CN101475368A - Process for preparing nickel-zine ferrite (NixZn1-xFe2O4) magnetic nano powder by alcohol-heating method - Google Patents

Process for preparing nickel-zine ferrite (NixZn1-xFe2O4) magnetic nano powder by alcohol-heating method Download PDF

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CN101475368A
CN101475368A CNA2009100451236A CN200910045123A CN101475368A CN 101475368 A CN101475368 A CN 101475368A CN A2009100451236 A CNA2009100451236 A CN A2009100451236A CN 200910045123 A CN200910045123 A CN 200910045123A CN 101475368 A CN101475368 A CN 101475368A
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nickel
zinc
salt
magnetic nano
nano powder
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李耀刚
闫伟
张燕玲
王宏志
张青红
朱美芳
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Donghua University
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Donghua University
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Abstract

The invention relates to a method for preparing nickel zinc ferrite NixZn1-xFe2O4 magnetic nanometer powder through an alcohol heating method. The method comprises the following steps: weighing iron salt, zinc salt and nickel salt and dissolving the iron salt, zinc salt and nickel salt in ethylene glycol at a room temperature, carrying out the ultrasonic dispersion, then adding anhydrous sodium acetate and a polyethylene glycol dispersant, carrying out the mechanical mixing, adding the mixture into a reaction kettle after complete dissolution, cooling down the mixture to the room temperature after the complete reaction, collecting the product through a magnet, washing the product through deionized water and drying the product to obtain the NixZn1-xFe2O4 magnetic nanometer powder. The preparation method has a simple process and is easy for the industrialized production. The NixZn1-xFe2O4 magnetic nanometer powder prepared through the method has a pure crystal phase, good dispersilbility, uneasy agglomeration and higher magnetization; and the magnetic material has the wide application prospect in the industrial and high-tech field due to the unique magnetic performance of the material.

