CN102923785A - Preparation method of CoFe2O4 magnetic nano material - Google Patents
Preparation method of CoFe2O4 magnetic nano material Download PDFInfo
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- CN102923785A CN102923785A CN2012104642234A CN201210464223A CN102923785A CN 102923785 A CN102923785 A CN 102923785A CN 2012104642234 A CN2012104642234 A CN 2012104642234A CN 201210464223 A CN201210464223 A CN 201210464223A CN 102923785 A CN102923785 A CN 102923785A
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Abstract
The invention provides a preparation method of a CoFe2O4 magnetic material. The preparation method comprises steps as follows: preparing a certain amount of ferric nitrate Fe(NO3)3.9H2O and a certain amount of cobalt nitrate Co(NO3)2.6H2O into a mixed solution; slowly adding to a NaOH solution with a certain concentration at a certain temperature; then agitating the reaction solution under reinforcement; maintaining the reaction temperature for a period of time; then filtering and washing until the filtrate is neutral; drying the product; grinding to obtain black brown precursors; and thermally processing the precursors for 1 hour at a certain temperature, so as to obtain the CoFe2O4 magnetic nano material.
Description
Technical field
The present invention relates to the preparation method of magnetic Nano material.
Background technology
Vectolite (CoFe
2O
4) be a kind of traditional spinel type ferrimagnetism compound, ferrite similar with other compared CoFe
2O
4Have higher coercive force, magnetocrystalline anisotropy constant and Curie temperature, moderate saturation magnetization, high resistivity, well chemical stability and the higher characteristics such as physical strength.These excellent performances are being with a wide range of applications it aspect permanent magnet, magnetic recording and the magnetic fluid.At present, synthetic CoFe
2O
4The method of nano material is a lot, and such as conventional ceramic technique, chemical coprecipitation, sol-gel method, microemulsion method etc., wherein to have an experiment condition simple for chemical coprecipitation, and reactant activity is high, the advantages such as fine size.
Prepare CoFe in coprecipitation method
2O
4In the research of particle, usually adopt the forward coprecipitation method, but the particle size that the method generates is inhomogeneous.And reverse coprecipitation method and forward chemical coprecipitation are different, the former has changed the adding mode of precipitation agent, being about to reactant solution is added dropwise in the precipitant solution, so just guarantee that precipitation agent is in excessive state always, thereby make the reactant complete reaction, be expected to obtain uniform particles, nanoparticle that particle diameter is less than the forward chemical coprecipitation.
Therefore, with the synthetic CoFe of reverse coprecipitation method
2O
4Magnetic Nano material, on the one hand the experimental implementation condition is simple, can obtain on the other hand uniform particles, nanoparticle that particle diameter is less, and presoma also is greatly improved through its saturation magnetization of Overheating Treatment and thermostability.
Chinese patent Zl200810064717.7 has reported a kind of preparation method of flower-shaped spinelle cobalt ferrite powder.This patent is taked the forward coprecipitation method, and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and iron nitrate are dissolved in the oxalic acid solution, regulates the pH value by sodium hydroxide, heats and stir 2 ~ 3h to obtain presoma in water-bath; It is used alcohol and distilled water wash for several times successively; Fine powder is dried and worn into to presoma, and 800 ℃ of lower calcining 6h obtain flower-shaped spinelle cobalt ferrite powder, but there is following distinct disadvantage in this patent:
(1) ageing reaction times and calcination time are respectively 2 ~ 3h and 6h in this patent, and be long to the reactant heat treatment time, causes the wasting of resources.
(2) owing to adopting a large amount of unsaturated organic acid solution in this patent, will produce a large amount of organic liquid wastes after the reaction, environment will be caused severe contamination.
Summary of the invention
The purpose of this invention is to provide a kind ofCoFe
2O
4The preparation method of magnetic Nano material.
