CN103204546B - Method for preparing nano cobalt ferrite - Google Patents
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- CN103204546B CN103204546B CN201310133530.9A CN201310133530A CN103204546B CN 103204546 B CN103204546 B CN 103204546B CN 201310133530 A CN201310133530 A CN 201310133530A CN 103204546 B CN103204546 B CN 103204546B
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 22
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 20
- 239000010941 cobalt Substances 0.000 title claims abstract description 20
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000000243 solution Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 14
- 239000011029 spinel Substances 0.000 claims abstract description 14
- 229910003321 CoFe Inorganic materials 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract 6
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 11
- 229910002518 CoFe2O4 Inorganic materials 0.000 abstract description 8
- 238000001556 precipitation Methods 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 30
- 230000005291 magnetic effect Effects 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000000975 co-precipitation Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 235000011194 food seasoning agent Nutrition 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 238000000593 microemulsion method Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 2
- 150000001868 cobalt Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011554 ferrofluid Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
本发明公开一种可在较低的温度下制备尖晶石结构的纳米钴铁氧体CoFe2O4的纳米粉体方法。本发明的尖晶石结构纳米钴铁氧体CoFe2O4的制备方法是：按比例称取三氯化铁与二氯化钴后混合配制成水溶液A，配制的NaOH或者KOH碱溶液，搅拌均匀后向其中滴加N2H4.H2O，以得到溶液B；在20~40℃下快速搅拌步骤1所获得的水溶液A，并将步骤2）所配制的混合溶液B缓慢滴加到水溶液A中反应，得到黑色尖晶石结构的钴铁氧体CoFe2O4粉末沉淀。The invention discloses a nano-powder method capable of preparing spinel-structured nano-cobalt ferrite CoFe2O4 at relatively low temperature . The preparation method of spinel structure nano-cobalt ferrite CoFe 2 O 4 of the present invention is: take ferric trichloride and cobalt dichloride in proportion, mix and prepare aqueous solution A, prepare NaOH or KOH alkali solution, stir After uniformity, add N 2 H 4 .H 2 O to it dropwise to obtain solution B; quickly stir the aqueous solution A obtained in step 1 at 20~40°C, and slowly add the mixed solution B prepared in step 2) dropwise React in aqueous solution A to obtain cobalt ferrite CoFe 2 O 4 powder precipitation with black spinel structure.
Description
Technical field
The present invention relates to a kind of preparation method's of Nanometer Cobalt Ferrite Oxide powder, particularly a kind of spinel structure Nanometer Cobalt Ferrite Oxide CoFe
2o
4preparation method.
Background technology
The vectolite of spinel type is a kind of magneticsubstance of excellent property, has high saturation magnetization, the outstanding plurality of advantages such as corrosion resistance nature and abrasion resistance properties.Its aspect magnetic recording, magnetics and magnetic fluid aspect be widely used.In addition because its high resistivity and significant Kerr magnetooptical effect make it have great application potential aspect absorbing material and New Type Magneto recording materials.Referring to: [1] " vectolite preparation and research thereof ", Zhang Chao, He'nan University's master thesis; [2] chemical method preparation technology and the absorbing property thereof of vectolite micro mist, Che Renchao, Li Yongqing etc., " aerospace material technique ",, the 6th phase in 1999; [3] Synthesis and characterization of size-controlled cobalt-ferrite-based ionic ferrofluids, Journal of Magnetism and Magnetic Materials, 225 (2001) 37-40.
