CN104150544A - Method for acetate-assisted synthesis of monodisperse ferric acid cobalt nano powder material - Google Patents
Method for acetate-assisted synthesis of monodisperse ferric acid cobalt nano powder material Download PDFInfo
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- CN104150544A CN104150544A CN201410382089.2A CN201410382089A CN104150544A CN 104150544 A CN104150544 A CN 104150544A CN 201410382089 A CN201410382089 A CN 201410382089A CN 104150544 A CN104150544 A CN 104150544A
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- acetate
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Abstract
The invention discloses a method for acetate-assisted synthesis of a monodisperse ferric acid cobalt nano powder material. The method has the characteristics of simplicity, one step and environmental friendliness; the method for acetate-assisted synthesis of the monodisperse ferric acid cobalt nano powder material comprises the following steps: soluble iron source and cobalt source are added to a certain quantity of solvent according to that a stoichiometric proportion of the iron element to cobalt element is 2 to 1; then, a certain quantity of soluble acetate is added; when uniform stirring, the solvent is transferred to a reaction kettle; the solvent is maintained for a certain period of time in a sealed condition at a certain temperature; black nano powder materials are obtained; then, anhydrous ethanol is adopted to wash the black nano powder materials and remove activators and solvents which are absorbed on the surface; vacuum drying is conducted for a certain period of time at a certain temperature, so as to remove the anhydrous ethanol absorbed on the powder surface; the ferric acid cobalt powders are eventually prepared. The obtained ferric acid cobalt nano-powder material has the characteristics of purity, monodispersion and the like.
Description
Technical field
The invention belongs to technical field prepared by material, relate in particular to a kind of method of acetate secondary solvent thermal synthesis monodisperse ferrum-acid cobalt nano-powder material.
Background technology
Co ferrite Nano powder material has high magnetocrystalline anisotropy, high coercive force, the saturation magnetization of medium tenacity, and stable chemical performance, corrosion-resistant and wearing and tearing, at aspects such as magneto-optic recording material, magnetic fluid techniques, there is potential purposes, thereby enjoy material educational circles to pay close attention to.But the magnetic property of cobalt ferrite and application are subject to the impact of uniformity coefficient, preparing monodispersed cobalt ferrite nano-powder material is the significant challenge in the synthetic field of material.
The method that can successfully prepare at present vectolite magnetic nano powder material is a lot, but nearly all will use tensio-active agent protects nano particle, to prevent secondary nucleation or particle agglomeration.For example; Chinese patent CN103058284A has announced " a kind of preparation method of spinel type ferrous acid cobalt "; utilize coprecipitation method to synthesize cobalt ferrite powder body material; with cetyl trimethylammonium bromide (CTAB), cook protective material; tensio-active agent is one of industrial primary pollution source, and a large amount of uses are very large to environmental influence.Chinese patent CN101962210A has announced a kind of " industrialized process for preparing of monodisperse ferrum-acid cobalt nanometer particle "; utilize sol-gel method to synthesize monodisperse ferrum-acid cobalt nanometer particle etc.; although do not use protective material; but used the jelling agents such as methylene dichloride, methyl-formiate and used in a large number methyl alcohol or ethanol equal solvent, also very large on the impact of environment.Therefore, nonsurfactant of development, eco-friendly nanocrystalline regulation and control synthetic route are significant.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for the synthetic cobalt ferrite nano material of a kind of nonsurfactant, specifically, only with acetate, does electrostatic protection agent and synthesizes cobalt ferrite dispersed nano powder body material.
For solving the problems of the technologies described above, technical solution of the present invention is:
A method for the auxiliary synthetic monodisperse ferrum-acid cobalt nano-powder material of acetate, comprises following steps:
(1) by solubility source of iron and solubility cobalt source, the ratio that is 2:1 according to the stoichiometric ratio of ferro element and cobalt element, adds in solvent, then adds solubility acetate as promoting agent, stirs into clear solution;
(2) this solution is transferred in reactor, under air tight condition, at 160-240 ℃, kept 6-48h, obtain black nano powdered material;
(3) with this powder of absolute ethanol washing, at 60-80 ℃ of dry 2-8h, finally make cobalt ferrite powder.
Preferably, described solubility source of iron is a kind of in iron nitrate and iron(ic) chloride.
Preferably, described solubility cobalt source is a kind of in Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and cobalt chloride.
Preferably, described solvent is a kind of in ethylene glycol and glycerol.
Preferably, described solubility acetate is a kind of in sodium-acetate, Potassium ethanoate and ammonium acetate.
Adopt after such scheme, the method for the invention has following features:
1. simple, a step has just been synthesized cobalt ferrite nanoparticle;
2. environmental friendliness, is not used tensio-active agent, only with acetate, does electrostatic protection agent, is conducive to subsequent wash and processes;
3. synthetic cobalt ferrite particle diameter is even, has the features such as pure, and is monodispersed.