The present invention is CoFe
2O
4The preparation method of magnetic Nano material the steps include:
(1) take by weighing iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and be added to the water and be mixed with mixing solutions, the mol ratio of iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 2:1;
(2) weighing sodium hydroxide is added to the water and is mixed with solution as precipitation agent again, is heated to 60 ~ 92 ℃, and the mol ratio of sodium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 9 ~ 16:1; The aqueous solution of precipitation agent or dimethylamine, the perhaps aqueous solution of triethylamine, the perhaps aqueous solution of potassium hydroxide, dimethylamine, triethylamine, the mol ratio of potassium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES consumption is 9 ~ 16:1;
(3) mixing solutions was at the uniform velocity joined in 30 minutes in the precipitation agent under the agitation condition, holding temperature, ageing reaction 30 ~ 120 minutes will precipitate filtering and washing to filtrate and be neutral, and the chocolate presoma is dried, ground to get to the product that obtains;
(4) with presoma 600 ~ 1000 ℃ of lower thermal treatment 1 hour in air ambient, namely get CoFe
2O
4Magnetic Nano material.
Usefulness of the present invention is: synthetic technological condition is gentle, and technical process is simple, and generated time is shorter; Product cost is lower; Synthetic used raw material and sintetics are all nontoxic; Synthetic CoFe
2O
4The magnetic Nano material saturation magnetization is high, can be used for the fields such as coating engineering building materials.
Description of drawings
Fig. 1 is the CoFe of embodiment 1
2O
4The XRD figure of magnetic Nano material spectrum, Fig. 2 is the transmission electron microscope photo of embodiment 1, Fig. 3, Fig. 4, Fig. 5, Fig. 6 are respectively embodiment 1,4,6,8 VSM figure.
Embodiment
The present invention is CoFe
2O
4The preparation method of magnetic Nano material the steps include:
(1) take by weighing iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and be added to the water and be mixed with mixing solutions, the mol ratio of iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 2:1;
(2) weighing sodium hydroxide is added to the water and is mixed with solution as precipitation agent again, is heated to 60 ~ 92 ℃, and the mol ratio of sodium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 9 ~ 16:1; The aqueous solution of precipitation agent or dimethylamine, the perhaps aqueous solution of triethylamine, the perhaps aqueous solution of potassium hydroxide, dimethylamine, triethylamine, the mol ratio of potassium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES consumption is 9 ~ 16:1;
(3) mixing solutions was at the uniform velocity joined in 30 minutes in the precipitation agent under the agitation condition, holding temperature, ageing reaction 30 ~ 120 minutes will precipitate filtering and washing to filtrate and be neutral, and the chocolate presoma is dried, ground to get to the product that obtains;
(4) with presoma 600 ~ 1000 ℃ of lower thermal treatment 1 hour in air ambient, namely get CoFe
2O
4Magnetic Nano material.
With the CoFe that obtains
2O
4Magnetic Nano material is by the agate mortar porphyrize, and the magnetic property by vibrating sample magnetometer (vibrating sample magnetometer) specimen can access CoFe
2O
4The saturation magnetization of magnetic Nano material and coercive force.
The present invention is described further below by 8 embodiment among 4 groups of different contrast experiments.
1. different precipitation agent consumptions:
| Title | Precipitation agent consumption/mol | Aging Temperature/℃ | Digestion time/min | Calcining temperature/℃ | Saturation magnetization/emu.g -1 | Coercive force/Oe |
| Embodiment 1 | 0.09 | 92 | 60 | 800 | 75.20 | 716 |
| Embodiment 2 | 0.16 | 92 | 60 | 800 | 72.00 | 620 |
Embodiment 1
Take by weighing 3.6051g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9086g Co (NO
3)
2.6H
20 with 8.0809gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
As shown in Figure 1, all characteristic peaks in the collection of illustrative plates: 2 θ=18.24 °, 30.06 °, 35.44 °, 43.10 °, 53.48 °, 57.02 °, 62.62 °, 74.06 ° with the JCPDS card in 22-1086(CoFe
2O
4) standard diagram matches, illustrate that all samples is the CoFe2O4 magnetic-particle of homogeneous, and have single spinel ferrite body structure.Utilize data in the collection of illustrative plates, according to Scherrer formula calculation sample grain-size, can draw, the average grain size of sample is 26.57nm.
As shown in Figure 2, this sample is nano particle, and mainly take sphere as main, grain diameter is about about 30nm microscopic appearance.Also have simultaneously the loose coacervate about some 60nm, this is because the powder grain-size is tiny, the table that it is strong and effect easily be agglomerated into some weak linkage interfaces than macro aggregate, to reduce its surface energy and magnetostatic energy.