At present, the preparation method of cobalt ferrite powder mainly contains sol-gel method, microemulsion method, solid reaction process and coprecipitation method etc., the people such as Lee J G synthesize Nanometer Cobalt Ferrite Oxide with sol-gel method, after 500 DEG C of calcinings of the method, prepared vectolite nanoparticle mean sizes is about 30nm, referring to: Lee J G, Kim C S, Lee H M, et a1. Magnetic properties of CoFe2O4 powers and thin films by a sol-gel method [J]. J Magn Mater, 1998,177 (2): 900-902..T. the people such as Pannaparayil has prepared vectolite between 135 ~ 175 DEG C by hydrothermal method, particle size is at 100 ~ 300nm, referring to: T. Pannaparayil and S. Komarneni, SYNTHESIS AND CHARACTERIZATION OF ULTRAFINE COBALT FERRITES, IEEE TRANSACTIONS ON MAGNETICS, VOL. 25, NO. 5, SEPTEMBER 1989,4233-4235.N. the people such as Moumen has prepared the vectolite particle of size at 2 ~ 5nm with microemulsion method, referring to: N. Moumen and M. P. Pileni, New Syntheses of Cobalt Ferrite Particles in the Range 25 nm:Comparison of the Magnetic Properties of the Nanosized Particles in Dispersed Fluid or in Powder Form, Chem. Mater., 1996,8 (5), pp 1128 – 1134.In preceding method, solid reaction process and sol-gel method all need the calcination process of comparatively high temps, referring to Chinese patent application 200410018797.8(publication number: CN101168452A) and Chinese patent application 201010045635.5(publication number: CN 101786668 A); The temperature of reaction of hydrothermal method is higher; Granule-morphology and size prepared by microemulsion method are better, but complex process, productive rate are low, and have residual organic matter.Coprecipitation method is a kind of relatively simple method of technique, but general coprecipitation method also need to just can be converted at boiling water or more than 60 DEG C spinel structure vectolite [3 under temperature condition, 9] referring to Synthesis and characterization of size-controlled cobalt-ferrite-based ionic ferrofluids, Journal of Magnetism and Magnetic Materials, 225 (2001) 37-40 and Chinese patent application 200510018262.1(publication number: CN1657490A).Yeong Il Kim etc. directly prepare vectolite with NaOH precipitation molysite and cobalt salt solution, and by controlling reaction temperature particle size, but at 60 DEG C, what obtain below is amorphous particle instead of ferrospinel, referring to: Yeong Il Kim, Don Kim, Choong Su Lee, Synthesis and characterization of CoFe2O4 magnetic nanoparticles prepared by temperature-controlled coprecipitation method, PhysicaB337 (2003) 42 – 51.The people such as M.Rajendran have provided a kind of method of preparing vectolite with NaOH and H2O2 mixing solutions co-precipitation molysite and cobalt salt solution, but the crystallization in the time of 20 DEG C of this method is poor, referring to M.Rajendran, R.C.Pullar, A.K.Bhattacharya, D.Das S.N.Chintalapudi, C.K.Majumdar, Magnetic properties of nanocrystalline CoFe2O4 powders prepared at room temperature:variation with crystallitesize, Journal of Magnetism and Magnetic Materials, 232 (2001), 71 – 83.
Summary of the invention
The invention provides one and can overcome prior art deficiency, can at lower temperature, prepare the method for cobalt ferrite powder with coprecipitation method.
The spinel structure Nanometer Cobalt Ferrite Oxide CoFe for preparing of the present invention
2o
4method be:
1) be hybridly prepared into water solution A after taking in proportion iron trichloride and cobalt dichloride;
2) preparation NaOH or KOH alkaline solution, drip N wherein after stirring
2h
4.H
2o, to obtain solution B;
3) water solution A that rapid stirring step 1 obtains at 20 ~ 40 DEG C, and by step 2) the mixing solutions B for preparing is slowly added drop-wise in water solution A and reacts, and obtains black precipitate;
4) chocolate precipitation distilled water step 3) reaction being produced fully wash to pH value be 7, then use washing with alcohol, then drying treatment obtains the vectolite CoFe of spinel structure
2o
4powder.
In the embodiment that the present invention provides, prepare spinel structure Nanometer Cobalt Ferrite Oxide CoFe
2o
4the iron trichloride of Shi Suoyong is FeCl
3.6H
2o, cobalt dichloride used is CoCl
2.6H
2o, FeCl when preparation A solution
3.6H
2o and CoCl
2.6H
2the mol ratio of O is 2: 1, and the NaOH of preparation or KOH alkaline concentration are 1.5 ~ 2.5 mol/L, and in the solution B of preparation, the concentration of hydrazine hydrate is 4 ~ 7mol/L.
In solution A in the embodiment of the present invention, concentration of metal ions is 0.01M ~ 0.05M.
Method of the present invention can (between 20 DEG C to 40 DEG C) be prepared vectolite CoFe at lower temperature
2o
4nanometer powder, and the particle crystallization obtaining is better, and transmission electron microscope (TEM) photo shows that particle mean size is 3 ~ 9nm, and the grain-size of calculating with X-ray diffraction spectrum meets, and is single crystal particle.Vibrating sample magnetometer (VSM) test shows that particle is at room temperature superparamagnetism, and under 1.2 T foreign fields, the specific magnetising moment is 11 ~ 40 emu/g.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrum of embodiment 1 product and embodiment 2 products.
Fig. 2 is TEM photo and the selected area electron diffraction figure (SAED) of embodiment 1 product.
