CN102921960A - Preparation method of magnetic cobalt nanometer material - Google Patents
Preparation method of magnetic cobalt nanometer material Download PDFInfo
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- CN102921960A CN102921960A CN2012104639918A CN201210463991A CN102921960A CN 102921960 A CN102921960 A CN 102921960A CN 2012104639918 A CN2012104639918 A CN 2012104639918A CN 201210463991 A CN201210463991 A CN 201210463991A CN 102921960 A CN102921960 A CN 102921960A
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Abstract
The invention discloses a preparation method of a magnetic cobalt nanometer material. The preparation method is characterized by comprising the following steps: (1) preparing glycerol solution of cobalt nitrate, hydrazine and anionic surfactant, wherein the weight percentage of the cobalt nitrate, the hydrazine and the anionic surfactant is 46-49.5% of the cobalt nitrate, 47-51% of the hydrazine and 0-5.5% of the anionic surfactant; (2) heating the solution prepared in the step (1) until boiling under a stirring condition, and backflowing for 1.5 hours; and (3) magnetically separating the solution which is subjected to the heating and the backflowing processes, and obtaining the magnetic cobalt nanometer material. A one-step method is used for preparing the strong magnetic response cobalt nanometer material of which the surface is coated with amorphous cobalt, so that the preparation method of the magnetic cobalt nanometer material requires less production equipment, is simple in operation steps, low in cost and suitable for industrial production. The cobalt nitrate which contains six crystal water is used as a raw material, so that the raw material is convenient to obtain and contributes to the industrial production.
Description
Technical field
The present invention relates to a kind of magnetic cobalt preparations of nanomaterials method, particularly a kind of method for preparing stable metal cobalt nano material and regulation and control appearance of nano material.
Background technology
In recent years, along with the development of nano material and nanometer technology, magnetic Nano material owing to have be different from conventional nano material and body mutually the special nature of magnetic material be subject to people and pay close attention to widely, and show in a lot of fields wide application prospect.Compare with general ferrimagnet, therefore the metallic cobalt Curie temperature has high-temperature stability up to 1403 K.
Before the present invention, because the chemical instability of metallic cobalt, the chemical activity of nanometer cobalt material is stronger, thereby its application is very restricted.And people often adopt at magnetic cobalt nano-material surface clad surface activating agent, polymer etc., strengthen thus the stability of cobalt nano material.But these methods have reduced again the magnetic of cobalt nano material.
Summary of the invention
Purpose of the present invention just is to overcome defects, design, a kind of stable magnetic cobalt preparation method of nano material of development.
Technical scheme of the present invention is: a kind of magnetic cobalt preparations of nanomaterials method, it is characterized in that, and comprise the steps:
(1) the glycerine solution of preparation cobalt nitrate, hydrazine and anion surfactant, take glycerine as solvent, in glycerine, add cobalt nitrate, hydrazine and anion surfactant, fully be dissolved into glycerine solution, wherein, the percentage by weight of cobalt nitrate, hydrazine and anion surfactant is: cobalt nitrate 46-49.5%, hydrazine 47-51%, anion surfactant 0-5.5%;
(2) solution with step (1) preparation is heated to boiling under stirring condition, refluxes 1.5 hours;
(3) solution after step (2) the heating reflow treatment is carried out magnetic and separate, obtain magnetic Nano material.
Glycerine solution described in the step (1) with glycerine as solvent.
Anion surfactant described in the step (1) is (2-ethylhexyl) succinate sodium sulfonate.
After the magnetic Nano material that the magnetic separation obtains in the step (3) replaces washing with absolute ethyl alcohol and acetone, drying.
The consumption of described glycerine fully dissolves for reaching cobalt nitrate, hydrazine and anion surfactant.
Advantage of the present invention and effect are that one-step method has prepared the strong magnetic response cobalt nano material of the amorphous cobalt of surperficial coating.Simultaneously, the adding of (2-ethylhexyl) succinate sodium sulfonate is the pattern of controlled material obviously, changes its magnetic property.
It is few that the one of the main divisions of the male role in traditional opera of the inventive method institute produces equipment, and operating procedure is simple, and cost is low, so than suitability for industrialized production.Raw material adopts the cobalt nitrate that contains six crystallizations water, and purpose is the raw material convenience, is easy to get, and is conducive to suitability for industrialized production.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the embodiment of the invention 1 made magnetic cobalt nano material.