Description

The hot legal system of a kind of alcohol is equipped with nickel-zinc ferrite (Ni xZn 1-xFe 2O 4) method of magnetic nano powder
Technical field
The invention belongs to nickel-zinc ferrite (Ni xZn 1-xFe 2O 4) preparation field of magnetic nano powder, particularly relate to the hot legal system of a kind of alcohol and be equipped with nickel-zinc ferrite (Ni xZn 1-xFe 2O 4) method of magnetic nano powder.
Background technology
Ni xZn 1-xFe 2O 4It is a kind of important magneticsubstance.Ni xZn 1-xFe 2O 4It is soft magnetic ferrite with spinel structure, the nanocrystalline synthetic and performance study of nickel-zinc ferrite becomes a focus of research field day by day, this be since the spinel type nickel-zinc ferrite as a kind of soft magnetic material, have high resistivity and high saturation and magnetic intensity, be widely used in the pointer read-write head of high speed, lightning rod, magnetic resonance device and electromagnetic wave absorbent material.Zahi S. etc. make respectively with sol-gel method and traditional china-clay method at the last report of MaterialsChemistry and Physics 106 (2007) 452-456 and form identical nickel-zinc ferrite (Ni xZn 1-xFe 2O 4).Cao Huiqun etc. got the nickel-zinc ferrite nano particle that particle diameter is 10-20nm with the hydro-thermal legal system in that Rare Metal Materials And Engineering37 (2008) 473-476 is last.J.S.Lee etc. are at Appl.Phys.A 74[Suppl.], S568-S570 (2002) goes up report and prepares the nickel-zinc ferrite nano particle by spreading method certainly.I.H.Gul etc. prepare the nickel-zinc ferrite nano particle at the last report of Journal of Magnetism and Magnetic Materials 320 (2008) 270-275 by chemical coprecipitation.This shows Ni xZn 1-xFe 2O 4Because of its unique magnetic property, absorbing property, in industry, fields such as military affairs have a wide range of applications.Do not see at present and adopt pure hot legal system to be equipped with Ni xZn 1-xFe 2O 4The report of magnetic nano powder.
Summary of the invention
Technical problem to be solved by this invention provides the hot legal system of a kind of alcohol and is equipped with nickel-zinc ferrite (Ni xZn 1-xFe 2O 4) method of magnetic nano powder, this preparation method's technology is simple, is easy to suitability for industrialized production; Prepared Ni xZn 1-xFe 2O 4The magnetic nano powder crystalline phase is pure, good dispersity, be difficult for to reunite, the specific magnetising moment is higher; This magneticsubstance is gathered around in industry and high-tech area because of its unique magnetic property and is had broad application prospects.
The hot legal system of a kind of alcohol of the present invention is equipped with nickel-zinc ferrite (Ni xZn 1-xFe 2O 4) method of magnetic nano powder, comprising:
Under the room temperature, taking by weighing 1/2～3/4 the concentration that molysite, zinc salt, nickel salt be dissolved in for the reactor volume is in the ethylene glycol of 98～99.5wt%, wherein Zn 2+And Ni 2+Mole ratio be 1:4～4:1; Zn 2+And Ni 2+Mole number sum and Fe 3+The ratio of mole number be 1:2, ultra-sonic dispersion 30～60min adds and Fe again 3+The ratio of mole number be: the anhydrous sodium acetate of 8:1～12:1,1/50～1/25 polyoxyethylene glycol dispersion agent for the ethylene glycol volume, mechanical stirring 20～60min, rotating speed is 500～800 rev/mins, after treating to dissolve fully mixture is put into reactor, be warming up to 180～220 ℃, reaction 9～12h after the complete reaction, is cooled to room temperature, collect product, deionized water wash product with magnet, 40～80 ℃, 15～24h oven dry obtain Ni xZn 1-xFe 2O 4Magnetic nano powder.
Described molysite, zinc salt, nickel salt are iron, nickel, the muriate of zinc, nitrate, the vitriol of solubility, preferentially use the muriate (FeCl of iron 36H 2O), the nitrate of nickel (Ni (NO 3) 2H 2O), the nitrate of zinc (Zn (NO 3) 26H 2O).The molecular weight of described polyoxyethylene glycol dispersion agent is 200～1000.
With respect to common liquid phase method, magnetic nanoparticle is more stable in organic phase, is difficult for generating the impurity phase.Because in liquid phase, magnetic nano-particle is very easily reunited because of the effect that is subjected to solion intensive electrostatic attraction, so present method selects electrostatic stabilization for use good anhydrous sodium acetate adds as alkaline reagents, to prevent Ni xZn 1-xFe 2O 4Extensive reunion.
Beneficial effect
(1) preparation technology is simple, and is low to the production unit requirement, is easy to suitability for industrialized production;
(2) prepared Ni xZn 1-xFe 2O 4The magnetic nanometer composite material crystalline phase is pure, good dispersity, be difficult for to reunite specific magnetising moment height.