Fig. 3 is TEM photo and the selected area electron diffraction figure (SAED) of embodiment 2 products.
Fig. 4 is embodiment 1 magnetic hysteresis loop that for product, vibrating sample magnetometer (VSM) is measured.
Fig. 5 is embodiment 2 magnetic hysteresis loop that for product, vibrating sample magnetometer (VSM) is measured.
Embodiment
The invention provides following specific embodiment.
1) take 0.1784g(0.00066mol with mol ratio 2:1) FeCl
3.6H
2o and 0.07815g(0.00033mol) CoCl
2.6H
2o, is dissolved in 50ml distilled water, fully stirring and dissolving, and concentration of metal ions is 0.02M.
2) taking 1.6g(0.04mol) NaOH is dissolved in 20ml distilled water, and NaOH concentration is 2M.After stirring, drip wherein N
2h
4.H
2o(85% hydrazine hydrate)
10ml, N
2h
4.H
2o concentration is 5.6mol/L.
3) exist
room temperatureunder (20
oc) rapid stirring under condition, by step 2) alkali configuring and the mixing solutions of hydrazine hydrate be slowly added drop-wise in the solution of Fe, Co salt, react 2 hours.
4) black precipitate step 3) reaction being produced is fully washed to pH value 7 left and right with distilled water, then uses washing with alcohol 2 ~ 3 times, and then seasoning or vacuum-drying, obtains CoFe2O4 particle.
In accompanying drawing 1, the X-ray diffraction of this routine gained sample spectrum shows the spinel nano crystal structure that crystal grain is, the grain-size of being calculated by diffraction peak is 3 nm left and right, shows that with the TEM photo of Fig. 2 particle size is consistent, is single crystal particle.In Fig. 1, in X-ray diffraction spectrum and Fig. 2, SAED figure all shows particle well-crystallized.Fig. 4 for this reason routine sample at room temperature uses the measured magnetic hysteresis loop of VSM, under result show sample ability room temperature, is superparamagnetism, and the specific magnetising moment under 1.2 T foreign fields is 17 emu/g.
Embodiment 2.
1) take 0.1784g(0.00066mol with mol ratio 2:1) FeCl
3.6H
2o and 0.07815g(0.00033mol) CoCl
2.6H
2o, is dissolved in 50ml distilled water, fully stirring and dissolving, and concentration of metal ions is 0.02M.
2) taking 1.6g(0.04mol) NaOH is dissolved in 20ml distilled water, and NaOH concentration is 2M.After stirring, drip wherein N
2h
4.H
2o(85% hydrazine hydrate)
10ml, N
2h
4.H
2o concentration is 5.6mol/L.
3) exist
40 o crapid stirring under water bath condition, by step 2) alkali configuring and the mixing solutions of hydrazine hydrate be slowly added drop-wise in the solution of Fe, Co salt, react 2 hours.
4) black precipitate step 3) reaction being produced is fully washed to pH value 7 left and right with distilled water, then uses washing with alcohol 2 ~ 3 times, and then seasoning or vacuum-drying, obtains CoFe2O4 particle.Average particle size particle size is 9nm, is superparamagnetism under room temperature, 1.2 T specific magnetising moment 40emu/g after the match outward.
In accompanying drawing 1, the X-ray diffraction of this routine gained sample spectrum shows the spinel nano crystal structure that crystal grain is, the particle size of being calculated by diffraction peak is 9 nm left and right, shows that with the TEM photo of Fig. 3 particle size is consistent, is single crystal particle.In Fig. 1, in X-ray diffraction spectrum and Fig. 3, SAED figure all shows particle well-crystallized, and TEM photo shows that particle dispersion is good.Fig. 5 for this reason routine sample at room temperature uses the measured magnetic hysteresis loop of VSM, under result show sample ability room temperature, is superparamagnetism, and the specific magnetising moment under 1.2 T foreign fields is 40 emu/g.
Embodiment 3.
1) take 0.1784g(0.00066mol with mol ratio 2:1) FeCl
3.6H
2o and 0.07815g(0.00033mol) CoCl
2.6H
2o, is dissolved in 50ml distilled water, fully stirring and dissolving, and concentration of metal ions is 0.02M.
2) take
1.2g(0.03mol) NaOH is dissolved in 20ml distilled water, and NaOH concentration is 1.5M.After stirring, drip wherein N
2h
4.H
2o(85% hydrazine hydrate) 14ml, N
2h
4.H
2o concentration is 7mol/L.