Fig. 2 is the transmission electron microscope photo of the embodiment of the invention 1 made magnetic cobalt nano material.
Fig. 3 is the hysteresis curve of the embodiment of the invention 1 made magnetic cobalt nano material.
Fig. 4 is the x-ray diffraction pattern of the embodiment of the invention 2 made magnetic cobalt nano materials.
Fig. 5 is the transmission electron microscope photo of the embodiment of the invention 2 made magnetic cobalt nano materials.
Fig. 6 is the hysteresis curve of the embodiment of the invention 2 made magnetic cobalt nano materials.
Fig. 7 is the transmission electron microscope photo of the embodiment of the invention 3 made magnetic cobalt nano materials.
Fig. 8 is the hysteresis curve of the embodiment of the invention 3 made magnetic cobalt nano materials.
The specific embodiment
Embodiment 1:
1. the mol ratio by cobalt nitrate and hydrazine is 1 ︰ 6, take by weighing respectively three cobalt nitrates, 1.4545 g that contain six crystallizations water, hydrazine 1.500 g of a crystallization water, be dissolved in (consumption of glycerine fully dissolves for reaching cobalt nitrate, hydrazine and anion surfactant) in the 70 ml glycerine.Add hydrazine and play the effect of reducing agent, simultaneously contained N atom can with the Co coordination, affect structure and the pattern of product.Glycerine utilizes its high viscosity as solvent, affects the movement of ion and the clustered pattern of control product.
2. mentioned solution is heated to boiling, and refluxed 1.5 hours.
3. the method for separating with magnetic is separated mentioned solution, obtains magnetic-particle.And with absolute ethyl alcohol, acetone alternately washing for several times, drying.
Shown in Fig. 1,2 and 3.The structure of product and phase are identified and are adopted German Bruker AXS D8 ADVANCE X-ray powder diffraction instrument (XRD, Cu K
αRadiation, λ=1.54056,40 kV, 200 mA) measure.Adopt JEM-2000EX type transmission electron microscope that pattern and the granular size of product are observed.(VSM, Lakeshore 7307, USA) measure sample magnetic to adopt vibrating specimen magnetometer.
Result of the test shows:
Fig. 1: the x-ray diffraction pattern of the embodiment of the invention 1 products made thereby.Its X-ray diffraction peak (approximately 45
o) corresponding to (002) crystal face (No.15-0806, JCPDS-ICDD) of cobalt, belong to the hexagonal closs packing crystal.20 ~ 40
oWith 40 ~ 60
oThe corresponding amorphous cobalt of the broad peak of scope.Illustrate that embodiment 1 products made thereby is high-purity cobalt simple substance.
Fig. 2: the transmission electron microscope photo of the embodiment of the invention 1 made magnetic Nano material.From this figure as can be known, products made thereby is sphere and blocky-shaped particle.The spheric granules particle diameter is the hundreds of nanometer approximately.The illustration of Fig. 2 is single spheroid, shows that obviously spheroid is nucleocapsid structure.The corresponding amorphous cobalt of shell, kernel is the cobalt crystal.
Fig. 3: the hysteresis curve of the embodiment of the invention 1 made magnetic Nano material.Show that the sample saturation magnetization is 152 emu/g, coercivity is 50 Oe.
Embodiment 2:
1. the mol ratio by cobalt nitrate and hydrazine is 1 ︰ 6, take by weighing respectively hydrazine 1.500 g, (2-ethylhexyl) succinate sodium sulfonate 0.0308 g of three cobalt nitrates, 1.4545 g that contain six crystallizations water, a crystallization water, be dissolved in (consumption of glycerine fully dissolves for reaching cobalt nitrate, hydrazine and anion surfactant) in the 70 ml glycerine.Add hydrazine and play the effect of reducing agent, simultaneously contained N atom can with the Co coordination, affect structure and the pattern of product.Glycerine utilizes its high viscosity as solvent, affects the movement of ion and the clustered pattern of control product.(2-ethylhexyl) succinate sodium sulfonate is the stronger two tail anion surfactants of surface-active.It can be adsorbed on solid particles surface, affects its growth and gathering.
