CN103771538A - Low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder - Google Patents

Low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder Download PDF

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CN103771538A
CN103771538A CN201410039357.0A CN201410039357A CN103771538A CN 103771538 A CN103771538 A CN 103771538A CN 201410039357 A CN201410039357 A CN 201410039357A CN 103771538 A CN103771538 A CN 103771538A
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nano
reaction preparation
powder
low
solid state
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CN103771538B (en
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籍凤秋
王冰冰
郝相雨
李佑均
于刚
王彩辉
赵娇娇
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HEBEI YIBAI READY MIXED CONCRETE Co Ltd
Shijiazhuang Tiedao University
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HEBEI YIBAI READY MIXED CONCRETE Co Ltd
Shijiazhuang Tiedao University
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Abstract

The invention discloses a low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder, and belongs to the technical field of the preparation process of magnetic nano materials. The low-temperature solid-phase reaction preparation method comprises the following steps of: adopting cobalt nitrate, ferric nitrate and sodium hydroxide as reactants, adopting polyvinyl alcohol as a dispersing agent, mixing according to the proportion, carrying out ball milling to be viscous and obtaining a CoFe2O4 precursor; washing, filtering and drying the precursor, then grinding to be powdery, carrying out constant-temperature calcining under the condition of 600 DEG C, cooling and taking out to prepare the nano CoFe2O4 powder. The low-temperature solid-phase reaction preparation method disclosed by the invention has the advantages that the nano powder aggregation is light; based on a low-temperature solid-phase synthesis method, the preparation condition is mild, a solvent is not needed, the pollution is avoided, the operation is simple, and the cost is low; and the low-temperature solid-phase reaction preparation method is a green nano-powder preparation technology and is easy to realize batch production.

Description

A kind of nano Co Fe 2o 4body hypothermia solid state reaction preparation method
Technical field
The invention belongs to magnetic Nano material fabricating technology field.
Background technology
Nanometer ferro-cobalt oxygen (CoFe2O4) body has spinel crystal structure, can be used as a kind of important microwave absorption and uses.In addition, Nanometer Cobalt Ferrite Oxide is the magnetoopticmemory material that has potentiality, aspect medical field, environmental treatment, is being with a wide range of applications.Its outstanding advantages is that saturation magnetization is higher, and magnetocrystalline anisotropy constant is larger, chemical stability, wear-resistant good corrosion resistance.At present, the synthetic main wet chemistry method that adopts of Nanometer Cobalt Ferrite Oxide, as chemical coprecipitation, sol-gel processing, microemulsion method, hydrothermal method etc., but reaction conditions is larger on the impact of resultant of reaction particle diameter, has comparatively serious agglomeration simultaneously.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of nano Co Fe2O 4body hypothermia solid state reaction preparation method, between nano-powder, agglomeration is light, preparation condition gentleness, have energy-conservation, do not need solvent, pollution-free, with short production cycle, productivity is high, simple to operate, be easy to the advantages such as batch production.。
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of nano Co Fe 2o 4the preparation method of powder, reaction principle is:
Figure 2014100393570100002DEST_PATH_IMAGE002
A kind of nano Co Fe 2o 4body hypothermia solid state reaction preparation method, take Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate and sodium hydroxide as raw material, in molar ratio for the stoichiometric ratio of 1:2:8-10 takes after described raw material mixing, then add polyvinyl alcohol as dispersion agent, once be ground to thickly, after having reacted, obtain CoFe 2o 4presoma; By described CoFe 2o 4presoma through washing, filter, dry, carry out regrind and become after powder shape, calcining at constant temperature 2-4h at 600 ℃, obtains nano Co Fe after cooling 2o 4body.
Described Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is Co (NO 3) 26H 2o, purity is>=99.0%; Described iron nitrate is Fe (NO 3) 39H 2o, purity is>=98.5%; The purity of described polyvinyl alcohol is>=85%.
Preferably, the mol ratio of described Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate, sodium hydroxide material is: 1:2:8.8.
The mol ratio of described polyvinyl alcohol and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 0.25-1:1.
The described employing ball mill grinding that once grinds, milling time is about 30-70 min, and the mass ratio of material and abrading-ball is 1:1.2-1.8.
Described CoFe 2o 4it is deionized water and dehydrated alcohol that presoma washs washings used; Described washing and filtration step hocket; First use deionized water wash presoma, until filtrate is neutral, and then wash for 2-3 time with dehydrated alcohol; Described filtration procedure adopts suction filtration mode to carry out;
Described CoFe 2o 4presoma dry is natural air drying at normal temperatures; Described regrind adopts hand lapping or ball mill grinding;
Described CoFe2O 4the calcination process of presoma carries out in resistance furnace under oxygen atmosphere, and temperature increasing schedule is 1-3 ℃/min.
The beneficial effect that adopts technique scheme to produce is: the present invention adopts polyvinyl alcohol as dispersion agent, and between nano-powder, agglomeration is light; Based on Low Temperature Solid-Phase synthesis method, preparation condition gentleness, does not need solvent, pollution-free, and the reaction times is short, with short production cycle, productivity is high, purity is high, simple to operate, cost is low, be easy to the advantages such as batch production, is a kind of Preen nono Preparation Technique of Powders.
Accompanying drawing explanation
Fig. 1 is the CoFe preparing in the embodiment of the present invention 1 2o 4the X ray diffracting spectrum of powder;
Fig. 2 is the CoFe preparing in the embodiment of the present invention 1 2o 4the SEM photo of powder, magnification is 60000 times;
Fig. 3 is the CoFe preparing in the embodiment of the present invention 2 2o 4the X ray diffracting spectrum of powder;
Fig. 4 is the CoFe preparing in the embodiment of the present invention 2 2o 4the SEM photo of powder, magnification is 60000 times;
Fig. 5 is the CoFe preparing in the embodiment of the present invention 3 2o 4the X ray diffracting spectrum of powder;
Fig. 6 is the CoFe preparing in the embodiment of the present invention 3 2o 4the SEM photo of powder, magnification is 60000 times.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
Weigh respectively the Co (NO of 29.10 g 3) 26H 2o(purity>=99.0%), the Fe (NO of 80.80 g 3) 39H 2o(purity>=98.5%) and the NaOH of 35.20 g and the polyvinyl alcohol (purity>=85%) of 4.40 g, be placed in ceramic pot and mix, adopt ball mill ball milling 60min, obtain CoFe 2o 4presoma.By CoFe 2o 4deionized water repetitive scrubbing for presoma, suction filtration are until after filtrate is neutrality, with absolute ethanol washing 2 times, by the sedimentable matter natural air drying having filtered, hand lapping becomes after powder shape, be placed in ceramic crucible, move in chamber type electric resistance furnace and is warmed up to 600 ℃ with the temperature increasing schedule of 2 ℃/min under oxygen atmosphere, calcining at constant temperature 3 h, obtain the powder of black.Characterize the structure of powder by X-ray diffraction (XRD) method, logical scanning electron microscope (SEM) method is observed the pattern of powder, and measuring result as depicted in figs. 1 and 2.Result shows: the strong peak of spinel master (311) and time strong peak (440) are very sharp-pointed, and peak width is narrow, peak is powerful, illustrates that the powder of preparation is pure spinel type nanometer CoFe 2o 4; Morphology microstructure pattern presents cellular, between particle, reunites, and particle diameter is 50 ~ 80 nm.
Embodiment 2
Be that with the difference of embodiment 1 adding the quality of polyvinyl alcohol is 2.20 g.The same structure that characterizes powder with X-ray diffraction method (XRD), logical scanning electron microscope (SEM) is observed the pattern of powder, and measuring result is as shown in Figure 3 and Figure 4.Result shows: the powder of preparation is pure spinel type nanometer CoFe 2o 4; Morphology microstructure is spherical, and slight reunion occurs between particle, and particle diameter is about 60 nm.
Embodiment 3:
Being to add polyvinyl alcohol quality with the difference of embodiment 1 is 1.10 g.The same structure that characterizes powder with X-ray diffraction method (XRD), logical scanning electron microscope (SEM) is observed the pattern of powder, and measuring result is as shown in Figure 5 and Figure 6.Result shows: the powder of preparation is pure spinel type nanometer CoFe 2o 4; Morphology microstructure is spherical, and particle is without obvious reunion, and particle diameter is 30 ~ 40 nm.