Embodiment 2
Take by weighing 6.4016g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9114g Co (NO
3)
2.6H
20 with 8.0821gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
2. different Aging Temperatures:
| Title | Precipitation agent consumption/mol | Aging Temperature/℃ | Digestion time/min | Calcining temperature/℃ | Saturation magnetization/emu.g -1 | Coercive force/Oe |
| Embodiment 1 | 0.09 | 92 | 60 | 800 | 75.20 | 716 |
| |
0.09 | 75 | 60 | 800 | 71.00 | 720 |
| Embodiment 4 | 0.09 | 60 | 60 | 800 | 70.00 | 724 |
Take by weighing 3.6005g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 75 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9129g Co (NO
3)
2.6H
20 with 8.0806gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 75 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
Embodiment 4
Take by weighing 3.6116g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 60 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9107g Co (NO
3)
2.6H
20 with 8.0813gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 60 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
3. different ageing:
| Title | Precipitation agent consumption/mol | Aging Temperature/℃ | Digestion time/min | Calcining temperature/℃ | Saturation magnetization/emu.g -1 | Coercive force/Oe |
| Embodiment 1 | 0.09 | 92 | 60 | 800 | 75.20 | 716 |
| Embodiment 5 | 0.09 | 92 | 30 | 800 | 74.20 | 580 |
| Embodiment 6 | 0.09 | 92 | 120 | 800 | 75.18 | 592 |
Embodiment 5
Take by weighing 3.6025g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9101g Co (NO
3)
2.6H
20 with 8.0816gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 30min will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
Embodiment 6
Take by weighing 3.6010g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9117g Co (NO
3)
2.6H
20 with 8.0802gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 2h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 800 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
4. different calcining temperatures:
| Title | Precipitation agent consumption/mol | Aging Temperature/℃ | Digestion time/min | Calcining temperature/℃ | Saturation magnetization/emu.g -1 | Coercive force/Oe |
| Embodiment 1 | 0.09 | 92 | 60 | 800 | 75.20 | 716 |
| Embodiment 7 | 0.09 | 92 | 60 | 600 | 72.00 | 600 |
| Embodiment 8 | 0.09 | 92 | 60 | 1000 | 74.87 | 478 |
Embodiment 7
Take by weighing 3.6014g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9104g Co (NO
3)
2.6H
20 with 8.0812gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 600 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
Embodiment 8
Take by weighing 3.6005g NaOH adding 100ml distilled water and place the 500ml there-necked flask as precipitant solution, it is heated to 92 ℃ under the stir speed (S.S.) of 1500r/min.Take by weighing 2.9103g Co (NO
3)
2.6H
20 with 8.0805gFe (NO
3)
3.9H
20 is mixed with the 200ml mixing solutions, is placed in the constant pressure funnel at the uniform velocity to join in 30min in the previously prepd 100ml precipitation agent.After precipitation was complete, holding temperature was 92 ℃, and ageing reaction 1h will precipitate filtering and washing to filtrate pH=7, with the product 105 ℃ of oven dry in vacuum drying oven that obtain, through grinding to get the chocolate presoma.
At last, presoma in 1000 ℃ of lower calcining 1h, is namely got black CoFe
2O
4Magnetic nano powder.
Such as Fig. 3, Fig. 4, Fig. 5, shown in Figure 6, the embodiment Isosorbide-5-Nitrae, 6,8 saturation magnetization and coercive force are respectively 75.20,70.00,75.18,74.87emu/g and 716,724,592,478Oe.Sample all has good magnetic property, and has moderate coercive force, forms to have high saturation and magnetic intensity and moderate coercitive magnetic characteristic.
