cleaning with carrene and ethanol.
3. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1, it is characterized in that: the bake out temperature described in the step (1) is 40～60 ℃, the time is 12～24h.
4. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1, it is characterized in that: the molecular weight of the polyvinylpyrrolidone described in the step (2) is 30000-1300000.
5. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1, it is characterized in that: the mass fraction of PVP ethanolic solution is 8～10% described in the step (2).
6. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1 is characterized in that: Co described in the step (2) 1-xNi xFe 2O 4Co in the/PVP mixed liquor 1-xNi xFe 2O 4The mass ratio of particle and PVP is 2:1～4:1.
7. the preparation method of a kind of cobalt nickel ferrite/polyvinyl pyrrolidone composite magnetic nano fibers according to claim 1 is characterized in that: being operating as of the electrostatic spinning described in the step (2): with described Co 1-xNi xFe 2O 4/ PVP mixed liquor is poured in the syringe, then described syringe is fixed on the miniflow pump, and advancing speed is 20～40 μ L/min, and nozzle is 10～20cm with the distance that receives aluminium foil, adds 10～15kV electrostatic field and carry out spinning between nozzle and reception aluminium foil.
CN 201110176335 2011-06-28 2011-06-28 Preparation of cobalt nickel ferrite/ polyvinyl pyrrolidone composite magnetic nano fibers Expired - Fee Related CN102251305B (en)

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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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