2. mentioned solution is heated to boiling, and refluxed 1.5 hours.
3. the method for separating with magnetic is separated mentioned solution, obtains magnetic-particle.And with absolute ethyl alcohol, acetone alternately washing for several times, drying.
Shown in Fig. 4,5 and 6.
Result of the test shows:
Fig. 4: the x-ray diffraction pattern of the embodiment of the invention 2 products made therebies.Its X-ray diffraction peak is (100), (002), (101), (102), (110) crystal faces (No.15-0806, JCPDS-ICDD) from left to right according to this, belongs to the hexagonal closs packing crystal.Illustrate that embodiment 2 products made therebies are high-purity cobalt simple substance.
Fig. 5: the transmission electron microscope photo of the embodiment of the invention 2 made magnetic Nano materials.From this figure as can be known, products made thereby mainly is spheric granules.Spheroid is nucleocapsid structure.The corresponding amorphous cobalt of shell, kernel is the cobalt crystal.
Fig. 6: the hysteresis curve of the embodiment of the invention 2 made magnetic Nano materials.Show that the sample saturation magnetization is 133 emu/g, coercivity is 70 Oe.
Embodiment 3:
1. the mol ratio by cobalt nitrate and hydrazine is 1 ︰ 6, take by weighing respectively hydrazine 1.500 g, (2-ethylhexyl) succinate sodium sulfonate 0.1540 g of three cobalt nitrates, 1.4545 g that contain six crystallizations water, a crystallization water, be dissolved in (consumption of glycerine fully dissolves for reaching cobalt nitrate, hydrazine and anion surfactant) in the 70 ml glycerine.Add hydrazine and play the effect of reducing agent, simultaneously contained N atom can with the Co coordination, affect structure and the pattern of product.Glycerine utilizes its high viscosity as solvent, affects the movement of ion and the clustered pattern of control product.(2-ethylhexyl) succinate sodium sulfonate is the stronger two tail anion surfactants of surface-active.It can be adsorbed on solid particles surface, affects its growth and gathering.
2. mentioned solution is heated to boiling, and refluxed 1.5 hours.
3. the method for separating with magnetic is separated mentioned solution, obtains magnetic-particle.And with absolute ethyl alcohol, acetone alternately washing for several times, drying.
Shown in Fig. 5,7 and 8.
Result of the test shows:
Fig. 5: the x-ray diffraction pattern of the embodiment of the invention 3 made samples and embodiment 2 products made therebies is identical.
Fig. 7: the transmission electron microscope photo of the embodiment of the invention 3 made magnetic Nano materials.From this figure as can be known, products made thereby mainly is linear structure.This structure also is nucleocapsid structure, the corresponding amorphous cobalt of shell, and kernel is the cobalt crystal.
Fig. 8: the hysteresis curve of the embodiment of the invention 3 made magnetic Nano materials.Show that the sample saturation magnetization is 126 emu/g, coercivity is 210 Oe.
According to above-mentioned result of study as can be known: the present invention uses fairly simple experimental technique, synthesized the magnetic hexagonal closs packing cobalt nano material of the stable amorphous cobalt of coating, and sample magnetic is adjustable.
Claims (4)
1. a magnetic cobalt preparations of nanomaterials method is characterized in that, comprises the steps:
(1) the glycerine solution of preparation cobalt nitrate, hydrazine and anion surfactant, take glycerine as solvent, in glycerine, add cobalt nitrate, hydrazine and anion surfactant, fully be dissolved into glycerine solution, wherein, the percentage by weight of cobalt nitrate, hydrazine and anion surfactant is: cobalt nitrate 46-49.5%, hydrazine 47-51%, anion surfactant 0-5.5%;
(2) solution with step (1) preparation is heated to boiling under stirring condition, refluxes 1.5 hours;
(3) solution after step (2) the heating reflow treatment is carried out magnetic and separate, obtain magnetic Nano material.
2. a kind of magnetic cobalt preparations of nanomaterials method according to claim 1 is characterized in that, glycerine solution described in the step (1) with glycerine as solvent.