Claims (8)

1. a nano Co Fe 2o 4body hypothermia solid state reaction preparation method, it is characterized in that: take Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate and sodium hydroxide as raw material, in molar ratio for the stoichiometric ratio of 1:2:8-10 takes after described raw material mixing, then add polyvinyl alcohol as dispersion agent, once be ground to thickly, after having reacted, obtain CoFe 2o 4presoma; By described CoFe 2o 4presoma through washing, filter, dry, carry out regrind and become after powder shape, calcining at constant temperature 2-4h at 600 ℃, obtains nano Co Fe after cooling 2o 4body.
2. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: described Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is Co (NO 3) 26H 2o, purity is>=99.0%; Described iron nitrate is Fe (NO 3) 39H 2o, purity is>=98.5%; The purity of described polyvinyl alcohol is>=85%.
3. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: the mol ratio of described Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate, sodium hydroxide material is: 1:2:8.8.
4. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: the mol ratio of described polyvinyl alcohol and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 0.25-1:1.
5. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: the described employing ball mill grinding that once grinds, and milling time is about 30-70 min, and the mass ratio of material and abrading-ball is 1:1.2-1.8.
6. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: described CoFe 2o 4it is deionized water and dehydrated alcohol that presoma washs washings used; Described washing and filtration step hocket; First use deionized water wash presoma, until filtrate is neutral, and then wash for 2-3 time with dehydrated alcohol; Described filtration procedure adopts suction filtration mode to carry out.
7. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: described CoFe 2o 4presoma dry is natural air drying at normal temperatures; Described regrind adopts hand lapping or ball mill grinding.
8. nano Co Fe according to claim 1 2o 4body hypothermia solid state reaction preparation method, is characterized in that: described CoFe 2o 4the calcination process of presoma carries out in resistance furnace, and temperature increasing schedule is 1-3 ℃/min.
CN201410039357.0A 2014-01-27 2014-01-27 Low-temperature solid-phase reaction preparation method of nano CoFe2O4 powder Expired - Fee Related CN103771538B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555042A (en) * 2009-05-19 2009-10-14 李峰 Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction
CN102276246A (en) * 2011-07-20 2011-12-14 盐城工学院 Method for preparing cobalt ferrite nanometer granules by mechanical force chemical method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555042A (en) * 2009-05-19 2009-10-14 李峰 Method for preparing spinel type iron-containing oxide nano-materials by low heat solid state reaction
CN102276246A (en) * 2011-07-20 2011-12-14 盐城工学院 Method for preparing cobalt ferrite nanometer granules by mechanical force chemical method

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
杨翠: ""低温固相法制备金属纳米氧化物"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *
秦润华等: ""尖晶石型(Zn1-δFeδ)[CoδFe2-δ]O4铁氧体纳米粒子的制备与磁性研究"", 《功能材料》 *
陈亮等: ""固相法合成锌铁氧体及其光催化性能"", 《西南科技大学学报》 *
黄磊等: ""低温固相反应法制备CoFe2O4纳米颗粒"", 《甘肃科学学报》 *

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