Accompanying drawing explanation
Fig. 1 is for adopting the X-ray diffraction analysis figure of the cobalt ferrite nanometer powder of the embodiment of the present invention 1 preparation;
Fig. 2 is for adopting the scanning electron microscope (SEM) photograph of the monodisperse ferrum-acid cobalt nanometer powder of the embodiment of the present invention 1 preparation.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
(1) by 0.2mol iron nitrate and 0.1mol Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, add in 200-400ml ethylene glycol, then add 0.9-1.5mol ammonium acetate, with stirrer, stirred into clear solution;
(2) this solution is transferred in 500ml reactor, at lower 180 ℃ of air tight condition, kept 12h, just obtain black nano powdered material;
(3), with this powder of absolute ethanol washing three times, at 70 ℃, dry 2h, finally makes cobalt ferrite powder.
(4) X-ray diffraction of the powdered sample obtaining and scanning electron microscope result are shown in respectively Fig. 1 and Fig. 2.
Embodiment 2
(1) by 0.2mol iron(ic) chloride and 0.1mol cobalt chloride, add in 200-400ml ethylene glycol, then add 0.9-1.5mol sodium-acetate, with stirrer, stirred into clear solution;
(2) this solution is transferred in 500ml reactor, at lower 180 ℃ of air tight condition, kept 12h, obtain black nano powdered material;
(3) with this powder of absolute ethanol washing three times to remove sodium-acetate and the ethylene glycol of surface adsorption, at 70 ℃, dry 2h, to remove the dehydrated alcohol of powder surface absorption, finally makes cobalt ferrite powder.
Embodiment 3
(1) by 0.2mol iron(ic) chloride and 0.1mol cobalt chloride, add in 200-400ml glycerol, then add 0.9-1.5mol Potassium ethanoate, with stirrer, stirred into clear solution;
(2) this solution is transferred in 500ml reactor, at lower 180 ℃ of air tight condition, kept 12h, obtain black nano powdered material;
(3) with this powder of absolute ethanol washing three times to remove Potassium ethanoate and the glycerol of surface adsorption, at 70 ℃, dry 2h, to remove the dehydrated alcohol of powder surface absorption, finally makes cobalt ferrite powder.
Claims (5)
1. acetate is assisted a method for synthetic monodisperse ferrum-acid cobalt nano-powder material, it is characterized in that comprising following steps:
(1) by solubility source of iron and solubility cobalt source, the ratio that is 2:1 according to the stoichiometric ratio of ferro element and cobalt element, adds in solvent, then adds solubility acetate as promoting agent, stirs into clear solution;
(2) this solution is transferred in reactor, under air tight condition, at 160-240 ℃, kept 6-48h, obtain black nano powdered material;
(3) with this powder of absolute ethanol washing, at 60-80 ℃ of dry 2-8h, finally make cobalt ferrite powder.
2. the method for the auxiliary synthetic monodisperse ferrum-acid cobalt nano-powder material of a kind of acetate according to claim 1, is characterized in that: described solubility source of iron is a kind of in iron nitrate and iron(ic) chloride.
3. the method for the auxiliary synthetic monodisperse ferrum-acid cobalt nano-powder material of a kind of acetate according to claim 1, is characterized in that: described solubility cobalt source is a kind of in Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES and cobalt chloride.
4. the method for the auxiliary synthetic monodisperse ferrum-acid cobalt nano-powder material of a kind of acetate according to claim 1, is characterized in that: described solvent is a kind of in ethylene glycol and glycerol.
5. the method for the auxiliary synthetic monodisperse ferrum-acid cobalt nano-powder material of a kind of acetate according to claim 1, is characterized in that: described solubility acetate is a kind of in sodium-acetate, Potassium ethanoate and ammonium acetate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410382089.2A CN104150544A (en) | 2014-08-06 | 2014-08-06 | Method for acetate-assisted synthesis of monodisperse ferric acid cobalt nano powder material |
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| CN201410382089.2A CN104150544A (en) | 2014-08-06 | 2014-08-06 | Method for acetate-assisted synthesis of monodisperse ferric acid cobalt nano powder material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800604A (en) * | 2016-04-22 | 2016-07-27 | 泰山医学院 | Preparation method of graphene-loaded cobalt ferrite quantum dot |
| CN107089688A (en) * | 2017-04-21 | 2017-08-25 | 四川理工学院 | A kind of preparation method and application of mesoporous cobalt ferrite material highly sensitive to acetone gas |
| CN110496592A (en) * | 2018-05-18 | 2019-11-26 | 南京理工大学 | The preparation method of magnetic montmorillonite adsorbent |
| 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 |
-
2014
- 2014-08-06 CN CN201410382089.2A patent/CN104150544A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| J. JIANG ET AL.: ""Synthesis and characterization of Fe–Co binary ferrospinel nanospheres via one-step nonaqueous solution pathway"", 《MATERIALS LETTERS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800604A (en) * | 2016-04-22 | 2016-07-27 | 泰山医学院 | Preparation method of graphene-loaded cobalt ferrite quantum dot |
| CN107089688A (en) * | 2017-04-21 | 2017-08-25 | 四川理工学院 | A kind of preparation method and application of mesoporous cobalt ferrite material highly sensitive to acetone gas |
| CN110496592A (en) * | 2018-05-18 | 2019-11-26 | 南京理工大学 | The preparation method of magnetic montmorillonite adsorbent |
| 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 |
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Application publication date: 20141119 |
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