3. a kind of magnetic cobalt preparations of nanomaterials method according to claim 1 is characterized in that, anion surfactant described in the step (1) is (2-ethylhexyl) succinate sodium sulfonate.
4. a kind of magnetic cobalt preparations of nanomaterials method according to claim 1 is characterized in that, after the magnetic Nano material that the magnetic separation obtains in the step (3) replaces washing with absolute ethyl alcohol and acetone, and drying.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170991A (en) * | 2015-08-20 | 2015-12-23 | 河北工业大学 | Method for preparing superfine metallic cobalt powder |
| CN109837534A (en) * | 2019-02-26 | 2019-06-04 | 西安文理学院 | A kind of method that gas-liquid interface prepares nanometer cobalt film |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN116180067A (en) * | 2022-10-27 | 2023-05-30 | 北京科技大学 | Preparation method of high-temperature ferromagnetic aluminum cobalt oxide parallel orientation nano-sheet array material |
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| CN1712157A (en) * | 2005-03-31 | 2005-12-28 | 中国工程物理研究院激光聚变研究中心 | Cobalt nanometer particle or crumb and production thereof |
| CN1923415A (en) * | 2006-07-20 | 2007-03-07 | 兰州大学 | Process for preparing nano granule with high shape anisotropic property |
| CN101121205A (en) * | 2007-09-14 | 2008-02-13 | 北京科技大学 | Method for preparing nanometer cobalt powder using with cobalt acetate low temperature |
| CN101298102A (en) * | 2008-06-13 | 2008-11-05 | 上海师范大学 | Preparation of nano cobalt granule |
| CN102091787A (en) * | 2009-12-11 | 2011-06-15 | 胥建中 | Method for preparing nano cobalt powder |
| CN102363219A (en) * | 2011-11-21 | 2012-02-29 | 新疆大学 | Method for synthesizing floriform cobalt magnetic powder by mixed solvent thermal method |
| US8152893B2 (en) * | 2008-12-03 | 2012-04-10 | Tatung Company | One dimension nano magnetic wires and manufacturing method thereof |
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2012
- 2012-11-19 CN CN2012104639918A patent/CN102921960A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1712157A (en) * | 2005-03-31 | 2005-12-28 | 中国工程物理研究院激光聚变研究中心 | Cobalt nanometer particle or crumb and production thereof |
| CN1923415A (en) * | 2006-07-20 | 2007-03-07 | 兰州大学 | Process for preparing nano granule with high shape anisotropic property |
| CN101121205A (en) * | 2007-09-14 | 2008-02-13 | 北京科技大学 | Method for preparing nanometer cobalt powder using with cobalt acetate low temperature |
| CN101298102A (en) * | 2008-06-13 | 2008-11-05 | 上海师范大学 | Preparation of nano cobalt granule |
| US8152893B2 (en) * | 2008-12-03 | 2012-04-10 | Tatung Company | One dimension nano magnetic wires and manufacturing method thereof |
| CN102091787A (en) * | 2009-12-11 | 2011-06-15 | 胥建中 | Method for preparing nano cobalt powder |
| CN102363219A (en) * | 2011-11-21 | 2012-02-29 | 新疆大学 | Method for synthesizing floriform cobalt magnetic powder by mixed solvent thermal method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170991A (en) * | 2015-08-20 | 2015-12-23 | 河北工业大学 | Method for preparing superfine metallic cobalt powder |
| CN109837534A (en) * | 2019-02-26 | 2019-06-04 | 西安文理学院 | A kind of method that gas-liquid interface prepares nanometer cobalt film |
| CN109837534B (en) * | 2019-02-26 | 2020-09-29 | 西安文理学院 | Method for preparing nano cobalt film on gas-liquid interface |
| CN113059179A (en) * | 2021-03-17 | 2021-07-02 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN116180067A (en) * | 2022-10-27 | 2023-05-30 | 北京科技大学 | Preparation method of high-temperature ferromagnetic aluminum cobalt oxide parallel orientation nano-sheet array material |
| CN116180067B (en) * | 2022-10-27 | 2024-03-12 | 北京科技大学 | Preparation method of high-temperature ferromagnetic aluminum cobalt oxide parallel orientation nano-sheet array material |
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Application publication date: 20130213 |