Description of drawings
The transmission electron microscope photo of Fig. 1 synthetic powder;
The X-ray diffractogram of Fig. 2 synthetic powder;
The magnetic hysteresis loop figure of Fig. 3 synthetic powder.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described 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 institute restricted portion equally.
Embodiment 1
Take by weighing the high iron(ic) chloride of 1.351g, 0.145g zinc nitrate hexahydrate, 0.595g zinc nitrate hexahydrate, add three-necked flask, add 50ml ethylene glycol again, ultra-sonic dispersion 60min.After treating ultra-sonic dispersion, add 3.6g anhydrous sodium acetate, 1ml Macrogol 200 again, be 500 rev/mins of following mechanical stirring 30min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 220 ℃, reaction 9h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 40 ℃ of following vacuum-drying 24h, obtain Ni xZn 1-xFe 2O 4Nano-powder.Fig. 1 is the X-ray diffractogram of present embodiment synthetic powder, and the diffraction peak among the figure shows: this nano-powder is Ni xZn 1-xFe 2O 4Fig. 2 is the transmission electron microscope photo of synthetic powder, as can be seen: Ni xZn 1-xFe 2O 4The Nano microsphere particle diameter is at 50～150nm, Ni xZn 1-xFe 2O 4Nano microsphere is by a plurality of Ni xZn 1-xFe 2O 4The directed gathering of nanocrystal forms.Fig. 3 is the magnetic hysteresis loop figure of this magnetic nano powder, and as can be seen: the specific magnetising moment of this nano-powder is higher, reaches 60.41emu/g.
Embodiment 2
Take by weighing the high iron(ic) chloride of 1.351g, 0.297g zinc nitrate hexahydrate, 0.436g six water nickelous nitrates, add three-necked flask, add 50ml ethylene glycol again, ultra-sonic dispersion 30min.After treating ultra-sonic dispersion, add 3.6g anhydrous sodium acetate, 0.8ml poly(oxyethylene glycol) 400 again, be 500 rev/mins of following mechanical stirring 60min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 180 ℃, reaction 12h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 80 ℃ of following vacuum-drying 15h, obtain Ni xZn 1-xFe 2O 4Nano-powder.The XRD test result shows: this nano-powder is Ni xZn 1-xFe 2O 4Transmission electron microscope observing shows: Ni xZn 1-xFe 2O 4The Nano microsphere particle diameter is at 50～150nm, the Ni in this nano-powder xZn 1-xFe 2O 4Nano microsphere is that a plurality of Ni are arranged xZn 1-xFe 2O 4The directed gathering of nanocrystal forms.The magnetic hysteresis loop figure of this magnetic nano powder shows: the specific magnetising moment of this nano-powder is higher, reaches 57.01emu/g.
Embodiment 3
Take by weighing the high iron(ic) chloride of 1.351g, 0.372g zinc nitrate hexahydrate, 0.363g six water nickelous nitrates, add three-necked flask, add 50ml ethylene glycol again, ultra-sonic dispersion 45min.After treating that ultra-sonic dispersion finishes, add 3.6g anhydrous sodium acetate, 0.6ml Polyethylene Glycol-600 again, be 500 rev/mins of following mechanical stirring 30min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 10h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 70 ℃ of following vacuum-drying 18h, obtain Ni xZn 1-xFe 2O 4Nano-powder.The XRD test result shows: this nano-powder is Ni xZn 1-xFe 2O 4Transmission electron microscope observing shows: Ni xZn 1-xFe 2O 4The Nano microsphere particle diameter is at 50～150nm, the Ni in this nano-powder xZn 1-xFe 2O 4Nano microsphere is that a plurality of Ni are arranged xZn 1-xFe 2O 4The directed gathering of nanocrystal forms.
Embodiment 4
Take by weighing the high iron(ic) chloride of 1.351g, 0.446g zinc nitrate hexahydrate, 0.290g zinc nitrate hexahydrate, add three-necked flask, add 50ml ethylene glycol again, ultra-sonic dispersion 50min.After treating ultra-sonic dispersion, add 3.6g anhydrous sodium acetate, 0.5ml cetomacrogol 1000 again, be 500 rev/mins of following mechanical stirring 45min, after treating to dissolve fully, more above-mentioned solution is poured in the reactor, be warming up to 200 ℃, reaction 12h at revolution.Reaction finishes, collect product with magnet, and use the deionized water wash product, then with product at 60 ℃ of following vacuum-drying 20h, obtain Ni xZn 1-xFe 2O 4Nano-powder.The XRD test result shows: this nano-powder is Ni xZn 1-xFe 2O 4Transmission electron microscope observing shows Ni xZn 1-xFe 2O 4The Nano microsphere particle diameter is at 50～150nm, the Ni in this nano-powder xZn 1-xFe 2O 4Nano microsphere is that a plurality of Ni are arranged xZn 1-xFe 2O 4The directed gathering of nanocrystal forms.The magnetic hysteresis loop figure of this magnetic nano powder shows: the specific magnetising moment of this nano-powder is higher, reaches 53.06emu/g.