3) exist
20 o crapid stirring under water bath condition, by step 2) alkali configuring and the mixing solutions of hydrazine hydrate be slowly added drop-wise in the solution of Fe, Co salt, react 3 hours.
4) black precipitate step 3) reaction being produced is fully washed to pH value 7 left and right with distilled water, then uses washing with alcohol 2 ~ 3 times, and then seasoning or vacuum-drying, obtains CoFe2O4 particle.Average particle size particle size is 3nm, is superparamagnetism under room temperature, 1.2 T specific magnetising moment 11emu/g after the match outward.
Embodiment 4.
1) take 0.1784g(0.00066mol with mol ratio 2:1) FeCl
3.6H
2o and 0.07815g(0.00033mol) CoCl
2.6H
2o, is dissolved in 50ml distilled water, fully stirring and dissolving, and concentration of metal ions is 0.02M.
2) take
2g(0.05mol) NaOH is dissolved in 20ml distilled water, and NaOH concentration is 2.5M.After stirring, drip wherein N
2h
4.H
2o(85% hydrazine hydrate)
6ml, N
2h
4.H
2o concentration is 3.8mol/L.
3) exist
20 o crapid stirring under water bath condition, by step 2) alkali configuring and the mixing solutions of hydrazine hydrate be slowly added drop-wise in the solution of Fe, Co salt, react 3 hours.
4) black precipitate step 3) reaction being produced is fully washed to pH value 7 left and right with distilled water, then uses washing with alcohol 2 ~ 3 times, and then seasoning or vacuum-drying, obtains CoFe2O4 particle.Average particle size particle size is 5nm, is superparamagnetism under room temperature, the 1.2 T specific magnetising moment 13 emu/g after the match outward.
Above-described embodiment shows, method provided by the invention can at room temperature be prepared the good spinel structure Nanocrystalline Cobalt of crystallization ferrite, and particle size is below 10 nanometers, and particle dispersion is good.This method technique is simple, and cost is lower, for preparation and the application of Nanometer Cobalt Ferrite Oxide powder provide a kind of valuable selection.
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| CN105129868B (en) * | 2015-07-16 | 2017-01-04 | 大连理工大学 | A method for preparing Cr3+ doped CoFe2O4 high-density magnetic recording material |
| CN107633946A (en) * | 2017-09-25 | 2018-01-26 | 常州市沃兰特电子有限公司 | A kind of preparation method of nanometer of magnet |
| CN109943285B (en) * | 2019-04-16 | 2021-09-17 | 贵州大学 | High-performance wave-absorbing material core-shell structure CoxFe3-xO4@MoS2Nano-composite and synthesis method thereof |
| CN110305364A (en) * | 2019-07-30 | 2019-10-08 | 济南大学 | A kind of preparation method of novel magnetic polyvinyl formal sponge |
| CN112588256A (en) * | 2021-01-28 | 2021-04-02 | 华东交通大学 | A kind of magnetic nanometer double metal oxide adsorbent and its application |
| CN112851326A (en) * | 2021-01-29 | 2021-05-28 | 兰州大学 | Co2Z-type ferrite material and preparation method thereof |
| CN113200572A (en) * | 2021-05-07 | 2021-08-03 | 景德镇陶瓷大学 | Process method for preparing cobalt ferrite powder at low temperature in dry state |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0555056A2 (en) * | 1992-02-05 | 1993-08-11 | Toda Kogyo Corp. | Magnetic iron oxide particles, a process for producing the same and a magnetic recording medium |
| CN102190483A (en) * | 2010-03-01 | 2011-09-21 | 中国科学院生态环境研究中心 | A three-dimensional micro-nano material composed of nano-CoFe2O4 and its preparation method |
| CN102923785A (en) * | 2012-11-19 | 2013-02-13 | 兰州理工大学 | Preparation method of CoFe2O4 magnetic nanometer material |
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2013
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0555056A2 (en) * | 1992-02-05 | 1993-08-11 | Toda Kogyo Corp. | Magnetic iron oxide particles, a process for producing the same and a magnetic recording medium |
| CN102190483A (en) * | 2010-03-01 | 2011-09-21 | 中国科学院生态环境研究中心 | A three-dimensional micro-nano material composed of nano-CoFe2O4 and its preparation method |
| CN102923785A (en) * | 2012-11-19 | 2013-02-13 | 兰州理工大学 | Preparation method of CoFe2O4 magnetic nanometer material |
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