Claims (1)
1.CoFe
2O
4The preparation method of magnetic Nano material the steps include:
(1) take by weighing iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and be added to the water and be mixed with mixing solutions, the mol ratio of iron nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 2:1;
(2) weighing sodium hydroxide is added to the water and is mixed with solution as precipitation agent again, is heated to 60 ~ 92 ℃, and the mol ratio of sodium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES is 9 ~ 16:1; The aqueous solution of precipitation agent or dimethylamine, the perhaps aqueous solution of triethylamine, the perhaps aqueous solution of potassium hydroxide, dimethylamine, triethylamine, the mol ratio of potassium hydroxide and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES consumption is 9 ~ 16:1;
(3) mixing solutions was at the uniform velocity joined in 30 minutes in the precipitation agent under the agitation condition, holding temperature, ageing reaction 30 ~ 120 minutes will precipitate filtering and washing to filtrate and be neutral, and the chocolate presoma is dried, ground to get to the product that obtains;
(4) with presoma 600 ~ 1000 ℃ of lower thermal treatment 1 hour in air ambient, namely get CoFe
2O
4Magnetic Nano material.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204546A (en) * | 2013-04-17 | 2013-07-17 | 兰州大学 | Method for preparing nano cobalt ferrite |
| CN103601483A (en) * | 2013-12-03 | 2014-02-26 | 沈阳工业大学 | Novel synthetic method for lanthanum-manganese doped strontium ferrite magnetic powder |
| CN104496456A (en) * | 2014-12-02 | 2015-04-08 | 北京科技大学 | Preparation method of cobalt ferrite magnetostrictive material |
| CN105177517A (en) * | 2015-09-23 | 2015-12-23 | 南京理工大学 | Nanometer thermite and preparing method thereof |
| CN105199667A (en) * | 2015-10-21 | 2015-12-30 | 李同乐 | Continuous synthesis method of graphene/ferrite nanocomposite |
| CN106430331A (en) * | 2016-09-19 | 2017-02-22 | 青岛鼎元磁材有限公司 | Preparation method of high-coercivity, high-remanence and anti-fake magnetic powder |
| CN113976146A (en) * | 2021-11-18 | 2022-01-28 | 六盘水师范学院 | Preparation method and application of magnetic heterojunction catalyst for peroxymonosulfate activation |
| CN114538528A (en) * | 2022-02-28 | 2022-05-27 | 北京科技大学 | CoFe2O4Method for producing nano magnetic material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413945A (en) * | 2002-09-29 | 2003-04-30 | 西南师范大学 | Preparation method of water-base acid Co ferrite CoFe2O4 magnetic solution |
-
2012
- 2012-11-19 CN CN2012104642234A patent/CN102923785A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1413945A (en) * | 2002-09-29 | 2003-04-30 | 西南师范大学 | Preparation method of water-base acid Co ferrite CoFe2O4 magnetic solution |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204546A (en) * | 2013-04-17 | 2013-07-17 | 兰州大学 | Method for preparing nano cobalt ferrite |
| CN103204546B (en) * | 2013-04-17 | 2014-07-02 | 兰州大学 | Method for preparing nano cobalt ferrite |
| CN103601483A (en) * | 2013-12-03 | 2014-02-26 | 沈阳工业大学 | Novel synthetic method for lanthanum-manganese doped strontium ferrite magnetic powder |
| CN103601483B (en) * | 2013-12-03 | 2015-10-21 | 沈阳工业大学 | The synthetic method of lanthanum additive Mn iron strontium oxide magnetic powder |
| CN104496456A (en) * | 2014-12-02 | 2015-04-08 | 北京科技大学 | Preparation method of cobalt ferrite magnetostrictive material |
| CN105177517A (en) * | 2015-09-23 | 2015-12-23 | 南京理工大学 | Nanometer thermite and preparing method thereof |
| CN105199667A (en) * | 2015-10-21 | 2015-12-30 | 李同乐 | Continuous synthesis method of graphene/ferrite nanocomposite |
| CN105199667B (en) * | 2015-10-21 | 2018-01-12 | 李同乐 | A kind of method for continuously synthesizing of graphene/ferrite nano composite |
| CN106430331A (en) * | 2016-09-19 | 2017-02-22 | 青岛鼎元磁材有限公司 | Preparation method of high-coercivity, high-remanence and anti-fake magnetic powder |
| CN113976146A (en) * | 2021-11-18 | 2022-01-28 | 六盘水师范学院 | Preparation method and application of magnetic heterojunction catalyst for peroxymonosulfate activation |
| CN113976146B (en) * | 2021-11-18 | 2023-09-22 | 六盘水师范学院 | Preparation method and application of magnetic heterojunction catalyst for peroxymonosulfate activation |
| CN114538528A (en) * | 2022-02-28 | 2022-05-27 | 北京科技大学 | CoFe2O4Method for producing nano magnetic material |
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