Claims (5)

1. the hot legal system of alcohol is equipped with nickel-zinc ferrite Ni xZn 1-xFe 2O 4The method of magnetic nano powder comprises:
Under the room temperature, taking by weighing the concentration that molysite, zinc salt, nickel salt be dissolved in for reactor volume 1/2～3/4 is in the ethylene glycol of 98～99.5wt%, wherein Zn 2+And Ni 2+Mole ratio be 1:4～4:1; Zn 2+And Ni 2+Mole number sum and Fe 3+The ratio of mole number be 1:2, ultra-sonic dispersion 30～60min adds respectively and Fe again 3+The ratio of mole number be: the anhydrous sodium acetate of 8:1～12:1,1/50～1/25 polyoxyethylene glycol dispersion agent for the ethylene glycol volume, mechanical stirring 20～60min, rotating speed is 500～800 rev/mins, after treating to dissolve fully mixture is put into reactor, be warming up to 180～220 ℃, reaction 9～12h after the complete reaction, is cooled to room temperature, collect product, deionized water wash product with magnet, 40～80 ℃, 15～24h oven dry obtain Ni xZn 1-xFe 2O 4Magnetic nano powder.
2. the hot legal system of a kind of alcohol according to claim 1 is equipped with nickel-zinc ferrite Ni xZn 1-xFe 2O 4The method of magnetic nano powder is characterized in that: described molysite, zinc salt, nickel salt are iron, nickel, the muriate of zinc, nitrate, the vitriol of solubility.
3. the hot legal system of a kind of alcohol according to claim 2 is equipped with nickel-zinc ferrite Ni xZn 1-xFe 2O 4The method of magnetic nano powder is characterized in that: described molysite, zinc salt, nickel salt are the muriate FeCl of iron 36H 2Nitrate Ni (the NO of O, nickel 3) 2H 2Nitrate Zn (the NO of O, zinc 3) 26H 2O.
4. the hot legal system of a kind of alcohol according to claim 1 is equipped with nickel-zinc ferrite Ni xZn 1-xFe 2O 4The method of magnetic nano powder is characterized in that: the molecular weight of described polyoxyethylene glycol dispersion agent is 200～1000.
5. the hot legal system of a kind of alcohol according to claim 2 is equipped with nickel-zinc ferrite Ni xZn 1-xFe 2O 4The method of magnetic nano powder is characterized in that: by regulating the ratio of described molysite, zinc salt, nickel salt, can obtain the different Ni that form xZn 1-xFe 2O 4Magnetic nano powder.
CNA2009100451236A 2009-01-09 2009-01-09 Process for preparing nickel-zine ferrite (NixZn1-xFe2O4) magnetic nano powder by alcohol-heating method Pending CN101475368A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503390A (en) * 2011-10-20 2012-06-20 同济大学 Preparation method of manganese-zinc ferrite magnetic nanoparticle
WO2013029200A1 (en) * 2011-08-29 2013-03-07 山西省电力公司 Method for preparing hollow ni-zn ferrite microsphere
CN103065751A (en) * 2011-10-19 2013-04-24 中国科学院宁波材料技术与工程研究所 Magnetic MFe2O4/C/M' compound and preparation method thereof using aniline small organic molecules as a carbon source
CN105958032A (en) * 2016-07-04 2016-09-21 吉林大学 Method for improving electrochemical performance of zinc ferrite by doping nickel element and application
CN106365205A (en) * 2016-08-18 2017-02-01 河北工业大学 Preparation method of manganese zinc ferrite nano-powder
CN112375541A (en) * 2020-10-13 2021-02-19 安徽理工大学环境友好材料与职业健康研究院(芜湖) Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof
CN115403366A (en) * 2022-08-24 2022-11-29 厦门大学 Lithium-doped nickel-zinc ferrite material and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013029200A1 (en) * 2011-08-29 2013-03-07 山西省电力公司 Method for preparing hollow ni-zn ferrite microsphere
CN103065751A (en) * 2011-10-19 2013-04-24 中国科学院宁波材料技术与工程研究所 Magnetic MFe2O4/C/M' compound and preparation method thereof using aniline small organic molecules as a carbon source
CN103065751B (en) * 2011-10-19 2016-08-10 中国科学院宁波材料技术与工程研究所 A kind of preparation method based on the magnetic MFe2O4/C/M ' that phenyl amines organic molecule is carbon source
CN102503390A (en) * 2011-10-20 2012-06-20 同济大学 Preparation method of manganese-zinc ferrite magnetic nanoparticle
CN105958032A (en) * 2016-07-04 2016-09-21 吉林大学 Method for improving electrochemical performance of zinc ferrite by doping nickel element and application
CN105958032B (en) * 2016-07-04 2018-12-11 吉林大学 A kind of method and application improving zinc ferrite chemical property by doping nickel element
CN106365205A (en) * 2016-08-18 2017-02-01 河北工业大学 Preparation method of manganese zinc ferrite nano-powder
CN112375541A (en) * 2020-10-13 2021-02-19 安徽理工大学环境友好材料与职业健康研究院(芜湖) Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof
CN112375541B (en) * 2020-10-13 2023-06-23 安徽理工大学环境友好材料与职业健康研究院(芜湖) Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof
CN115403366A (en) * 2022-08-24 2022-11-29 厦门大学 Lithium-doped nickel-zinc ferrite material and preparation method thereof

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